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Sample records for reconstructed layered hydroxide

  1. Novel synthesis of layered double hydroxides (LDHs) from zinc hydroxide

    Science.gov (United States)

    Meng, Zilin; Zhang, Yihe; Zhang, Qian; Chen, Xue; Liu, Leipeng; Komarneni, Sridhar; Lv, Fengzhu

    2017-02-01

    The most common synthesis methods for layered double hydroxides (LDHs) are co-precipitation and reconstruction, which can have some limitations for application. Here, we report a novel synthesis method for LDHs. We use zinc hydroxide as the precursor to synthesize LDHs phase through a simple transformation process of zinc hydroxide phase. For this transformation process, aluminum can enter into zinc hydroxide and replace zinc quickly to transform it into LDH by creating positive charges in the zinc hydroxide solid phase. The mechanism of LDH formation was through Al3+ reaction first with zinc hydroxide followed by recrystallization of the original structure of zinc hydroxide. Thus, the new process of LDH formation involves a reaction of Al to substitute for Zn and recrystallization leading to LDH and the final pH influences the crystallization of LDHs by this process. In addition, Cr3+ was employed as a trivalent cation for LDH formation to react with zinc hydroxide, which also led to LDH structure.

  2. Hybridization Between Natural Extract of Angelica gigas Nakai and Inorganic Nanomaterial of Layered Double Hydroxide via Reconstruction Reaction.

    Science.gov (United States)

    Kim, Tae-Hyun; Kim, Hyoung-Jun; Choi, Ae-Jin; Choi, Hyun-Jin; Oh, Jae-Min

    2016-01-01

    We have hybridized layered double hydroxide (LDH) with Angelica gigas Nakai root extract (AGNR) through reversible dehydration-rehydration reaction which is known as reconstruction. LDHs having well-ordered hydrotalcite-like crystal structure and average size 250 ± 20 nm were prepared by hydrothermal method. The root of Angelica gigas Nakai, which has been utilized in the treatment of female disorders as herbal medicine, was treated with methanol to obtain extract. Pristine LDHs were calcined at 400 °C for 8 hours to obtain layered double oxide (LDO), which was further dispersed into extract solution with various AGNR/LDO weight ratios, 0.11, 0.21 and 0.43. The extract content in each hybrid increased in proportion to initial AGNR/LDO ratio, showing the highest content of ~12%. The zeta potential of LDH shifted from +44 mV to +20 mV upon hybridization with extract, which was attributed to the adsorption of negatively charged organic moieties in AGNR on LDH surface. The scanning electron microscopic (SEM) results exhibited that the random stacking of LDH nanolayers resulted in LDH-AGNR hybrid with house-of-cards structure, of which inter-particle cavity serves nano-reservoir for natural extract. According to quantitative analyses, it was revealed that the content of active components in AGNR increased when they were hybridized with LDHs compared with those in AGNR alone.

  3. Supermolecular layered dou- ble hydroxides

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Research progresses in the layered double hydroxides ·mH2O intercalated with metal coordinate ions or oxometalates in the last ten years are reviewed. These layered double hydroxides are mainly intercalated with polyoxometalate (POM) ions, a LiAl-LDH photochemical assembly containing TiO2 and CH3(CH2)12COO- anions, together with Zn(TPPC) (porphy-rin derivate) and macrocyclic ligand-containing porphyrin derivate anions. Emphasis is put on the synthesis methods for intercalation of the anions into the interlayer regions, the characterization techniques and structures for the layered compounds and the newest research progress in the fields such as catalysis. The review also forecasts the prospects of the field.

  4. Thermal decomposition and reconstruction of CaFe-layered double hydroxide studied by X-ray diffractometry and 57Fe Mössbauer spectroscopy

    Science.gov (United States)

    Bugris, Valéria; Ádok-Sipiczki, Mónika; Anitics, Tamás; Kuzmann, Ernő; Homonnay, Zoltán; Kukovecz, Ákos; Kónya, Zoltán; Sipos, Pál; Pálinkó, István

    2015-06-01

    In spite of numerous investigations on the various processes of the thermal decomposition and rehydration of layered double hydroxides (LDHs) by a variety sophisticated experimental means, many details are still unexplored and some contradictions are still unresolved. In this work, our efforts were focussed on clarifying the composition, structure and properties of thermally decomposed metaphases originating from CaFe-LDH, heat treated in the 373-973 K temperature range. The structure reconstruction ability of mixed metal oxide phases obtained after heat treatments was also investigated, mainly concentrating on the changes in the microenvironment of Fe(III), in the presence of controlled amount of water vapour (i.e., at different relative humidities). All samples were characterised by X-ray diffractometry, and the iron-containing phases were studied by 57Fe Mössbauer spectroscopy.

  5. Thermal decomposition behavior of Cu–Al layered double hydroxide, and ethylenediaminetetraacetate-intercalated Cu–Al layered double hydroxide reconstructed from Cu–Al oxide for uptake of Y{sup 3+} from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Kameda, Tomohito, E-mail: kameda@env.che.tohoku.ac.jp [Graduate School of Environmental Studies, Tohoku University, 6-6-07 Aoba, Aramaki, Aoba-ku, Sendai 980-8579 (Japan); Hoshi, Kazuaki; Yoshioka, Toshiaki [Graduate School of Environmental Studies, Tohoku University, 6-6-07 Aoba, Aramaki, Aoba-ku, Sendai 980-8579 (Japan)

    2012-12-15

    Graphical abstract: Display Omitted Highlights: ► Decomposition of CO{sub 3}·Cu–Al LDH occurred in four stages. ► The edta·Cu–Al LDH was found to take up Y{sup 3+} in aqueous solution. ► The edta·Cu–Al LDH could selectively take up rare earth ions from a mixed solution. -- Abstract: CO{sub 3}{sup 2−}-intercalated Cu–Al layered double hydroxide (CO{sub 3}·Cu–Al LDH) was calcined to yield Cu–Al oxide, and then ethylenediaminetetraacetate-intercalated Cu–Al LDH (edta·Cu–Al LDH) was prepared by reconstructing Cu–Al oxide in edta solution. Decomposition of CO{sub 3}·Cu–Al LDH occurred in four stages. The production of Cu–Al oxide was caused by the thermal decomposition of CO{sub 3}·Cu–Al LDH until the third stage. The first stage was the elimination of adsorbed surface water and interlayer water in CO{sub 3}·Cu–Al LDH. The second and third stages were the dehydroxylation of the brucite-like octahedral layers and the elimination of CO{sub 3}{sup 2−} intercalated in the interlayers. The edta·Cu–Al LDH was found to take up Y{sup 3+} in aqueous solution. The uptake of Y{sup 3+} was caused not only by the chelating function of Hedta{sup 3−} in the interlayer but also by the chemical behavior of Cu–Al LDH itself. The edta·Cu–Al LDH was found to selectively take up rare earth ions from a mixed solution. The degree of uptake was high, in the order Sc{sup 3+} > Y{sup 3+} > La{sup 3+} for all time durations, which was attributable to differences among the stabilities of Sc(edta){sup −}, Y(edta){sup −} and La(edta){sup −}.

  6. Uptake of Sc 3+ and La 3+ from aqueous solution using ethylenediaminetetraacetate-intercalated Cu-Al layered double hydroxide reconstructed from Cu-Al oxide

    Science.gov (United States)

    Kameda, Tomohito; Hoshi, Kazuaki; Yoshioka, Toshiaki

    2011-02-01

    A Cu-Al layered double hydroxide intercalated with ethylenediaminetetraacetate (edta·Cu-Al LDH) was prepared by suspending Cu-Al oxide, obtained by the calcination of CO32--intercalated Cu-Al LDH, in edta solution. It was found that the reconstruction of Cu-Al oxide to Cu-Al LDH was promoted with an increase in the temperature and time. The reaction in the pH range of around 8 suggests that Hedta 3- was intercalated in the interlayer of Cu-Al LDH. Edta·Cu-Al LDH was found to take up rare metal ions such as Sc 3+ and La 3+ in an aqueous solution at a pH of around 6-6.5. The uptake of Sc 3+ was caused not only by the chelating function of Hedta 3- in the interlayer but also by the chemical behavior of Cu-Al LDH itself. On the other hand, the uptake of La 3+ was caused only by the chelating function of Hedta 3- in the interlayer. The Hedta 3- in the interlayer of edta·Cu-Al LDH had the potential to form a chelate complex more preferentially with Sc 3+ than with La 3+.

  7. Synthesis of layered double hydroxides from eggshells

    Energy Technology Data Exchange (ETDEWEB)

    Li Songnan [Key Laboratory of Superlight Materials and Surface Technology, Ministry of Education, 150001 (China); Wang Fangyong [College of Engineering and Technology, Northeast Forestry University, 150001 (China); Jing Xiaoyan [Key Laboratory of Superlight Materials and Surface Technology, Ministry of Education, 150001 (China); Wang Jun, E-mail: zhqw1888@sohu.com [Key Laboratory of Superlight Materials and Surface Technology, Ministry of Education, 150001 (China); Saba, Jamil; Liu Qi; Ge Lan; Song Dalei; Zhang Milin [Key Laboratory of Superlight Materials and Surface Technology, Ministry of Education, 150001 (China)

    2012-01-16

    Graphical abstract: This is the XRD pattern and TEM image of 4Ca-Al layered double hydroxide, which is obtained from eggshells. It can be seen that the sample is of layered double hydroxide and shows the plate-like agglomerations with an average size of 20-100 nm. Highlights: Black-Right-Pointing-Pointer We synthesize layered double hydroxides from eggshells. Black-Right-Pointing-Pointer Eggshells are the mainly material in this method. Black-Right-Pointing-Pointer The additional alkaline solution is not required. - Abstract: Ca-Al and Ca-Fe layered double hydroxides (LDHs) were successfully synthesized from chicken eggshells by an ultrasonic wave assistant method. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR) techniques. XRD and TEM analyses showed that the 4Ca-Al LDHs were of high purity but other samples were not. The present study provides a simple, efficient and environmental friendly method to obtain LDHs from biowaste eggshells, in which additional alkaline solution is not required for synthesis. Moreover, eggshells provide all the requisite bivalent metal ions, which are needed to form layered double hydroxides.

  8. Polysulfide intercalated layered double hydroxides for metal capture applications

    Science.gov (United States)

    Kanatzidis, Mercouri G.; Ma, Shulan

    2017-04-04

    Polysulfide intercalated layered double hydroxides and methods for their use in vapor and liquid-phase metal capture applications are provided. The layered double hydroxides comprise a plurality of positively charged host layers of mixed metal hydroxides separated by interlayer spaces. Polysulfide anions are intercalated in the interlayer spaces.

  9. Polysulfide intercalated layered double hydroxides for metal capture applications

    Energy Technology Data Exchange (ETDEWEB)

    Kanatzidis, Mercouri G.; Ma, Shulan

    2017-04-04

    Polysulfide intercalated layered double hydroxides and methods for their use in vapor and liquid-phase metal capture applications are provided. The layered double hydroxides comprise a plurality of positively charged host layers of mixed metal hydroxides separated by interlayer spaces. Polysulfide anions are intercalated in the interlayer spaces.

  10. Layered Double Hydroxide as Cordycepin Delivery Nanocarrier

    Institute of Scientific and Technical Information of China (English)

    Qin Zheng YANG; Jing YANG; Chang Kai ZHANG

    2006-01-01

    Layered double hydroxide was investigated as cordycepin delivery nanocarrier for the first time in this study. Negatively charged biomolecule-cordycepin was intercalated in the gallery spaces of [Mg-Al-NO3], which was confirmed by the results of X-ray diffraction and electrophoretic mobility. Cell experiment suggested that the new bio-LDH nanohybrid could prevent cordycepin decomposition by adenosine deaminase. This new formulation could possibly be used as a novel form cordycepin intravenous injection.

  11. Layered double hydroxide stability. 1. Relative stabilities of layered double hydroxides and their simple counterparts

    Science.gov (United States)

    Boclair, J. W.; Braterman, P. S.

    1999-01-01

    Solutions containing di- and trivalent metal chlorides [M(II) = Mg2+, Zn2+, Co2+, Ni2+, Mn2+; M(III) = Al3+, Fe3+] were titrated with NaOH to yield hydrotalcite-like layered double hydroxides (LDH), [[M(II)]1-x[M(III)]x(OH)2][Cl]x yH2O, by way of M(III) hydroxide/hydrous oxide intermediates. Analysis of the resultant titration curves yields nominal solubility constants for the LDH. The corresponding LDH stabilities are in the order Mg hydroxides/hydrous oxides is discussed.

  12. USING COLLOIDAL LAYERED DOUBLE HYDROXIDES AS CATIONIC MICROPARTICULATE COMPONENT

    Institute of Scientific and Technical Information of China (English)

    Songlin Wang; Wenxia Liu

    2004-01-01

    Layered double hydroxides consisting of layers with cationic charges may be potential candidates of cationic microparticles forming synergetic retention effect with anionic polyacrylamide. In this work, the layered double hydroxides with various molar ratios of Mg/Al were synthesized by co-precipitation of magnesium chloride and aluminum chloride and peptized by intense washing with water. The chemical formula, particle size, Zeta potential of the layered double hydroxide were analyzed. It was found that positively charged magnesium aluminum hydroxide with particle diameter in nanoparticle size could be prepared. The Zeta potential and particle size vary with the feed molar ratio of Mg/Al and the peptizing process, respectively. The Zeta potential is also pH dependent. The retention experiments carried out on DDJ show that when used together with anionic polyacrylamide, the positively charged colloidal double hydroxide greatly improves the retention of reed pulps. The chemical formula, particle size and Zeta potential of the colloidal double hydroxide all affect its retention behavior.

  13. Photo-oxidation of EPDM/layered double hydroxides composites: Influence of layered hydroxides and stabilizers

    Directory of Open Access Journals (Sweden)

    2007-11-01

    Full Text Available The photo-oxidation of ethylene propylene diene monomer (EPDM/ layered double hydroxide (LDH composites as well as EPDM/LDH with stabilizers is studied under accelerated UV irradiation (λ≥290 nm at 60°C for different time intervals. The development of functional groups during oxidation was monitored by FT-IR spectroscopy. The photodegradation of the pristine polymer and composites take place and the increase in hydroxyl and carbonyl groups with irradiation times, was estimated. EPDM filled LDH showed higher degradation rate than pristine EPDM, while in acidic medium EPDM/LDH showed almost equal degradation as in isolated conditions. These results show the advantages of LDHs as a filler as well as an acid killer. The effect of stabilizers is very less because of their concentration in comparison of LDH.

  14. USING COLLOIDAL LAYERED DOUBLE HYDROXIDES AS CATIONICMICROPARTICULATE COMPONENT

    Institute of Scientific and Technical Information of China (English)

    SonglinWang; WenxiaLiu

    2004-01-01

    Layered double hydroxides consisting of layers withcationic charges may be potential candidates ofcationic microparticles forming synergetic retentioneffect with anionic polyacrylamide. In this work, thelayered double hydroxides with various molar ratiosof Mg/AI were synthesized by co-precipitation ofmagnesium chloride and aluminum chloride and pep-tized by intense washing with water. The chemicalformula, particle size, Zeta potential of the layereddouble hydroxide were analyzed. It was found thatpositively charged magnesium aluminum hydroxidewith particle diameter in nanoparticle size could beprepared. The Zeta potential and particle size varywith the feed molar ratio of Mg/A1 and the peptizingprocess, respectively. The Zeta potential is also pHdependent. The retention experiments carried out onDDJ show that when used together with anionic poly-acrylamide, the positively charged colloidal doublehydroxide greatly improves the retention of reedpulps. The chemical formula, particle size and Zetapotential of the colloidal double hydroxide all affectits retention behavior.

  15. Synthesis of ACECLOFENAC/HYDROXYPROPYL-β-CYCLODEXTRIN Intercalated Layered Double Hydroxides and Controlled Release Properties

    Science.gov (United States)

    Li, Shifeng; Shen, Yanming; Liu, Dongbin; Fan, Lihui; Wu, Keke; Xiao, Min

    2013-04-01

    Aceclofenac (AC)/hydroxypropyl-β-cyclodextrin (HP-β-CD) complex intercalated layered double hydroxides (LDHs) have been synthesized by reconstruction method. X-ray diffraction, Fourier transform infrared and thermal gravimetric analyses indicated a successful intercalation of AC/HP-β-CD complex into the LDHs gallery. The AC release properties were also studied in different pH values buffer solution. The results indicate that the AC/HP-β-CD intercalated LDH has a potential application in drug delivery agent.

  16. Recent progress in polymer/layered double hydroxide nanocomposites

    Institute of Scientific and Technical Information of China (English)

    DING Peng; CHEN Wei; QU Baojun

    2006-01-01

    New developments in the studies of nanocomposites based on polymer matrixes and layered double hydroxides (LDHs)in recent years are reviewed combining our relative research work, among which the synthesis techniques, the physicochemical characterizations, and the improved material properties are especially discussed. The possible application of polymer/LDH nanocomposites is also proposed.

  17. Preferential Intercalation of Pyridinedicarboxylates into Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    李蕾; 莫丹; 陈大舟

    2005-01-01

    Intercalation of 2,3-,2,4-,2,5-,2,6-,3,4-,or3,5-pyridincdicarboxylate into the layered double hydroxide (LDH),[Mg0.73AIo.27(OH)2](CO3)0.14*1.34H2O was carried out by the reconstruction method in the molar ratio of organic acid: calcined LDH=3:8, in 80% alcoholic aqueous solution at 70℃. Selective reaction was observed in com-petitive experiments involving an equal concentration pairs of acids. The preference order of the organic acids intercalated into the Mg-Al-LDH was found to be in the order of 2,3-pyridinedicarboxylate>2,5-pyridinedicarboxylate>2,4-pyridinedicarboxylate>3,5-pyridinedicarboxylate>3,4-pyridinedicarboxylate>2,6-pyridinedic arboxylate. The structures of the intercalates formed by the reaction of six guests with Mg-Al-LDH were characterized by X-ray diffraction, infrared and thermogravimetry techniques. And the charge density on the oxygens of each of the carboxylate groups for the six anions was investigated utilizing ab initio (HF/6-31G) method by G98w. From the X-ray diffraction data, the guest size and the charge density of the oxygens of the guest, the orientation of 2,3-,2,4-,2,5-,2,6-,3,4-, or 3,5-pyridinedicarboxylate anions between the layers was determined and the preferential intercalation mechanism was discussed. These results indicate the possibility of a molecular recognition ability of LDH and it would be exploited for the chemical separation of some anions from solution.

  18. Oxidative leaching of chromium from layered double hydroxides: Mechanistic studies

    Indian Academy of Sciences (India)

    A V Radha; P Vishnu Kamath

    2004-08-01

    The layered double hydroxide (LDH) of Zn with Cr on treatment with a hypochlorite solution releases chromate ions as a result of oxidative leaching by a dissolution–reprecipitation mechanism. The residue is found to be -Zn(OH)2. The LDH of Mg with Cr on the other hand is resistant to oxidative leaching. In contrast, a X-ray amorphous gel of the coprecipitated hydroxides of Mg and Cr yields chromate ions. These results suggest that the oxidation potential of Cr(III) in LDHs is determined by the nature of the divalent ion and the crystallinity of the phase while being unaffected by the nature of the intercalated anions.

  19. Immobilization of laccase on hybrid layered double hydroxide

    Directory of Open Access Journals (Sweden)

    David Isidoro Camacho Córdova

    2009-01-01

    Full Text Available Crystals of Mg/Al layered double hydroxide were synthesized by alkaline precipitation and treated in an aqueous solution of glutamic acid. The glutamate ions were not intercalated into the interlayer space, but were detected in the material by Fourier transform infrared spectroscopy, suggesting that only the external surfaces of crystals were modified with glutamate ions. The resulting hybrid material was tested as a support for immobilization of the enzyme laccase (Myceliophthora thermophila. The immobilized enzyme preparation was characterized by electronic paramagnetic resonance spectroscopy and by assays of catalytic activity. The activity of the immobilized laccase was 97% of the activity in the free enzyme. Layered double hydroxide is a suitable support for use in remediation of soil studies.

  20. Hydrothermal Synthesis of Ni/Al Layered Double Hydroxide Nanorods

    OpenAIRE

    Yun Zhao; Fenfei Xiao; Qingze Jiao

    2011-01-01

    Ni/Al layered double hydroxide (LDH) nanorods were successfully synthesized by the hydrothermal reaction. The crystal structure of the products was characterized by X-ray diffraction (XRD). The morphology of the products was observed using transmission electron microscopy (TEM) and field emission scanning electron microscopy (SEM). The influences of reaction time and pH value on the morphology of the Ni/Al LDHs were investigated. The result showed that the well-crystallized nanorods of Ni/Al ...

  1. Chemical modification of zinc hydroxide nitrate and Zn-Al-layered double hydroxide with dicarboxylic acids.

    Science.gov (United States)

    Arizaga, Gregorio Guadalupe Carbajal; Mangrich, Antonio Salvio; da Costa Gardolinski, José Eduardo Ferreira; Wypych, Fernando

    2008-04-01

    A zinc hydroxide nitrate (ZHN), Zn5(OH)8(NO3)2.2H2O, and a layered double hydroxide (LDH), Zn/Al-NO3 were doped with 0.2 mol% of Cu2+ during alkaline chemical precipitation. Both compounds were intercalated with adipate ((-)OOC(CH2)4COO(-)), azelate ((-)OOC(CH2)7COO(-)), and benzoate (C6H5COO(-)) ions through ion exchange reactions. Solid state 13C nuclear magnetic resonance spectroscopy showed only one signal of carboxylic carbon for adipate and azelate intercalated into LDH, indicating that the carboxylic ends of both acids were equivalent, whereas the signal split when the intercalation was into the ZHN matrix. The electron paramagnetic resonance (EPR) spectrum of copper in octahedral cation sites of LDH layers showed a Hamiltonian parameter ratio g ||/A ||=170 cm and, after intercalation of adipate, the change was not significant: g ||/A ||=174 cm. This result indicates that the carboxylate ions did not coordinate with copper centers. Nonetheless, the intercalation of azelate increased the ratio to g ||/A ||=194 cm, similar to the spectra of ZHN modified with adipate, g ||/A ||=199 cm, and azelate, g ||/A ||=183 and 190 cm, which are associated with the coordination of copper by weak carboxylate anion ligands. Copper occupies octahedral or tetrahedral sites in ZHN layers, and the EPR spectra indicate that the dicarboxylate anions reacted preferentially with octahedral sites, whereas benzoate reacted with both sites.

  2. Cation ordering and superstructures in natural layered double hydroxides.

    Science.gov (United States)

    Krivovichev, Sergey V; Yakovenchuk, Victor N; Zolotarev, Andrey A; Ivanyuk, Gregory N; Pakhomovsky, Yakov A

    2010-01-01

    Layered double hydroxides (LDHs) constitute an important group of materials with many applications ranging from catalysis and absorption to carriers for drug delivery, DNA intercalation and carbon dioxide sequestration. The structures of LDHs are based upon double brucite-like hydroxide layers [M(2+)(n)M(3+)(m)(OH)(2(m+n)](m+), where M(2+) = Mg(2+), Fe(2+), Mn(2+), Zn(2+), etc.; M(3+) = Al(3+), Fe(3+), Cr(3+), Mn(3+), etc. Structural features of LDHs such as cation ordering, charge distribution and polytypism have an immediate influence upon their properties. However, all the structural studies on synthetic LDHs deal with powder samples that prevent elucidation of such fine details of structure architecture as formation of superstructures due to cation ordering. In contrast to synthetic materials, natural LDHs are known to form single crystals accessible to single-crystal X-ray diffraction analysis, which provides a unique possibility to investigate 3D cation ordering in LDHs that results in formation of complex superstructures, where 2D cation order is combined with a specific order of layer stacking (polytypism). Therefore LDH minerals provide an indispensable source of structural information for modeling of structures and processes happening in LDHs at the molecular and nanoscale levels.

  3. Cellular Uptake Behavior of Fluorescein: Intercalated Layered Double Hydroxide

    Science.gov (United States)

    Tanaka, Miyuki; Aisawa, Sumio; Hirahara, Hidetoshi; Narita, Eiichi; Yin, Shu; Sato, Tsugio

    2012-06-01

    In order to define the ability of layered double hydroxide (LDH) as materials for drug delivery, fluorescein (Fluo) anion intercalated LDH (Fluo/LDH) was synthesized by hydrothermal treatment and observed the cellular uptake of the Fluo/LDH for mammalian cell (L929). The synthesized Fluo/LDH showed a LDH structure, high fluorescence and low cytotoxicity. According to the fluorescence, confocal and TEM images of cells, the Fluo/LDH seemed to be internalized into the L929 cell by cellular endocytosis and dissolved inside the cell to exhibit the fluorescence of cellular cytoplasm.

  4. The photoluminescence of Co-Al-layered double hydroxide

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    We report a new optical behaviour of pure Co-Al-layered double hydroxide (LDH). It was found that the Co-Al-LDH sample could emit fluorescence without any fluorescent substances intercalated. Its excitation spectrum shows a maximum peak near the wavelength 370 nm, the maximum emission peak appears at 430 nm and the photoluminescence colour of the Co-Al-LDH sample is blue. This new optical property will be expected to extend the potential applications of LDHs in optical materials field.

  5. LAYERED DOUBLE HYDROXIDES: NANOMATERIALS FOR APPLICATIONS IN AGRICULTURE

    Directory of Open Access Journals (Sweden)

    Luíz Paulo Figueredo Benício

    2015-02-01

    Full Text Available The current research aims to introduce Layered Double Hydroxides (LDH as nanomaterials to be used in agriculture, with particular reference to its use as storage and slow release matrix of nutrients and agrochemicals for plant growing. Structural characteristics, main properties, synthesis methods and characterization of LDH were covered in this study. Moreover, some literature data have been reported to demonstrate their potential for storage and slow release of nitrate, phosphate, agrochemicals, besides as being used as adsorbent for the wastewater treatment. This research aims to expand, in near future, the investigation field on these materials, with application in agriculture, increasing the interface between chemistry and agronomy.

  6. Selectivity of Crystal Growth Direction in Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    赵芸; 梁吉; 李峰; 段雪

    2004-01-01

    Investigation of selectivity of crystal growth direction in layered double hydroxides is helpful to control their particle sizes in different directions. Mg-Al layered double hydroxides (LDHs) were synthesized using a coprecipitation method. The influences of aging temperature, aging time, and Mg/Al molar ratio on the crystal structure, the LDHs particle size, and the selectivity of crystal growth in different directions were investigated. The results show that the size of the crystallites in the a direction is larger than that in the c direction for all experimental conditions, indicating faster crystal growth in the a direction than in the c direction. The crystallite sizes in the a and c directions both increase with decreasing Mg/Al molar ratio but with less difference between the sizes in the two directions. Therefore, the crystal growth rate in the c direction increases more than that in the a direction as the Mg/Al molar ratio decreases. The influence of the aging time, aging temperature, and Mg/Al molar ratio on the selectivity of the crystal growth direction can be used to prepare LDHs with selected sizes in the a and c directions.

  7. Biodiesel synthesis using calcined layered double hydroxide catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Schumaker, J. Link [University of Kentucky; Crofcheck, Czarena [University of Kentucky; TAckett, S. Adam [University of Kentucky; Santillan-Jimenez, Eduardo [University of Kentucky; Morgan, Tonya [University of Kentucky; Ji, Yaying [University of Kentucky; Crocker, Mark [University of Kentucky; Toops, Todd J [ORNL

    2008-01-01

    The catalytic properties of calcined Li-Al, Mg-Al and Mg-Fe layered double hydroxides (LDHs) were examined in two transesterification reactions, namely, the reaction of glyceryl tributyrate with methanol, and the reaction of soybean oil with methanol. While the Li-Al catalysts showed high activity in these reactions at the reflux temperature of methanol, the Mg-Fe and Mg-Al catalysts exhibited much lower methyl ester yields. CO2 TPD measurements revealed the presence of sites of weak, medium and strong basicity on both Mg-Al and Li-Al catalysts, the latter showing higher concentrations of medium and strong base sites; by implication, these are the main sites active in transesterification catalyzed by calcined Li-Al LDHs. Maximum activity was observed for the Li-Al catalysts when a calcination temperature of 450-500 aC was applied, corresponding to decomposition of the layered double hydroxide to the mixed oxide without formation of crystalline lithium aluminate phases.

  8. Ageing behaviour of unary hydroxides in trivalent metal salt solutions: Formation of layered double hydroxide (LDH)-like phases

    Indian Academy of Sciences (India)

    Michael Rajamathi; P Vishnu Kamath

    2000-10-01

    The hydroxides of Mg, Ni, Cu and Zn transform into layered double hydroxide (LDH)-like phases on ageing in solutions of Al or Cr salts. This reaction is similar to acid leaching and proceeds by a dissolution–reprecipitation mechanism offering a simple method of LDH synthesis, with implications for the accepted theories of formation of LDH minerals in the earth’s crust.

  9. Polymerization reaction in restricted space of layered double hydroxides (LDHs)

    Institute of Scientific and Technical Information of China (English)

    SI Lichun; WANG Ge; CAI Fuli; WANG Zhiqiang; DUAN Xue

    2004-01-01

    This paper reported the preparation of styrene sulfonate intercalated layered double hydroxides (LDHs) material, SS-LDHs by coprecipitation method, followed by in-situ polymerization of the monomers in the interlayer space of LDHs. The polymerization reaction was monitored by UV and NMR. It is confirmed that when the reaction occurred at 100℃ for 24 h, part of monomers did not react .When the reaction was carried out at 150℃, the polymeriza tion of the intercalated monomers is complete to afford the polymer intercalated product PSS-LDHs. During the polymerization process, the layered structure remains well. At thesame time the gallery height increases with the lengthening of reaction time. This is preliminarily because that the PSS becomes more swelling with the amount of water it absorbs due to its hygroscopicity property.

  10. Structural characterisation of a layered double hydroxide nanosheet

    Science.gov (United States)

    Funnell, Nicholas P.; Wang, Qiang; Connor, Leigh; Tucker, Matthew G.; O'Hare, Dermot; Goodwin, Andrew L.

    2014-06-01

    We report the atomic-scale structure of a Zn2Al-borate layered double hydroxide (LDH) nanosheet, as determined by reverse Monte Carlo (RMC) modelling of X-ray total scattering data. This study involves the extension of the RMC method to enable structural refinement of two-dimensional nanomaterials. The refined LDH models show the intra-layer geometry in this highly-exfoliated phase to be consistent with that observed in crystalline analogues, with the reciprocal-space scattering data suggesting a disordered arrangement of the Zn2+ and Al3+ cations within the nanosheet. The approach we develop is generalisable and so offers a method of characterising the structures of arbitrary nanosheet phases, including systems that support complex forms of disorder within the nanosheets themselves.We report the atomic-scale structure of a Zn2Al-borate layered double hydroxide (LDH) nanosheet, as determined by reverse Monte Carlo (RMC) modelling of X-ray total scattering data. This study involves the extension of the RMC method to enable structural refinement of two-dimensional nanomaterials. The refined LDH models show the intra-layer geometry in this highly-exfoliated phase to be consistent with that observed in crystalline analogues, with the reciprocal-space scattering data suggesting a disordered arrangement of the Zn2+ and Al3+ cations within the nanosheet. The approach we develop is generalisable and so offers a method of characterising the structures of arbitrary nanosheet phases, including systems that support complex forms of disorder within the nanosheets themselves. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr01265h

  11. Target delivery and controlled release of the chemopreventive drug sulindac by using an advanced layered double hydroxide nanomatrix formulation system.

    Science.gov (United States)

    Minagawa, Keiji; Berber, Mohamed R; Hafez, Inas H; Mori, Takeshi; Tanaka, Masami

    2012-04-01

    Target delivery and controlled release of the chemopreventive drug sulindac that possesses low water solubility present a great challenge for its pharmaceutical industry. Here, we offered an advanced nanomatrix formulation system of sulindac based on layered double hydroxide materials. The X-ray analysis and infrared spectroscopy confirmed the incorporation of sulindac into the gallery of the layered double hydroxides. The incorporation ratios of sulindac were recorded to be 45, 31 and 20 for coprecipitation, anion-exchange and reconstruction techniques, respectively. The scanning electron microscopy showed a nanomatrix-structure of ~50 nm. The release studies of sulindac-nanomatrix showed a 96% controlled release at the small intestine solution during 3 h(s), indicating an enhancement in the dissolution profile of sulindac after the matrix formation. The layered structure of the matrix supplied sulindac with a well-ordered structure and a relatively hydrophobic microenvironment that controlled the guest hydrolysis and reactivity during the release process. The laminar structure of layered double hydroxides offered a safe preservation for sulindac against photodecarboxylation, and enhanced the drug thermal stability from 190 to 230° C. The ionic electrostatic interaction of sulindac through its acidic group with layered double hydroxides demolished the gastrointestinal ulceration.

  12. Electronic spectra of anions intercalated in layered double hydroxides

    Indian Academy of Sciences (India)

    S Radha; P Vishnu Kamath

    2013-10-01

    Transition metal complexes intercalated in layered double hydroxides have a different electronic structure as compared to their free state owing to their confinement within the interlayer gallery. UV–Vis absorptions of the intercalated complex anions show a significant shift as compared to their free state. The ligand to metal charge transfer transitions of the ferricyanide anion show a red shift on intercalation. The ferrocyanide ion shows a significant blue shift of – bands due to the increased separation between 2g and g levels on intercalation. MnO$^{-}_{4}$ ion shows a blue shift in its ligand to metal charge transfer transition since the non-bonding 1 level of oxygen from which the transition arises is stabilized.

  13. Biological evaluation of layered double hydroxides as efficient drug vehicles

    Energy Technology Data Exchange (ETDEWEB)

    Li Yan; Liu Dan; Chang Qing; Liu Dandan; Xia Ying; Liu Shuwen; Peng Nanfang; Yang Xu [Hubei Key Laboratory of Genetic Regulation and Integrative Biology, College of Life Science, Huazhong Normal University, Wuhan 430079 (China); Ai Hanhua [College of Physical Science and Technology, Huazhong Normal University, Wuhan 430079 (China); Xi Zhuge, E-mail: yangxu@mail.ccnu.edu.cn [Tianjin Institutes of Health and Environmental Medicine, Tianjin 300050 (China)

    2010-03-12

    Recently there has been a rapid expansion of the development of bioinorganic hybrid systems for safe drug delivery. Layered double hydroxides (LDH), a variety of available inorganic matrix, possess great promise for this purpose. In this study, an oxidative stress biomarker system, including measurement of reactive oxygen species, glutathione content, endogenous nitric oxide, carbonyl content in proteins, DNA strand breaks and DNA-protein crosslinks, was designed to evaluate the biocompatibility of different concentrations of nano-Zn/Al-LDH with a Hela cell line. The drug delivery activity of the LDH-folic-acid complex was also assessed. The resulting data clearly demonstrated that nano-LDH could be applied as a relatively safe drug vehicle with good delivery activity, but with the caveat that the effects of high dosages observed here should not be ignored when attempting to maximize therapeutic activity by increasing LDH concentration.

  14. Hydrothermal Synthesis of Ni/Al Layered Double Hydroxide Nanorods

    Directory of Open Access Journals (Sweden)

    Yun Zhao

    2011-01-01

    Full Text Available Ni/Al layered double hydroxide (LDH nanorods were successfully synthesized by the hydrothermal reaction. The crystal structure of the products was characterized by X-ray diffraction (XRD. The morphology of the products was observed using transmission electron microscopy (TEM and field emission scanning electron microscopy (SEM. The influences of reaction time and pH value on the morphology of the Ni/Al LDHs were investigated. The result showed that the well-crystallized nanorods of Ni/Al LDHs could be obtained when the pH value was about 10.0 with a long reaction time (12–18 h at 180°C.

  15. Layered Double Hydroxide-Based Nanocarriers for Drug Delivery

    Science.gov (United States)

    Bi, Xue; Zhang, Hui; Dou, Liguang

    2014-01-01

    Biocompatible clay materials have attracted particular attention as the efficient drug delivery systems (DDS). In this article, we review developments in the use of layered double hydroxides (LDHs) for controlled drug release and delivery. We show how advances in the ability to synthesize intercalated structures have a significant influence on the development of new applications of these materials. We also show how modification and/or functionalization can lead to new biotechnological and biomedical applications. This review highlights the most recent progresses in research on LDH-based controlled drug delivery systems, focusing mainly on: (i) DDS with cardiovascular drugs as guests; (ii) DDS with anti-inflammatory drugs as guests; and (iii) DDS with anti-cancer drugs as guests. Finally, future prospects for LDH-based drug carriers are also discussed. PMID:24940733

  16. Layered Double Hydroxide-Based Nanocarriers for Drug Delivery

    Directory of Open Access Journals (Sweden)

    Xue Bi

    2014-06-01

    Full Text Available Biocompatible clay materials have attracted particular attention as the efficient drug delivery systems (DDS. In this article, we review developments in the use of layered double hydroxides (LDHs for controlled drug release and delivery. We show how advances in the ability to synthesize intercalated structures have a significant influence on the development of new applications of these materials. We also show how modification and/or functionalization can lead to new biotechnological and biomedical applications. This review highlights the most recent progresses in research on LDH-based controlled drug delivery systems, focusing mainly on: (i DDS with cardiovascular drugs as guests; (ii DDS with anti-inflammatory drugs as guests; and (iii DDS with anti-cancer drugs as guests. Finally, future prospects for LDH-based drug carriers are also discussed.

  17. Layered double hydroxide stability. 2. Formation of Cr(III)-containing layered double hydroxides directly from solution

    Science.gov (United States)

    Boclair, J. W.; Braterman, P. S.; Jiang, J.; Lou, S.; Yarberry, F.

    1999-01-01

    Solutions containing divalent metal [M(II) = Mg2+, Zn2+, Co2+, Ni2+, Mn2+] chlorides and CrCl3 6H2O were titrated with NaOH to yield, for M(II) = Zn, Co, and Ni, hydrotalcite-like layered double hydroxides (LDHs), [[M(II)]1-z[Cr(III)]z(OH)2][Cl]z yH2O, in a single step, without intermediate formation of chromium hydroxide. Analysis of the resultant titration curves yields solubility constants for these compounds. These are in the order Zn < Ni approximately Co, with a clear preference for formation of the phase with z = 1/3. With Mg2+ as chloride, titration gives a mixture of Cr(OH)3 and Mg(OH)2, but the metal sulfates give Mg2Cr(OH)6 1/2(SO4) by a two-step process. Titrimetric and spectroscopic evidence suggests short-range cation order in the one-step LDH systems.

  18. Physical properties of fixed-charge layer double hydroxides

    Science.gov (United States)

    Hines, D. R.; Solin, S. A.; Costantino, Umberto; Nocchetti, Morena

    2000-05-01

    The physical properties of a series of layer double hydroxides (LDH) of the form [(CO3)0.195(1-x)Cl0.39x(H2O)y]:[Zn0.61Al0.39(OH)2], 0layer water molecules form a hydration ring which defines the height of the solvated, nested Cl anion. The water molecules can tilt around their C2v axis such that the height of the solvated Cl ion is a function of the number of molecules forming the hydration ring. The composition dependence of the basal spacing, determined from x-ray-diffraction powder patterns measured as a function of humidity and temperature for these materials, is a function of both the Cl concentration (x) and the number of guest layer water molecules (y). Distinct basal spacing curves are observed for fully hydrated, partially hydrated, and dehydrated materials. At x=1 the Cl end-member material exhibits a change in stacking sequence from a 3R polytype to a 2H polytype upon dehydration. The dehydrated form of this material also exhibits a (3×3)R30° superlattice ordering of the Cl ions. Due to the nesting of the Cl ion and the active nature of the water molecules, the basal spacing vs x curve for the dehydrated materials is the only curve that can be fit by the discrete finite layer rigidity model. The interlayer rigidity parameter for LDH materials has been determined to be p=4.84+/-0.06 indicating that these materials are stiffer than class-II layered solids but not as stiff as class-III layered solids.

  19. Mg/Al Ordering in Layered Double Hydroxides Revealed by Multinuclear NMR Spectroscopy

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Grey, Clare P.; Sideris, Paul J.

    2008-01-01

    The anion- exchange ability of layered double hydroxides ( LDHs) has been exploited to create materials for use in catalysis, drug delivery, and environmental remediation. The specific cation arrangements in the hydroxide layers of hydrotalcite- like LDHs, of general formula Mg1-x2+Alx3+OH2(Anion...

  20. Synthesis of Layered Double Hydroxide Single-Layer Nanosheets in Formamide.

    Science.gov (United States)

    Yu, Jingfang; Liu, Jingjing; Clearfield, Abraham; Sims, Johnathan E; Speiegle, Michael T; Suib, Steven L; Sun, Luyi

    2016-11-21

    Layered double hydroxide (LDH) single-layer nanosheets were synthesized through a single-step process in the presence of formamide. This one-step process is simple, fast, and efficient and thus is potentially viable for large-scale production. Two key factors for the growth of LDH single-layer nanosheets, formamide concentration and LDH layer charge, were investigated thoroughly. A higher formamide concentration and a higher LDH layer charge are favorable for the growth of LDH single-layer nanosheets. The LDH single-layer nanosheets obtained at the premium formamide concentration and LDH layer charge were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and atomic force micrscopy (AFM). Poly(vinyl alcohol) (PVA)/LDH nanocomposite coatings were also prepared. The coated polyethylene terephthalate (PET) and poly(lactic acid) (PLA) films exhibited significantly improved oxygen gas barrier properties thanks to the well-dispersed and -aligned LDH single-layer nanosheets in the coating.

  1. Texture effect of layered double hydroxides on chemisorption of Orange II

    Science.gov (United States)

    Géraud, Erwan; Bouhent, Mustapha; Derriche, Zoubir; Leroux, Fabrice; Prévot, Vanessa; Forano, Claude

    2007-05-01

    The chemisorption properties of hydrotalcite (HT) with novel macroporous properties have been investigated for azo dye, Orange II (O-II), and compared to coprecipitated HT and their calcined derivatives. Adsorption isotherms satisfactorily fit the Langmuir model. Adsorption capacities of the layered double hydroxides (LDH) macroporous structures are very high, particularly for the calcined materials (4.34 mmol/g) compared to standard HT (0.504 mmol/g), showing that accessibility to the LDH layer surface insures better sorptive properties. For both synthetic materials, the calcination/reconstruction process gives rise to highest concentrations of adsorbed O-II and a partial intercalation of O-II molecules in the structure as shown by the expansion of the basal spacing (d=2.4nm). Conversely, the uncalcined HT phases mainly display a surface exchange chemisorption process.

  2. Layered-double-hydroxide-modified electrodes: electroanalytical applications.

    Science.gov (United States)

    Tonelli, Domenica; Scavetta, Erika; Giorgetti, Marco

    2013-01-01

    Two-dimensional inorganic solids, such as layered double hydroxides (LDHs), also defined as anionic clays, have open structures and unique anion-exchange properties which make them very appropriate materials for the immobilization of anions and biomolecules that often bear an overall negative charge. This review aims to describe the important aspects and new developments of electrochemical sensors and biosensors based on LDHs, evidencing the research from our own laboratory and other groups. It is intended to provide an overview of the various types of chemically modified electrodes that have been developed with these 2D layered materials, along with the significant advances made over the last several years. In particular, we report the main methods used for the deposition of LDH films on different substrates, the conductive properties of these materials, the possibility to use them in the development of membranes for potentiometric anion analysis, the early analytical applications of chemically modified electrodes based on the ability of LDHs to preconcentrate redox-active anions and finally the most recent applications exploiting their electrocatalytic properties. Another promising application field of LDHs, when they are employed as host structures for enzymes, is biosensing, which is described considering glucose as an example.

  3. Synthesis and structure refinement of layered double hydroxides of Co, Mg and Ni with Ga

    Indian Academy of Sciences (India)

    G V Manohara; P Vishnu Kamath

    2010-06-01

    Homogeneous precipitation by urea hydrolysis results in the formation of highly ordered layered double hydroxides of divalent metal ions (Co, Mg, Ni) and Ga. Structure refinement shows that these carbonate containing layered hydroxides crystallize with rhombohedral symmetry (space group -3) in the structure of the 31 polytype. An analysis of the structure shows that, coulombic attraction between the layer and interlayer remains invariant in different layered hydroxides, whereas the strength of hydrogen bonding varies. The Ni–Ga LDH has the weakest hydrogen bonding and Co–Ga, the strongest, as reflected by the layer–interlayer oxygen–oxygen distances. The poor polarity of the OH bond in the Ni–Ga hydroxide points to the greater covalency of the (2+}/′3+)-oxygen bond in this compound as opposed to the Co–Ga hydroxide. These observations are supported by IR spectra.

  4. From Zn-Al layered double hydroxide to ZnO nanostructure:Gradually etching by sodium hydroxide

    Institute of Scientific and Technical Information of China (English)

    Gang Qiang Wan; Dong Xiang Li; Chun Fang Li; Jie Xu; Wan Guo Hou

    2012-01-01

    Zn-Al layered double hydroxide (LDH) was used as precursor to produce ZnO nanostructures through dissolution of aluminum hydroxide in caustic soda.The Zn-Al LDH could transform into different nanostructures of ZnO on LDH nanosheets and even pure ZnO nanorods under various NaOH concentration.The formed ZnO nanorods vertically aligned on both LDH sides.UV-vis diverse reflectance spectra show that the obtained ZnO nanorods have a band gap of approximately 3.05 eV.Such ZnO/LDH nanostructures might be used as photocatalyst in the organic pollutant decomposition.

  5. Intercalation of Layered Silicates, Layered Double Hydroxides, and Lead Iodide: Synthesis, Characterization and Properties.

    Science.gov (United States)

    Mehrotra, Vivek

    Layered silicates, layered double hydroxides, and lead iodide are lamellar solids that can incorporate guest species into the galleries between their layers. Various intercalated forms of these layered materials have been synthesized and their properties studied. The dielectric behavior of pristine fluorohectorite, a typical layered silicate, and Zn-Al layered double hydroxide is explained by considering the structural ordering and mobility of the intercalated water molecules, as well as models invoking fractal time processes and fractal structure. Intercalative polymerization of aniline and pyrrole into fluorohectorite leads to a multilayered structure consisting of single polymer chains alternately stacked with the 9.6 A thick silicate layers. The polymer chains are confined to the quasi two-dimensional interlayer space between the rigid host layers. The hybrid films exhibit highly anisotropic properties. The optical, electrical and mechanical behavior is discussed in terms of the molecular confinement of the polymer chains. Ethylenediamine functionalized C _{60} clusters have also been intercalated into fluorohectorite via an ion-exchange procedure. Intercalation results in an improved thermal stability of the functionalized C_{60} clusters. Rutherford backscattering spectrometry has been used to elucidate the mechanism of intercalative ion exchange of silver in muscovite mica, a layered silicate with a layer charge density of 2e per unit cell. It is proposed that ion-exchange progresses by intercalating successive galleries through the edges of the mica layers. Guest-host interactions have been studied in the system aniline-PbI_2. The optical and structural effects of aniline intercalation in lead iodide thin films is discussed. Intercalation leads to a large shift in the optical band gap of PbI_2. The observed change in band gap is not only due to the increased separation between the PbI_2 layers but also because of an electrostatic interaction between the

  6. Enhanced aerobic sludge granulation with layered double hydroxide

    Directory of Open Access Journals (Sweden)

    Jizhi Zhou

    2014-06-01

    Full Text Available Aerobic granular sludge technology has been developed for the biochemical treatment of wastewater in the present study. A fast cultivation of aerobic granular sludge was realized in Sequencing Batch Reactor (SBR, where Mg-Al layered double hydroxide (LDH was used as a carrier for granules growth. In comparison, the sludge particle size with LDH addition was bigger than those without LDH, with more than 50% of compact granular sludge >1.4 mm in size. This indicatestheLDH improved the growth ofthegranular sludge. The frequency of LDH addition had little effect on the granule growth. Moreover, the formation of granules led to the low sludge volume index (SVI and high mixed liquid suspended solids (MLSS in SBR reactor. With the formation of granular sludge, more than 80% of COD was removed in SBR reactor. The high COD removal efficiency of wastewater was observed regardless of various COD loading strength. The results suggest that the growth of granular sludge with LDH as a carrier enhanced the treatment efficiency. Therefore, our results have provided a promising way to prepare the granular sludge for wastewater treatment.

  7. Methotrexate intercalated ZnAl-layered double hydroxide

    Science.gov (United States)

    Chakraborty, Manjusha; Dasgupta, Sudip; Soundrapandian, Chidambaram; Chakraborty, Jui; Ghosh, Swapankumar; Mitra, Manoj K.; Basu, Debabrata

    2011-09-01

    The anticancerous drug methotrexate (MTX) has been intercalated into an ZnAl-layered double hydroxide (LDH) using an anion exchange technique to produce LDH-MTX hybrids having particle sizes in the range of 100-300 nm. X-ray diffraction studies revealed increases in the basal spacings of ZnAl-LDH-MTX hybrid on MTX intercalation. This was corroborated by the transmission electron micrographs, which showed an increase in average interlayer spacing from 8.9 Å in pristine LDH to 21.3 Å in LDH-MTX hybrid. Thermogravimetric analyses showed an increase in the decomposition temperature for the MTX molecule in the LDH-MTX hybrid indicating enhanced thermal stability of the drug molecule in the LDH nanovehicle. The cumulative release profile of MTX from ZnAl-LDH-MTX hybrids in phosphate buffer saline (PBS) at pH 7.4 was successfully sustained for 48 h following Rigter-Peppas model release kinetics via diffusion.

  8. Bionanocomposites based on layered double hydroxides as drug delivery systems

    Science.gov (United States)

    Aranda, Pilar; Alcântara, Ana C. S.; Ribeiro, Ligia N. M.; Darder, Margarita; Ruiz-Hitzky, Eduardo

    2012-10-01

    The present work introduces new biohybrid materials involving layered double hydroxides (LDH) and biopolymers to produce bionanocomposites, able to act as effective drug delivery systems (DDS). Ibuprofen (IBU) and 5-aminosalicylic acid (5-ASA) have been chosen as model drugs, being intercalated in a Mg-Al LDH matrix. On the one side, the LDHIBU intercalation compound prepared by ion-exchange reaction was blended with the biopolymers zein, a highly hydrophobic protein, and alginate, a polysaccharide widely applied for encapsulating drugs. On the other side, the LDH- 5-ASA intercalation compound prepared by co-precipitation was assembled to the polysaccharides chitosan and pectin, which show mucoadhesive properties and resistance to acid pH values, respectively. Characterization of the intercalation compounds and the resulting bionanocomposites was carried out by means of different experimental techniques: X-ray diffraction, infrared spectroscopy, chemical and thermal analysis, as well as optical and scanning electron microscopies. Data on the swelling behavior and drug release under different pH conditions are also reported.

  9. Immobilization of Penicillin G Acylase on Calcined Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    REN Ling-ling; HE Jing; Evans D. G.; DUAN Xue

    2003-01-01

    A hydrotalcite-like Mg2+/Al3+ layered double hydroxide(LDH) material was prepared by means of a modified coprecipitation method involving a rapid mixing step followed by a separate aging process. LDH calcined at 500 ℃, denoted as CLDH, was characterized by XRD, IR and BET surface area measurements. CLDH has a poor crystalline MgO-like structure with a high surface area and porosity. CLDH was used as a support for the immobilization of penicillin G acylase(PGA). The effect of varying the immobilization conditions, such as pH, contact time and the ratio of enzyme to support, on the activity of the immobilized enzyme in the hydrolysis of penicillin G has been studied. It was found that the activity of the immobilized enzyme decreased slightly with decreasing pH and reached a maximum after a contact time of 24 h. The activity of the immobilized enzyme increased with increasing the ratio of enzyme to support. It was found that the adsorption of PGA inhibited the expected reaction of CLDH with an aqueous medium to regenerate a LDH phase. Its original activity(36%) after 15 cycles of reuse of the immobilized enzyme was retained, but no further loss in the activity was observed.

  10. Intercalation and controlled release properties of vitamin C intercalated layered double hydroxide

    Science.gov (United States)

    Gao, Xiaorui; Lei, Lixu; O'Hare, Dermot; Xie, Juan; Gao, Pengran; Chang, Tao

    2013-07-01

    Two drug-inorganic composites involving vitamin C (VC) intercalated in Mg-Al and Mg-Fe layered double hydroxides (LDHs) have been synthesized by the calcination-rehydration (reconstruction) method. Powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), and UV-vis absorption spectroscopy indicate a successful intercalation of VC into the interlayer galleries of the LDH host. Studies of VC release from the LDHs in deionised water and in aqueous CO32- solutions imply that Mg3Al-VC LDH is a better controlled release system than Mg3Fe-VC LDH. Analysis of the release profiles using a number of kinetic models suggests a solution-dependent release mechanism, and a diffusion-controlled deintercalation mechanism in deionised water, but an ion exchange process in CO32- solution.

  11. Silver Orthophosphate Immobilized on Flaky Layered Double Hydroxides as the Visible-Light-Driven Photocatalysts

    Directory of Open Access Journals (Sweden)

    Xianlu Cui

    2012-01-01

    Full Text Available Flaky layered double hydroxide (FLDH was prepared by the reconstruction of its oxide in alkali solution. The composites with FLDH/Ag3PO4 mass ratios at 1.6 : 1 and 3 : 1 were fabricated by the coprecipitation method. The powders were characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscope, and UV-vis diffuse reflectance spectroscopy. The results indicated that the well-distributed Ag3PO4 in a fine crystallite size was formed on the surface of FLDH. The photocatalytic activities of the Ag3PO4 immobilized on FLDH were significantly enhanced for the degradation of acid red G under visible light irradiation compared to bare Ag3PO4. The composite with the FLDH/Ag3PO4 mass ratio of 3 : 1 showed a higher photocatalytic efficiency.

  12. Development of polymer nanocomposites based on layered double hydroxides

    Directory of Open Access Journals (Sweden)

    Sipusic, J.

    2009-05-01

    Full Text Available Polymeric nanocomposites are commonly considered as systems composed of a polymeric matrix and - usually inorganic - filler. The types of nanofillers are indicated in Fig. 1. Beside wellknown layered silicate fillers, recent attention is attracted to layered double hydroxide fillers (LDH, mainly of synthetic origin. The structure of LDH is based on brucite, or magnesium hydroxide, Mg(OH2 and is illustrated in Fig. 2. The modification of LDHs is commonly done by organic anions, to increase the original interlayer distance and to improve the organophilicity of the filler, keeping in mind their final application as fillers for, usually hydrophobic, polymer matrices. We have used the modified rehydration procedure for preparing organically modified LDH. The stoichiometric quantities of Ca33Al2O6, CaO and benzoic (B (or undecenoic (U acid were mixed with water and some acetone. After long and vigorous shaking, the precipitated fillers were washed, dried and characterized. X-ray diffraction method (XRD has shown the increase of the original interlayer distance for unmodified LDH (OH–-saturated of 0.76 nm to the 1.6 nm in LDH-B or LDH-U fillers (Fig. 3. Infrared spectroscopy method (FTIR has confirmed the incorporation of benzoic anion within the filler layers (Fig. 4. For the preparation of LDH-B and LDH-U composites with polystyrene (PS, poly(methyl methacrylate (PMMA and copolymer (SMMA matrices, a two-step in situ bulk radical polymerization was selected (Table 1 for recipes, azobisisobutyronitrile as initiator, using conventional stirred tank reactor in the first step, and heated mold with the movable wall (Fig. 6 in the second step of polymerization. All the prepared composites with LDH-U fillers were macroscopically phase-separated, as was the PMMA/LDH-B composite.PS/LDH-B and SMMA/LDH-B samples were found to be transparent and were further examined for deduction of their structure (Fig. 5 and thermal properties. FTIR measurements showed that

  13. Layered double hydroxides as containers of inhibitors in organic coatings for corrosion protection of carbon steel

    OpenAIRE

    Hang, To Thi Xuan; Truc, Trinh Anh; Duong, Nguyen Thuy; Pébère, Nadine; Olivier, Marie-Georges

    2012-01-01

    International audience; The present work focuses on the use of layered double hydroxides (LDH) as containers for corrosion inhibitors in an epoxy coating. 2-Benzothiazolylthio-succinic acid (BTSA), used as corrosion inhibitor, was intercalated by co-precipitation in magnesium-aluminum layered double hydroxides. The obtained LDH-BTSA was characterized by infrared spectroscopy, X-ray diffraction and scanning electron microscopy. BTSA release from LDH-BTSA in NaCl solutions was investigated by U...

  14. Mixing Acid Salts and Layered Double Hydroxides in Nanoscale under Solid Condition

    OpenAIRE

    2014-01-01

    The immobilization of potassium sorbate, potassium aspartate and sorbic acid in layered double hydroxide under solid condition was examined. By simply mixing two solids, immobilization of sorbate and aspartate in the interlayer space of nitrate-type layered double hydroxide, so called intercalation reaction, was achieved, and the uptakes, that is, the amount of immobilized salts and the interlayer distances of intercalation compounds were almost the same as those obtained in aqueous solution...

  15. On the dielectric response of complex layered oxides: Mica-type silicates and layered double hydroxides

    Science.gov (United States)

    Mehrotra, Vivek; Giannelis, Emmanuel P.

    1992-08-01

    The dielectric properties of mica-type silicates and layered double hydroxides have been studied in the pristine and various intercalated forms in the frequency range 101-107 Hz. A relaxation peak has been observed for the pristine silicate, whereas the pristine layered double hydroxide exhibits an anomalous low-frequency dispersion. The dielectric response is rationalized in terms of structural ordering and fluctuation of charge carriers as well as models invoking fractal time processes and fractal structure. The response is also related to the structure and mobility of the intercalated water molecules. In both pristine hosts, the predominant conduction mechanism is proton hopping between sites generated by a network of intercalated water molecules. Silicate intercalated with the insulating form of polyaniline exhibits an almost frequency-independent response. In the case of conducting polyaniline intercalated silicate, where polarons are the majority charge carriers, an anomalous low-frequency dispersion is observed and the response is typical of a metal-insulator composite. Finally, impedance measurements have been used to calculate the spatial disorder and/or surface irregularity of the host layers, expressed by the fractal dimension ds. The changes observed in ds upon intercalation of high-charge ions are correlated to the stacking disorder of the host layers.

  16. Large-scale simulations of layered double hydroxide nanocomposite materials

    Science.gov (United States)

    Thyveetil, Mary-Ann

    Layered double hydroxides (LDHs) have the ability to intercalate a multitude of anionic species. Atomistic simulation techniques such as molecular dynamics have provided considerable insight into the behaviour of these materials. We review these techniques and recent algorithmic advances which considerably improve the performance of MD applications. In particular, we discuss how the advent of high performance computing and computational grids has allowed us to explore large scale models with considerable ease. Our simulations have been heavily reliant on computational resources on the UK's NGS (National Grid Service), the US TeraGrid and the Distributed European Infrastructure for Supercomputing Applications (DEISA). In order to utilise computational grids we rely on grid middleware to launch, computationally steer and visualise our simulations. We have integrated the RealityGrid steering library into the Large-scale Atomic/Molecular Massively Parallel Simulator (LAMMPS) 1 . which has enabled us to perform re mote computational steering and visualisation of molecular dynamics simulations on grid infrastruc tures. We also use the Application Hosting Environment (AHE) 2 in order to launch simulations on remote supercomputing resources and we show that data transfer rates between local clusters and super- computing resources can be considerably enhanced by using optically switched networks. We perform large scale molecular dynamics simulations of MgiAl-LDHs intercalated with either chloride ions or a mixture of DNA and chloride ions. The systems exhibit undulatory modes, which are suppressed in smaller scale simulations, caused by the collective thermal motion of atoms in the LDH layers. Thermal undulations provide elastic properties of the system including the bending modulus, Young's moduli and Poisson's ratios. To explore the interaction between LDHs and DNA. we use molecular dynamics techniques to per form simulations of double stranded, linear and plasmid DNA up

  17. A Ni-Fe Layered Double Hydroxide-Carbon Nanotube Complex for Water Oxidation

    CERN Document Server

    Gong, Ming; Wang, Hailiang; Liang, Yongye; Wu, Justin Zachary; Zhou, Jigang; Wang, Jian; Regier, Tom; Wei, Fei; Dai, Hongjie

    2013-01-01

    Highly active, durable and cost-effective electrocatalysts for water oxidation to evolve oxygen gas hold a key to a range of renewable energy solutions including water splitting and rechargeable metal-air batteries. Here, we report the synthesis of ultrathin nickel iron layered double hydroxide nanoplates on mildly oxidized multi-walled carbon nanotubes. Incorporation of Fe into the nickel hydroxide induced the formation of NiFe-layered double hydroxide. The nanoplates were covalently attached to a network of nanotubes, affording excellent electrical wiring to the nanoplates. The ultra-thin Ni-Fe layered double hydroxide nanoplates/carbon nanotube complex was found to exhibit unusually high electro-catalytic activity and stability for oxygen evolution and outperformed commercial precious metal Ir catalysts.

  18. Effect of monobutylether ethylene glycol on Mg/Al layered double hydroxide: a physicochemical and conductivity study

    Energy Technology Data Exchange (ETDEWEB)

    Paulo, Maria Joao [Materiaux et Telecommunications, Institut National de la Rechercher Scientifique - Energie (Canada); Matos, Bruno Ribeiro de [Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP (Brazil); Ntais, Spyridon [Materiaux et Telecommunications, Institut National de la Rechercher Scientifique - Energie (Canada); Coral Fonseca, Fabio [Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP (Brazil); Tavares, Ana C., E-mail: tavares@emt.inrs.ca [Materiaux et Telecommunications, Institut National de la Rechercher Scientifique - Energie (Canada)

    2013-02-15

    Mg-Al hydrotalcite-like compounds with OH{sup -} ions intercalated in the gallery and modified with monobutylether ethylene glycol (mbeeg) were prepared from Mg{sub 6}Al{sub 2}(CO{sub 3})(OH){sub 16}{center_dot}4H{sub 2}O by the reconstruction method. The effect of the ethylene glycol, a moderate surfactant, on the textural properties and on the vapor water sorption of the layered double hydroxides was investigated by transmission electron microscopy and nitrogen and water sorption techniques. The ion conductivity of the samples was measured at 98 % RH up to 180 Degree-Sign C. The compounds are formed by nanoplatelets with a lateral size inferior to 20 nm. The addition of the ethylene glycol was found to increase the specific surface area, total pore volume, and water sorption capacity of the Mg-Al layered double hydroxide. However, it also decreased the average pore diameter, and the ion conductivity of the ethylene glycol modified layered double hydroxide was lower than expected based on the samples' specific surface area and water content.

  19. Effect of monobutylether ethylene glycol on Mg/Al layered double hydroxide: a physicochemical and conductivity study

    Science.gov (United States)

    Paulo, Maria Joao; de Matos, Bruno Ribeiro; Ntais, Spyridon; Fonseca, Fabio Coral; Tavares, Ana C.

    2013-02-01

    Mg-Al hydrotalcite-like compounds with OH- ions intercalated in the gallery and modified with monobutylether ethylene glycol ( mbeeg) were prepared from Mg6Al2(CO3)(OH)16·4H2O by the reconstruction method. The effect of the ethylene glycol, a moderate surfactant, on the textural properties and on the vapor water sorption of the layered double hydroxides was investigated by transmission electron microscopy and nitrogen and water sorption techniques. The ion conductivity of the samples was measured at 98 % RH up to 180 °C. The compounds are formed by nanoplatelets with a lateral size inferior to 20 nm. The addition of the ethylene glycol was found to increase the specific surface area, total pore volume, and water sorption capacity of the Mg-Al layered double hydroxide. However, it also decreased the average pore diameter, and the ion conductivity of the ethylene glycol modified layered double hydroxide was lower than expected based on the samples' specific surface area and water content.

  20. Cu2+ ions as a paramagnetic probe to study the surface chemical modification process of layered double hydroxides and hydroxide salts with nitrate and carboxylate anions.

    Science.gov (United States)

    Arizaga, Gregorio Guadalupe Carbajal; Mangrich, Antonio Salvio; Wypych, Fernando

    2008-04-01

    A layered zinc hydroxide nitrate (Zn5(OH)8(NO3)2.2H2O) and a layered double hydroxide (Zn/Al-NO3) were synthesized by coprecipitation and doped with different amounts of Cu2+ (0.2, 1, and 10 mol%), as paramagnetic probe. Although the literature reports that the nitrate ion is free (with D3h symmetry) between the layers of these two structures, the FTIR spectra of two zinc hydroxide nitrate samples show the C2v symmetry for the nitrate ion, whereas the g ||/A || value in the EPR spectra of Cu2+ is high. This fact suggests bonding of some nitrate ions to the layers of the zinc hydroxide nitrate. The zinc hydroxide nitrate was used as matrix in the intercalation reaction with benzoate, o-chlorobenzoate, and o-iodobenzoate ions. FTIR spectra confirm the ionic exchange reaction and the EPR spectroscopy reveals bonding of the organic ions to the inorganic layers of the zinc hydroxide nitrate, while the layered double hydroxides show only exchange reactions.

  1. Mixing Acid Salts and Layered Double Hydroxides in Nanoscale under Solid Condition

    Directory of Open Access Journals (Sweden)

    Hirokazu Nakayama

    2014-07-01

    Full Text Available The immobilization of potassium sorbate, potassium aspartate and sorbic acid in layered double hydroxide under solid condition was examined. By simply mixing two solids, immobilization of sorbate and aspartate in the interlayer space of nitrate-type layered double hydroxide, so called intercalation reaction, was achieved, and the uptakes, that is, the amount of immobilized salts and the interlayer distances of intercalation compounds were almost the same as those obtained in aqueous solution. However, no intercalation was achieved for sorbic acid. Although intercalation of sorbate and aspartate into chloride-type layered double hydroxide was possible, the uptakes for these intercalation compounds were lower than those obtained using nitrate-type layered double hydroxide. The intercalation under solid condition could be achieved to the same extent as for ion-exchange reaction in aqueous solution, and the reactivity was similar to that observed in aqueous solution. This method will enable the encapsulation of acidic drug in layered double hydroxide as nano level simply by mixing both solids.

  2. Synthesis of Zn–Fe layered double hydroxides via an oxidation process and structural analysis of products

    Energy Technology Data Exchange (ETDEWEB)

    Morimoto, Kazuya, E-mail: kazuya.morimoto@aist.go.jp [Institute for Geo-Resources and Environment, National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8567 (Japan); Tamura, Kenji [Environmental Remediation Materials Unit, National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Anraku, Sohtaro [Graduate School of Engineering, Hokkaido University, Kita 13 Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Sato, Tsutomu [Faculty of Engineering, Hokkaido University, Kita 13 Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Suzuki, Masaya [Institute for Geo-Resources and Environment, National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8567 (Japan); Yamada, Hirohisa [Environmental Remediation Materials Unit, National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

    2015-08-15

    The synthesis of Zn–Fe(III) layered double hydroxides was attempted, employing different pathways using either Fe(II) or Fe(III) species together with Zn as the initial reagents. The product derived from the synthesis employing Fe(II) was found to transition to a Zn–Fe(III) layered double hydroxides phase following oxidation process. In contrast, the product obtained with Fe(III) did not contain a layered double hydroxides phase, but rather consisted of simonkolleite and hydrous ferric oxide. It was determined that the valency of the Fe reagent used in the initial synthesis affected the generation of the layered double hydroxides phase. Fe(II) species have ionic radii and electronegativities similar to those of Zn, and therefore are more likely to form trioctahedral hydroxide layers with Zn species. - Graphical abstract: The synthesis of Zn–Fe(III) layered double hydroxides was attempted, employing different pathways using either Fe(II) or Fe(III) species together with Zn as the initial reagents. - Highlights: • Iron valency affected the generation of Zn–Fe layered double hydroxides. • Zn–Fe layered double hydroxides were successfully synthesized using Fe(II). • Fe(II) species were likely to form trioctahedral hydroxide layers with Zn species.

  3. Antimycobacterial, antimicrobial, and biocompatibility properties of para-aminosalicylic acid with zinc layered hydroxide and Zn/Al layered double hydroxide nanocomposites.

    Science.gov (United States)

    Saifullah, Bullo; El Zowalaty, Mohamed E; Arulselvan, Palanisamy; Fakurazi, Sharida; Webster, Thomas J; Geilich, Benjamin M; Hussein, Mohd Zobir

    2014-01-01

    The treatment of tuberculosis by chemotherapy is complicated due to multiple drug prescriptions, long treatment duration, and adverse side effects. We report here for the first time an in vitro therapeutic effect of nanocomposites based on para-aminosalicylic acid with zinc layered hydroxide (PAS-ZLH) and zinc-aluminum layered double hydroxides (PAS-Zn/Al LDH), against mycobacteria, Gram-positive bacteria, and Gram-negative bacteria. The nanocomposites demonstrated good antimycobacterial activity and were found to be effective in killing Gram-positive and Gram-negative bacteria. A biocompatibility study revealed good biocompatibility of the PAS-ZLH nanocomposites against normal human MRC-5 lung cells. The para-aminosalicylic acid loading was quantified with high-performance liquid chromatography analysis. In summary, the present preliminary in vitro studies are highly encouraging for further in vivo studies of PAS-ZLH and PAS-Zn/Al LDH nanocomposites to treat tuberculosis.

  4. Antimycobacterial, antimicrobial, and biocompatibility properties of para-aminosalicylic acid with zinc layered hydroxide and Zn/Al layered double hydroxide nanocomposites

    Directory of Open Access Journals (Sweden)

    Saifullah B

    2014-07-01

    Full Text Available Bullo Saifullah,1 Mohamed E El Zowalaty,2,3 Palanisamy Arulselvan,2 Sharida Fakurazi,2,4 Thomas J Webster,5,6 Benjamin M Geilich,5 Mohd Zobir Hussein1 1Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA, Universiti Putra Malaysia, Serdang, Selangor, Malaysia; 2Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, Serdang, Selangor, Malaysia; 3Department of Environmental Health, Faculty of Public Health and Tropical Medicine, Jazan University, Jazan, Saudi Arabia; 4Department of Human Anatomy, Faculty of Medicine and Health Science, Universiti Putra Malaysia, Serdang, Selangor, Malaysia; 5Department of Chemical Engineering and Program in Bioengineering, Northeastern University, Boston, MA, USA; 6Center of Excellence for Advanced Materials Research, King Abdulaziz University, Jeddah, Saudi Arabia Abstract: The treatment of tuberculosis by chemotherapy is complicated due to multiple drug prescriptions, long treatment duration, and adverse side effects. We report here for the first time an in vitro therapeutic effect of nanocomposites based on para-aminosalicylic acid with zinc layered hydroxide (PAS-ZLH and zinc-aluminum layered double hydroxides (PAS-Zn/Al LDH, against mycobacteria, Gram-positive bacteria, and Gram-negative bacteria. The nanocomposites demonstrated good antimycobacterial activity and were found to be effective in killing Gram-positive and Gram-negative bacteria. A biocompatibility study revealed good biocompatibility of the PAS-ZLH nanocomposites against normal human MRC-5 lung cells. The para-aminosalicylic acid loading was quantified with high-performance liquid chromatography analysis. In summary, the present preliminary in vitro studies are highly encouraging for further in vivo studies of PAS-ZLH and PAS-Zn/Al LDH nanocomposites to treat tuberculosis.  Keywords: Zn/Al-layered double hydroxides, zinc layered hydroxides, tuberculosis, para

  5. Development of Drug Delivery Systems Based on Layered Hydroxides for Nanomedicine

    Directory of Open Access Journals (Sweden)

    Farahnaz Barahuie

    2014-05-01

    Full Text Available Layered hydroxides (LHs have recently fascinated researchers due to their wide application in various fields. These inorganic nanoparticles, with excellent features as nanocarriers in drug delivery systems, have the potential to play an important role in healthcare. Owing to their outstanding ion-exchange capacity, many organic pharmaceutical drugs have been intercalated into the interlayer galleries of LHs and, consequently, novel nanodrugs or smart drugs may revolutionize in the treatment of diseases. Layered hydroxides, as green nanoreservoirs with sustained drug release and cell targeting properties hold great promise of improving health and prolonging life.

  6. Synthesis and characterization of laurate-intercalated Mg–Al layered double hydroxide prepared by coprecipitation

    DEFF Research Database (Denmark)

    Gerds, Nathalie Christiane; Katiyar, Vimal; Koch, Christian Bender

    2012-01-01

    Effective utilization of layered double hydroxides (LDH) for industrial applications requires the synthesis of pure and well-defined LDH phases. In the present study, dodecanoate (laurate) anions were intercalated into Mg–Al-layered double hydroxide (LDH-C12) by coprecipitation in the presence...... intercalated structure, but we here demonstrate it to be magnesium laurate (Mg-C12). The LDH-C12 compound showed high structural order with a basal spacing of 2.41nm. Fourier-transform IR-spectra confirmed the intercalation of the laurate anions in the interlayer. Transmission electron microscopy showed plate...

  7. Synthesis and Characterization of Layered Double Hydroxides Containing Optically Active Transition Metal Ion

    Science.gov (United States)

    Tyagi, S. B.; Kharkwal, Aneeta; Nitu; Kharkwal, Mamta; Sharma, Raghunandan

    2017-01-01

    The acetate intercalated layered double hydroxides of Zn and Mn, have been synthesized by chimie douce method. The materials were characterized by XRD, TGA, CHN, IR, XPS, SEM-EDX and UV-visible spectroscopy. The photoluminescence properties was also studied. The optical properties of layered hydroxides are active transition metal ion dependent, particularly d1-10 system plays an important role. Simultaneously the role of host - guest orientation has been considered the basis of photoluminescence. Acetate ion can be exchanged with iodide and sulphate ions. The decomposed product resulted the pure phase Mn doped zinc oxide are also reported.

  8. Structure, molecular simulation, and release of aspirin from intercalated Zn-Al-layered double hydroxides.

    Science.gov (United States)

    Meng, Zilin; Li, Xiaowei; Lv, Fengzhu; Zhang, Qian; Chu, Paul K; Zhang, Yihe

    2015-11-01

    Aspirin or acetylsalicylic acid (AA), a non-steroidal anti-inflammatory drug, is intercalated into Zn-Al-layered double hydroxides (ZnAl-LDHs) by co-precipitation and reconstruction methods. The composition, structure, and morphology of the intercalated products as well as their release behavior are determined experimentally and theoretically by Material Studio 5.5. Experimental results disclose the strong interaction between the LDHs sheets and AA in the intercalated ZnAl-LDHs produced by co-precipitation and slow release of AA from the intercalated ZnAl-LDHs in both phosphate buffered saline (PBS) and borate buffered saline (BBS) solutions. The percentage of AA released from the ZnAl-LDHs prepared by both methods in PBS (96.87% and 98.12%) are much more than those in BBS (68.59% and 81.22%) implying that both H4BO4(-) and H2PO4(-) can exchange with AA in the ZnAl-LDHs. After AA is released to PBS, ZnAl-LDHs break into small pieces. The experimental results are explained theoretically based on the calculation of the bonding energy between the anions and LDHs sheets as well as the AlO bond length change in the LDHs sheets. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Superior coagulation of graphene oxides on nanoscale layered double hydroxides and layered double oxides.

    Science.gov (United States)

    Zou, Yidong; Wang, Xiangxue; Chen, Zhongshan; Yao, Wen; Ai, Yuejie; Liu, Yunhai; Hayat, Tasawar; Alsaedi, Ahmed; Alharbi, Njud S; Wang, Xiangke

    2016-12-01

    With the development and application of graphene oxides (GO), the potential toxicity and environmental behavior of GO has become one of the most forefront environmental problems. Herein, a novel nanoscale layered double hydroxides (glycerinum-modified nanocrystallined Mg/Al layered double hydroxides, LDH-Gl), layered double oxides (calcined LDH-Gl, LDO-Gl) and metallic oxide (TiO2) were synthesized and applied as superior coagulants for the efficient removal of GO from aqueous solutions. Coagulation of GO as a function of coagulant contents, pH, ionic strength, GO contents, temperature and co-existing ions were studied and compared, and the results showed that the maximum coagulation capacities of GO were LDO-Gl (448.3 mg g(-1)) > TiO2 (365.7 mg g(-1)) > LDH-Gl (339.1 mg g(-1)) at pH 5.5, which were significantly higher than those of bentonite, Al2O3, CaCl2 or other natural materials due to their stronger reaction active and interfacial effect. The presence of SO3(2-) and HCO3(-) inhibited the coagulation of GO on LDH-Gl and LDO-Gl significantly, while other cations (K(+), Mg(2+), Ca(2+), Ni(2+), Al(3+)) or anion (Cl(-)) had slightly effect on GO coagulation. The interaction mechanism of GO coagulation on LDO-Gl and TiO2 might due to the electrostatic interactions and strong surface complexation, while the main driving force of GO coagulation on LDH-Gl might be attributed to electrostatic interaction and hydrogen bond, which were further evidenced by TEM, SEM, FT-IR and XRD analysis. The results of natural environmental simulation showed that LDO-Gl, TiO2 or other kinds of natural metallic oxides could be superior coagulants for the efficient elimination of GO or other toxic nanomaterials from aqueous solutions in real environmental pollution cleanup.

  10. Hydrothermal Synthesis and Characterization of 3R Polytypes of Mg-Al Layered Double Hydroxides

    NARCIS (Netherlands)

    Budhysutanto, W.N.

    2010-01-01

    Layered Double Hydroxides (LDH) is a unique group of clays that have an anionic exchange capability. This research explored the hydrothermal method as an alternative method to synthesize Mg-Al LDH. It is a simple and more environmentally friendly compared to the conventional method of co-precipitati

  11. Studies on Synthesis and Properties of Mg-Al-nitrate Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A positive Mg-Al-nitrate layered double hydroxides (LDHs) has been synthesized using a non-steady coprccipitation method. The shape, size, chemical composition, electrical property and anion exchange property of the positive nanoparticle were studied by SEM, XRD, FTIR,chemical analysis, spectroanalysis and measuring of electrophoretic mobilities. Preliminary results show the positive nanopartiele is a promising precursor ofpolymer/LDHs nanocomposite.

  12. Formation of nematic liquid crystals of sterically stabilized layered double hydroxide platelets

    NARCIS (Netherlands)

    Mourad, M.C.D.; Devid, E.J.; van Schooneveld, M.M.; Vonk, Ch.; Lekkerkerker, H.N.W.

    2008-01-01

    Colloidal platelets of hydrotalcite, a layered double hydroxide, have been prepared by coprecipitation at pH 11−12 of magnesium nitrate and aluminum nitrate at two different magnesium to aluminum ratios. Changing the temperature and ionic strength during hydrothermal treatment, the platelets were ta

  13. Optimization of layered double hydroxide stability and adsorption capacity for anionic surfactants

    NARCIS (Netherlands)

    Schouten, Natasja; Ham, Louis G.J. van der; Euverink, Gert-Jan W.; Haan, André B. de

    2007-01-01

    Low cost adsorption technology offers high potential to clean up laundry rinsing water. From an earlier selection of adsorbents, layered double hydroxide (LDH) proved to be an interesting material for the removal of anionic surfactant, linear alkyl benzene sulfonate (LAS) which is the main contamina

  14. Glycine buffered synthesis of layered iron(II)-iron(III) hydroxides (green rusts)

    DEFF Research Database (Denmark)

    Yin, Weizhao; Huang, Lizhi; Pedersen, Emil Bjerglund;

    2016-01-01

    Layered Fe(II)-Fe(III) hydroxides (green rusts, GRs) are efficient reducing agents against oxidizing contaminants such as chromate, nitrate, selenite, and nitroaromatic compounds and chlorinated solvents. In this study, we adopted a buffered precipitation approach where glycine (GLY) was used in ...

  15. Optimization of layered double hydroxide stability and adsorption capacity for anionic surfactants

    NARCIS (Netherlands)

    Schouten, Natasja; Ham, van der Louis G.J.; Euverink, Gert-Jan W.; Haan, de André B.

    2007-01-01

    Low cost adsorption technology offers high potential to clean up laundry rinsing water. From an earlier selection of adsorbents (Schouten et al. 2007), layered double hydroxide (LDH) proved to be an interesting material for the removal of anionic surfactant, linear alkyl benzene sulfonate (LAS) whic

  16. Evaluation of layered zinc hydroxide nitrate and zinc/nickel double hydroxide salts in the removal of chromate ions from solutions

    Science.gov (United States)

    de Oliveira, Henrique Bortolaz; Wypych, Fernando

    2016-11-01

    Layered zinc hydroxide nitrate (ZnHN) and Zn/Ni layered double hydroxide salts were synthesized and used to remove chromate ions from solutions at pH 8.0. The materials were characterized by many instrumental techniques before and after chromate ion removal. ZnHN decomposed after contact with the chromate solution, whereas the layered structure of Zn/Ni hydroxide nitrate (Zn/NiHN) and Zn/Ni hydroxide acetate (Zn/NiHA) remained their layers intact after the topotactic anionic exchange reaction, only changing the basal distances. ZnHN, Zn/NiHN, and Zn/NiHA removed 210.1, 144.8, and 170.1 mg of CrO42-/g of material, respectively. Although the removal values obtained for Zn/NiHN and Zn/NiHA were smaller than the values predicted for the ideal formulas of the solids (194.3 and 192.4 mg of CrO42-/g of material, respectively), the measured capacities were higher than the values achieved with many materials reported in the literature. Kinetic experiments showed the removal reaction was fast. To facilitate the solid/liquid separation process after chromium removal, Zn/Ni layered double hydroxide salts with magnetic supports were also synthesized, and their ability to remove chromate was evaluated.

  17. Functionalized layered double hydroxide-based epoxy nanocomposites with improved flame retardancy and mechanical properties

    OpenAIRE

    Ehsan Naderi Kalali; Xin Wanga; De-Yi Wang

    2015-01-01

    Functionalized layered double hydroxides (LDHs) based on a multi-modifier system composed of hydroxypropyl-sulfobutyl-beta-cyclodextrin sodium (sCD), dodecylbenzenesulfonate (DBS) and taurine (T) have been designed and fabricated in this paper, aiming at developing high performance fire retardant epoxy nanocomposites. In this multi-modifier system, sCD was utilized to improve the char yield, DBS was used to enlarge the inter-layer distance of LDH and T was used to enhance the interaction betw...

  18. Understanding surface interactions in aqueous miscible organic solvent treated layered double hydroxides.

    OpenAIRE

    Erastova, Valentina; Degiacomi, Matteo T.; O'Hare, Dermot; Greenwell, H. Chris

    2016-01-01

    Layered materials are of interest for use in a wealth of technological applications, many of which require a high surface area for optimal properties and performance. Recently, an industrially scalable method to create high surface area layered double hydroxide (LDH) materials, which may be readily dispersed in non-polar solvents, has been developed. This method involves treatment of LDHs with aqueous miscible organic (AMO) solvents. Here, molecular modeling is exploited to elucidate the AMO ...

  19. Morphologies, Preparations and Applications of Layered Double Hydroxide Micro-/Nanostructures

    Directory of Open Access Journals (Sweden)

    Mingdong Dong

    2010-12-01

    Full Text Available Layered double hydroxides (LDHs, also well-known as hydrotalcite-like layered clays, have been widely investigated in the fields of catalysts and catalyst support, anion exchanger, electrical and optical functional materials, flame retardants and nanoadditives. This feature article focuses on the progress in micro-/nanostructured LDHs in terms of morphology, and also on the preparations, applications, and perspectives of the LDHs with different morphologies.

  20. Modification of nano-sized layered double hydroxides by long-chain organic aliphatic surfactants

    OpenAIRE

    RAMASAMY ANBARASAN; SEUNG SOON IM; WANDUC LEE

    2008-01-01

    The inter-layer anion of layered double hydroxides (LDH) with a hydrotalcite (HT)-like structure was ion-exchanged with various organic surfactants, particularly with long chain aliphatic surfactants. After the ion-exchange process, the basal spacing of the LDH was increased and the increase of the basal spacing depended on various factors, such as the intercalation capacity functionality and orientation capability of the surfactant. Of the employed surfactants, stearic acid intercalated LDH ...

  1. 双(羟基)金属复合氧化物的表面改性%Surface Modification of Layered Double Hydroxide

    Institute of Scientific and Technical Information of China (English)

    冯春瑶; 矫庆泽; 李蕾; 张春英; 段雪

    2001-01-01

    Mg/Al layered double hydroxide(LDH) was treated with stearic acid by a wet method. The modified double hydroxide showed good dispersion and floatation property with their layer structure being remained almost unchanged.

  2. Effect of the smear layer in the removal of calcium hydroxide from root canal walls

    Directory of Open Access Journals (Sweden)

    Hakan Arslan

    2012-01-01

    Full Text Available Background: The aim of this study was to investigate whether the smear layer influences the removal of calcium hydroxide from the root canal with manual or rotary instruments. Materials and Methods: The root canals of 48 freshly extracted single-rooted maxillary incisors were prepared to apical size 40 (n=40 and finally irrigated with sodium hypochlorite (group A, or ethylene diamine tetra acetic acid (EDTA followed by sodium hypo chlorite (group B. 20 teeth were assigned to each group, while the remaining eight teeth served as positive and negative controls. Each group was divided into two subgroups of 10 teeth (subgroup I - calcium hydroxide was removed with master apical file; subgroup II - with profile file; and, in all removal procedures, citric acid was used for irrigation. The percentage of calcium hydroxide-[Ca(OH [Ca(OH 2 ] coated surface area was calculated by image processing analysis. Results: Considering the root canal as a whole, the removal of Ca(OH 2 from the dentinal walls in group B showed significantly better results (P<0.05 as compared to group A. Conclusions: Under the conditions of this study, it can be concluded that the smear layer is important in the removal of calcium hydroxide.

  3. Anion exchange kinetics of nanodimensional layered metal hydroxides: use of isoconversional analysis.

    Science.gov (United States)

    Majoni, Stephen; Hossenlopp, Jeanne M

    2010-12-16

    Anion exchange reactions of nanodimensional layered metal hydroxide compounds are utilized to create materials with targeted physical and chemical properties and also as a means for controlled release of intercalated anions. The kinetics of this important class of reaction are generally characterized by model-based approaches. In this work, a different approach based on isothermal, isoconversional analysis was utilized to determine effective activation energies with respect to extent of reaction. Two different layered metal hydroxide materials were chosen for reaction with chloride anions, using a temperature range of 30-60 °C. The concentrations of anions released into solution and the changes in polycrystalline solid phases were evaluated using model-based (Avrami-Erofe'ev nucleation-growth model) and model-free (integral isoconversional) methods. The results demonstrate the utility of the isoconversional approach for identifying when fitting to a single model is not appropriate, particularly for characterizing the temperature dependence of the reaction kinetics.

  4. Inclusion of poly-aromatic hydrocarbon (PAH) molecules in a functionalized layered double hydroxide

    Indian Academy of Sciences (India)

    L Mohanambe; S Vasudevan

    2006-01-01

    The internal surface of an Mg-Al layered double hydroxide has been functionalized by anchoring carboxy-methyl derivatized -cyclodextrin cavities to the gallery walls. Neutral polyaromatic hydrocarbon (PAH) molecules have been included within the functionalized solid by driving the hydrophobic aromatic molecules from a polar solvent into the less polar interior of the anchored cyclodextrin cavities by a partitioning process. The optical (absorption and emission) properties of the PAH molecules included within the functionalized Mg-Al layered double hydroxide solid are similar to that of dilute solutions of the PAH in non-polar solvents. The unique feature of these hybrid materials is that they are thermally stable over a wide temperature range with their emission properties practically unaltered.

  5. Strategy for synthesizing quantum dot-layered double hydroxide nanocomposites and their enhanced photoluminescence and photostability.

    Science.gov (United States)

    Cho, Seungho; Jung, Sungwook; Jeong, Sanghwa; Bang, Jiwon; Park, Joonhyuck; Park, Youngrong; Kim, Sungjee

    2013-01-08

    Layered double hydroxide-quantum dot (LDH-QD) composites are synthesized via a room temperature LDH formation reaction in the presence of QDs. InP/ZnS (core/shell) QD, a heavy metal free QD, is used as a model constituent. Interactions between QDs (with negative zeta potentials), decorated with dihydrolipoic acids, and inherently positively charged metal hydroxide layers of LDH during the LDH formations are induced to form the LDH-QD composites. The formation of the LDH-QD composites affords significantly enhanced photoluminescence quantum yields and thermal- and photostabilities compared to their QD counterparts. In addition, the fluorescence from the solid LDH-QD composite preserved the initial optical properties of the QD colloid solution without noticeable deteriorations such as red-shift or deep trap emission. Based on their advantageous optical properties, we also demonstrate the pseudo white light emitting diode, down-converted by the LDH-QD composites.

  6. Synthesis and carbon dioxide sorption of layered double hydroxide/silica foam nanocomposites with hierarchical mesostructure

    KAUST Repository

    Fu, Liling

    2014-03-05

    Layered double hydroxides (LDHs) with a hierarchical mesostructure are successfully synthesized on mesoporous silica foams by simple impregnation and hydrothermal treatment. The as-synthesized LDH/silica foam nanocomposites show well-defined mesostructures with high surface areas, large pore volumes, and mesopores of 6-7 nm. The nanocomposites act as carbon dioxide (CO2) sorbents under simulated flue gas conditions. They also exhibit significantly enhanced CO2 capacities under high-pressure conditions and high CO2/N2 and CO2/CH4 selectivities. Respect the hierarchy: Hierarchical mesoporous layered double hydroxide (LDH) nanocomposites with high surface areas and large pore volumes are synthesized by controlled hydrothermal growth of LDH precursors on a mesoporous silica foam. The as-synthesized nanocomposites exhibit a significantly enhanced capacity and selectivity towards carbon dioxide, making them very promising candidates for carbon dioxide (CO2) separation applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Interaction of pristine hydrotalcite-like layered double hydroxides with CO2: a thermogravimetric study

    Indian Academy of Sciences (India)

    Shivanna Marappa; P Vishnu Kamath

    2015-12-01

    Metal oxides in general have surface acidic sites, but for exceptional circumstances, are not expected to mineralize CO2. Given their intrinsic basicity and an expandable interlayer gallery, the hydrotalcite-like layered double hydroxides (LDHs) are expected to be superior candidate materials for CO2 mineralization. However, the incorporation of Al3+ adversely impacts the ability of the metal hydroxide layer to interact with CO2 in the gas phase in comparison with the unitary Mg(OH)2. Thermogravimetric analysis shows that the decomposition reaction of the [Mg–Al–CO3] LDH is only marginally delayed in flowing CO2 in comparison with flowing N2, showing only an apparent marginal CO2 uptake. Al3+ ion severely attenuates the surface basicity of the LDHs, as the unitary Al(OH)3 is acidic in comparison with Mg(OH)2 and shows little or no interaction with CO2 in the gas phase.

  8. Degradation of l-polylactide during melt processing with layered double hydroxides

    DEFF Research Database (Denmark)

    Gerds, Nathalie; Katiyar, Vimal; Koch, Christian Bender;

    2012-01-01

    PLA was melt compounded in small-scale batches with two forms of laurate-modified magnesium–aluminum layered double hydroxide (Mg-Al-LDH-C12), the corresponding carbonate form (Mg-Al-LDH-CO3) and a series of other additives. Various methods were then adopted to characterize the resulting compounds...... in an effort to gain greater insights into PLA degradation during melt processing. PLA molecular weight reduction was found to vary according to the type of LDH additive. It is considered that the degree of particle dispersion and LDH exfoliation, and hence the accessibility of the hydroxide layer surfaces...... may be active degrading agents. Phosphate treatment of laurate-modified LDH was investigated and this may be a promising way of reducing PLA degradation, thereby making such processes more practically realistic....

  9. Synthesis, sustained release properties of magnetically functionalized organic-inorganic materials: Amoxicillin anions intercalated magnetic layered double hydroxides via calcined precursors at room temperature

    Science.gov (United States)

    Wang, Jun; Liu, Qi; Zhang, Guangchun; Li, Zhanshuang; Yang, Piaoping; Jing, Xiaoyan; Zhang, Milin; Liu, Tianfu; Jiang, Zhaohua

    2009-09-01

    Zinc-aluminum-carbonate-layered double hydroxides (ZnAl-CO 3-LDHs), loaded with magnetic substrates (Fe 3O 4), were prepared for sustained drug-targeting delivery. From the X-ray diffraction results, it was found that the magnetic substrates were successfully incorporated with LDHs and highly dispersed in the hydrotalcite structure. After intercalation with an antibiotic drug (amoxicillin) by using a calcinations-reconstruction method, the basal spacing of layered double hydroxides increased from 7.51 Å to 12.35 Å, indicating that amoxicillin was successfully intercalated into the interlay space of LDHs as a monolayer. Furthermore, in vitro drug release experiments in pH 7.4 phosphate buffer solution (PBS) showed sustained release profiles with amoxicillin as a model drug. Magnetic measurements revealed that the composite possessed paramagnetic properties at room temperature.

  10. Hybrid magnetic materials based on layered double hydroxides: from the chemistry towards the applications

    OpenAIRE

    ABELLÁN SÁEZ, GONZALO

    2014-01-01

    Layered double hydroxides (LDHs) are the leitmotiv of this dissertation. Contradicting the assertion that “any past was better”, LDHs have been continuously revisited from the middle of the twentieth century, and represent an excellent example of the never-ending beauty of Chemistry. New synthetic perspectives are giving a new impetus to LDH chemistry, which among hybrid materials, are finding their heyday. This is resulting in novel materials and also paving the way for new fundamental and p...

  11. Tunable Electronic Transport Properties of 2D Layered Double Hydroxide Crystalline Microsheets with Varied Chemical Compositions.

    Science.gov (United States)

    Zhao, Yibing; Hu, Hai; Yang, Xiaoxia; Yan, Dongpeng; Dai, Qing

    2016-09-01

    Transistors based on layered double hydroxides (LDH) single microcrystal are fabricated, whose conductivity of LDH can be tuned by varying metal cations or interlayer anions, but weakly affected by external electric field. The carrier mobility can reach about 1 × 10(-5) cm(2) V(-1) s(-1) , a value comparable to that of organic C60-based transistors. This work paves a way for future electrical applications of LDH.

  12. Nanotube synthesis from reaction of 4-chloro phenoxy acetate with zinc layered hydroxide

    OpenAIRE

    2015-01-01

    Objective Intercalations of plant growth regulator 4-chloro phenoxy acetate (4CPA) with zinc oxide (ZnO), developed using ZnO-layered hydroxide (ZLH) as host material and 4CPA as a guest. Methods Ion exchange technique via sol-gel method synthesized under aqueous environment, resulted in the formation of inorganic– organic nanotube materials. Results The release of 4CPA from its nanohybrid was found to occur in a controlled manner, governed by pseudo-second order kinetics model...

  13. Preparation of Monodisperse Nanoparticle of Layered Double Hydroxides and Polyoxyethylene Sulfate

    Institute of Scientific and Technical Information of China (English)

    XU Huizhong; QIN Lianjie; ZHANG Hong; YANG Qinzheng; YANG Jing

    2005-01-01

    In order to obtain the bio-molecule/ LDHs nanocomposites having regular crystal structure,three nanocomposites of layered double hydroxides and polyoxyethylene sulfates were prepared by ion-exchange method. TEM analysis reveals that the monodisperse rigid .sphere of approximately 200 nm in diameter could be gotten when the intergallery anion was PEGS-400. Such monodisperse nanoparticle could be used as a promising precursor for preparing bio-molecule/LDHs nanocomposites.

  14. Study of organo-hybrid layered double hydroxides by medium and near infrared spectroscopy

    Science.gov (United States)

    Mora, Manuel; López, M. Isabel; Jiménez-Sanchidrián, César; Ruiz, J. Rafael

    2011-03-01

    An Mg/Al layered double hydroxide (LDH) containing carbonate ion in its interlayer region was examined by medium infrared (MIR) and near infrared reflectance spectroscopy (NIRS). The MIR and NIR spectroscopy techniques was also used to study two organo-hybrid LDHs containing interlayer dodecylbenzenesulphonate (DBS) and dodecylsulphate (DS) ions, respectively. The NIR spectra for the latter solids were found to exhibit the overtone and combination bands for the hydroxyl groups in addition to those typical bands of the organic host functions.

  15. Magnetic behavior of Mg-Al-Zn-Fe mixed oxides from precursors layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Oliva, M.I., E-mail: marcosivanoliva@gmail.com [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina); IFFAM AF (CONICET - FaMAF UNC), M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina); Heredia, A. [CITeQ - Facultad R. Cordoba, Universidad Tecnologica Nacional Maestro Lopez esq. Cruz Roja Argentina, CP 5016 Cordoba (Argentina); Zandalazini, C.I. [Centro Laser de Ciencias Moleculares. INFIQC-FCQ-Grupo de Ciencia de Materiales-FaMAF-Universidad Nacional de Cordoba, Ciudad Universitaria, CP5000 Cordoba, Argentina CONICET (Argentina); Crivello, M. [CITeQ - Facultad R. Cordoba, Universidad Tecnologica Nacional Maestro Lopez esq. Cruz Roja Argentina, CP 5016 Cordoba (Argentina); Corchero, E. [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina)

    2012-08-15

    Mixed oxides of Mg-Al-Zn-Fe were obtained by calcination of layered double hydroxides (LDH) prepared by coprecipitation reaction with hydrothermal treatment. The structural characterization of precursors and oxides was carried out by X rays diffraction, showing increases of ZnO phase with the increase of the zinc content. Magnetic behavior was studied by vibrating sample magnetometer (VSM) and by a superconducting quantum interference device (SQUID) showing both paramagnetic and super paramagnetic behavior depending on both particles size and composition.

  16. Optimization of layered double hydroxide stability and adsorption capacity for anionic surfactants

    OpenAIRE

    2007-01-01

    Low cost adsorption technology offers high potential to clean up laundry rinsing water. From an earlier selection of adsorbents, layered double hydroxide (LDH) proved to be an interesting material for the removal of anionic surfactant, linear alkyl benzene sulfonate (LAS) which is the main contaminant in rinsing water. The main research question was to identify the effect of process parameters of the LDH synthesis on the stability of the LDH structure and the adsorption capacity of LAS. LDH w...

  17. Insights into the Synthesis of Layered Double Hydroxide (LDH) Nanoparticles: Part 2. Formation Mechanisms of LDH

    OpenAIRE

    Sun, Xiaodi; Dey, Sandwip K.

    2015-01-01

    This study demonstrates the effect of (co)intercalated anion compositions on nanostructure evolution to understand the formation mechanisms of layered double hydroxide (LDH) nanoparticles following coprecipitation and hydrothermal treatments (HT). Initially, the room temperature coprecipitation resulted in amorphous primary nanoparticles that agglomerated at the edges due to low surface charge densities. The reversibility of such agglomeration was determined by the crystalline quality upon HT...

  18. Synthesis, characterization, and efficacy of antituberculosis isoniazid zinc aluminum-layered double hydroxide based nanocomposites.

    Science.gov (United States)

    Saifullah, Bullo; El Zowalaty, Mohamed Ezzat; Arulselvan, Palanisamy; Fakurazi, Sharida; Webster, Thomas J; Geilich, Benjamin Mahler; Hussein, Mohd Zobir

    2016-01-01

    The chemotherapy for tuberculosis (TB) is complicated by its long-term treatment, its frequent drug dosing, and the adverse effects of anti-TB drugs. In this study, we have developed two nanocomposites (A and B) by intercalating the anti-TB drug isoniazid (INH) into Zn/Al-layered double hydroxides. The average size of the nanocomposites was found to bê164 nm. The efficacy of the Zn/Al-layered double hydroxides intercalated INH against Mycobacterium tuberculosis was increased by approximately three times more than free INH. The nanocomposites were also found to be active against Gram-positive and -negative bacteria. Compared to the free INH, the nanodelivery formulation was determined to be three times more biocompatible with human normal lung fibroblast MRC-5 cells and 3T3 fibroblast cells at a very high concentration of 50 µg/mL for up to 72 hours. The in vitro release of INH from the Zn/Al-layered double hydroxides was found to be sustained in human body-simulated buffer solutions of pH 4.8 and 7.4. This research is a step forward in making the TB chemotherapy patient friendly.

  19. Toxicity and metabolism of layered double hydroxide intercalated with levodopa in a Parkinson's disease model.

    Science.gov (United States)

    Kura, Aminu Umar; Ain, Nooraini Mohd; Hussein, Mohd Zobir; Fakurazi, Sharida; Hussein-Al-Ali, Samer Hasan

    2014-04-09

    Layered hydroxide nanoparticles are generally biocompatible, and less toxic than most inorganic nanoparticles, making them an acceptable alternative drug delivery system. Due to growing concern over animal welfare and the expense of in vivo experiments both the public and the government are interested to find alternatives to animal testing. The toxicity potential of zinc aluminum layered hydroxide (ZAL) nanocomposite containing anti-Parkinsonian agent may be determined using a PC 12 cell model. ZAL nanocomposite demonstrated a decreased cytotoxic effect when compared to levodopa on PC12 cells with more than 80% cell viability at 100 µg/mL compared to less than 20% cell viability in a direct levodopa exposure. Neither levodopa-loaded nanocomposite nor the un-intercalated nanocomposite disturbed the cytoskeletal structure of the neurogenic cells at their IC50 concentration. Levodopa metabolite (HVA) released from the nanocomposite demonstrated the slow sustained and controlled release character of layered hydroxide nanoparticles unlike the burst uptake and release system shown with pure levodopa treatment.

  20. Corrosion Resistance of the Superhydrophobic Mg(OH)2/Mg-Al Layered Double Hydroxide Coatings on Magnesium Alloys

    National Research Council Canada - National Science Library

    Zhang, Fen; Zhang, Changlei; Zeng, Rongchang; Song, Liang; Guo, Lian; Huang, Xiaowen

    2016-01-01

      Coatings of the Mg(OH)2/Mg-Al layered double hydroxide (LDH) composite were formed by a combined co-precipitation method and hydrothermal process on the AZ31 alloy substrate in alkaline condition...

  1. Cadmium-Aluminum Layered Double Hydroxide Microspheres for Photocatalytic CO2Reduction

    KAUST Repository

    Saliba, Daniel

    2016-03-30

    We report the synthesis of cadmium-aluminum layered double hydroxide (CdAl LDH) using the reaction-diffusion framework. As the hydroxide anions diffuse into an agar gel matrix containing the mixture of aluminum and cadmium salts at a given ratio, they react to give the LDH. The LDH self-assembles inside the pores of the gel matrix into a unique spherical-porous shaped microstructure. The internal and external morphologies of the particles are studied by electron microscopy and tomography revealing interconnected channels and a high surface area. This material is shown to exhibit a promising performance in the photoreduction of carbon dioxide using solar light. Moreover, the palladium-decorated version shows a significant improvement in its reduction potential at room temperature. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Cadmium-Aluminum Layered Double Hydroxide Microspheres for Photocatalytic CO2 Reduction.

    Science.gov (United States)

    Saliba, Daniel; Ezzeddine, Alaa; Sougrat, Rachid; Khashab, Niveen M; Hmadeh, Mohamad; Al-Ghoul, Mazen

    2016-04-21

    We report the synthesis of cadmium-aluminum layered double hydroxide (CdAl LDH) using the reaction-diffusion framework. As the hydroxide anions diffuse into an agar gel matrix containing the mixture of aluminum and cadmium salts at a given ratio, they react to give the LDH. The LDH self-assembles inside the pores of the gel matrix into a unique spherical-porous shaped microstructure. The internal and external morphologies of the particles are studied by electron microscopy and tomography revealing interconnected channels and a high surface area. This material is shown to exhibit a promising performance in the photoreduction of carbon dioxide using solar light. Moreover, the palladium-decorated version shows a significant improvement in its reduction potential at room temperature.

  3. Micrometer-Thick Graphene Oxide-Layered Double Hydroxide Nacre-Inspired Coatings and Their Properties.

    Science.gov (United States)

    Yan, You-Xian; Yao, Hong-Bin; Mao, Li-Bo; Asiri, Abdullah M; Alamry, Khalid A; Marwani, Hadi M; Yu, Shu-Hong

    2016-02-10

    Robust, functional, and flame retardant coatings are attractive in various fields such as building construction, food packaging, electronics encapsulation, and so on. Here, strong, colorful, and fire-retardant micrometer-thick hybrid coatings are reported, which can be constructed via an enhanced layer-by-layer assembly of graphene oxide (GO) nanosheets and layered double hydroxide (LDH) nanoplatelets. The fabricated GO-LDH hybrid coatings show uniform nacre-like layered structures that endow them good mechanic properties with Young's modulus of ≈ 18 GPa and hardness of ≈ 0.68 GPa. In addition, the GO-LDH hybrid coatings exhibit nacre-like iridescence and attractive flame retardancy as well due to their well-defined 2D microstructures. This kind of nacre-inspired GO-LDH hybrid thick coatings will be applied in various fields in future due to their high strength and multifunctionalities.

  4. Mechanochemical synthesis of finite particle of layered double hydroxide-acetate intercalation compound: Swelling, thin film and ion exchange

    Science.gov (United States)

    Kuramoto, Kyoko; Intasa-Ard, Soontaree (Grace); Bureekaew, Sareeya; Ogawa, Makoto

    2017-09-01

    Acetate intercalated Mg-Al layered double hydroxide was successfully synthesized by the solid-state reactions between magnesium acetate and aluminum hydroxide as the starting materials using a planetary mil. The acetate intercalated Mg-Al layered double hydroxide prepared by the present solid-state reaction was finite particle and was processed into stable aqueous suspension with variable transparency and viscosity depending on the concentration. By drying the suspension on a substrate under nitrogen atmosphere, thin film (with the thickness of several micrometers) of the acetate intercalated Mg-Al layered double hydroxide with the basal plane oriented parallel to the substrate was obtained. The ion exchange ability of the film, which is as an advantage of the acetate form of layered double hydroxide, was shown by the ion exchange with coumarin-3-carboxylate to give a photoluminescent film. The solid-solid reaction is advantageous for the preparation of layered double hydroxides due to the simple and eco-friendly nature (no solvent) of the operation, lower possibility of carbonate contamination and finite particles of the products.

  5. Layered double hydroxide intercalated with p-methylbenzoate and p-bromobenzoate: molecular simulations and XRD analysis.

    Science.gov (United States)

    Kovár, Petr; Melánová, Klára; Zima, Vítezslav; Benes, Ludvík; Capková, Pavla

    2008-03-01

    Samples of Mg4Al2 layered double hydroxide (LDH) intercalated with p-methylbenzoate and p-bromobenzoate anions were prepared by reconstruction of calcined LDH. The interlayer arrangement of guests was investigated by molecular modeling combined with X-ray powder diffraction and thermogravimetry. Molecular modeling was carried out in a Cerius2 modeling environment. In both structures the guest anions adopt a nearly perpendicular arrangement of their long axis with respect to the host layers and they are anchored to the OH groups of the layers through COO* groups via electrostatic interactions. Molecular modeling revealed that both structures of the intercalates exhibit a certain disorder of guest anions in the interlayer space. In the case of LDH-p-methylbenzoate intercalate the anions tend to be situated in disordered rows, and the LDH-p-bromobenzoate intercalate exhibits a total disorientation of guest anions. A good agreement between calculated and measured X-ray diffraction patterns and between experimental and calculated basal spacings was obtained. In the LDH-p-methylbenzoate intercalate d exp=16.96 A and d calc=16.97 A, and in the case of LDH-p-bromobenzoate intercalate d exp=17.19 A and d calc=17.40 A.

  6. A chiroptical switch based on DNA/layered double hydroxide ultrathin films.

    Science.gov (United States)

    Shi, Wenying; Jia, Yankun; Xu, Simin; Li, Zhixiong; Fu, Yi; Wei, Min; Shi, Shuxian

    2014-11-04

    A highly oriented film was fabricated by layer-by-layer self-assembly of DNA and MgAl-layered double hydroxide nanosheets, and its application in chiroptical switch was demonstrated via intercalation and deintercalation of an achiral molecule into the DNA cavity. DNA molecules are prone to forming an ordered and dispersive state in the interlayer region of rigid layered double hydroxide (LDH) nanosheets as confirmed by scanning electron microscopy and atomic force microscopy. The induced chiroptical ultrathin film (UTF) is achieved via the intercalation of an achiral chromophore [5,10,15,20-tetrakis(4-N-methylpyridyl)porphine tetra(p-toluenesulfonate) (TMPyP)] into the spiral cavity of DNA stabilized in the LDH matrix [denoted as TMPyP-(DNA/LDH)20]. Fluorescence and circular dichroism spectroscopy are utilized to testify the intercalation of TMPyP into (DNA/LDH)20 UTF that involves two steps: the electrostatic binding of TMPyP onto the surface of (DNA/LDH)20 followed by intercalation into base pairs of DNA. In addition, the TMPyP-(DNA/LDH)20 UTF exhibits good reversibility and repeatability in induced optical chirality, based on the intercalation and deintercalation of TMPyP by alternate exposure to HCl and NH3/H2O vapor, which can be potentially used as a chiroptical switch in data storage.

  7. Synthesis, characterization and application of two-dimensional layered metal hydroxides for environmental remediation purposes

    Science.gov (United States)

    Machingauta, Cleopas

    Two-dimensional layered nano composites, which include layered double hydroxides (LDHs), hydroxy double salts (HDSs) and layered hydroxide salts (LHSs) are able to intercalate different molecular species within their gallery space. These materials have a tunable structural composition which has made them applicable as fire retardants, adsorbents, catalysts, catalyst support materials, and ion exchangers. Thermal treatment of these materials results in destruction of the layers and formation of mixed metal oxides (MMOs) and spinels. MMOs have the ability to adsorb anions from solution and may also regenerate layered structures through a phenomenon known as memory effect. Zinc-nickel hydroxy nitrate was used for the uptake of a series of halogenated acetates (HAs). HAs are pollutants introduced into water systems as by-products of water chlorination and pesticide degradation; their sequestration from water is thus crucial. Optimization of layered materials for controlled uptake requires an understanding of their ion-exchange kinetics and thermodynamics. Exchange kinetics of these anions was monitored using ex-situ PXRD, UV-vis, HPLC and FTIR. It was revealed that exchange rates and uptake efficiencies are related to electronic spatial extents and the charge on carboxyl-oxygen atoms. In addition, acetate and nitrate-based HDSs were used to explore how altering the hydroxide layer affects uptake of acetate/nitrate ions. Changing the metal identities affects the interaction of the anions with the layers. From FTIR, we observed that nitrates coordinate in a D3h and Cs/C 2v symmetry; the nitrates in D3h symmetry were easily exchangeable. Interlayer hydrogen bonding was also revealed to be dependent on metal identity. Substituting divalent cations with trivalent cations produces materials with a higher charge density than HDSs and LHSs. A comparison of the uptake efficiency of zinc-aluminum, zinc-gallium and zinc-nickel hydroxy nitrates was performed using trichloroacetic

  8. Anticancer Drug-Incorporated Layered Double Hydroxide Nanohybrids and Their Enhanced Anticancer Therapeutic Efficacy in Combination Cancer Treatment

    Directory of Open Access Journals (Sweden)

    Tae-Hyun Kim

    2014-01-01

    Full Text Available Objective. Layered double hydroxide (LDH nanoparticles have been studied as cellular delivery carriers for anionic anticancer agents. As MTX and 5-FU are clinically utilized anticancer drugs in combination therapy, we aimed to enhance the therapeutic performance with the help of LDH nanoparticles. Method. Anticancer drugs, MTX and 5-FU, and their combination, were incorporated into LDH by reconstruction method. Simply, LDHs were thermally pretreated at 400°C, and then reacted with drug solution to simultaneously form drug-incorporated LDH. Thus prepared MTX/LDH (ML, 5-FU/LDH (FL, and (MTX + 5-FU/LDH (MFL nanohybrids were characterized by X-ray diffractometer, scanning electron microscopy, infrared spectroscopy, thermal analysis, zeta potential measurement, dynamic light scattering, and so forth. The nanohybrids were administrated to the human cervical adenocarcinoma, HeLa cells, in concentration-dependent manner, comparing with drug itself to verify the enhanced therapeutic efficacy. Conclusion. All the nanohybrids successfully accommodated intended drug molecules in their house-of-card-like structures during reconstruction reaction. It was found that the anticancer efficacy of MFL nanohybrid was higher than other nanohybrids, free drugs, or their mixtures, which means the multidrug-incorporated LDH nanohybrids could be potential drug delivery carriers for efficient cancer treatment via combination therapy.

  9. Synthesis and controlled release properties of 2,4-dichlorophenoxy acetate–zinc layered hydroxide nanohybrid

    Energy Technology Data Exchange (ETDEWEB)

    Bashi, Abbas M., E-mail: abbasmatrood@yahoo.com [Department of Medical Analysis, Faculty of Medical Science, Karbala University (Iraq); Hussein, Mohd Zobir; Zainal, Zulkarnain [Chemistry Department Faculty of Science-UPM (Malaysia); Tichit, Didier [Institut Charles Gerhardt UMR 5253 CNRS/UM2/ENSCM/UM1, Matériaux Avancés pour la Catalyse et la Santé, 8 rue Ecole Normale, 34296 Montpellier Cedex 5 (France)

    2013-07-15

    Direct reaction of ZnO with 2,4-dichlorophenoxyacetic acid (24D) solutions of different concentrations allows obtaining new organic–inorganic nanohybrid materials formed by intercalation of 24D into interlayers of zinc layered hydroxide (ZLH). XRD patterns show a progressive evolution of the structure as 24D concentration increases. The nanohybrid obtained at higher 24D concentration (24D–ZLH(0.4)) reveals a well ordered layered structure with two different basal spacings at 25.2 Å and 24 Å. The FTIR spectrum showing the vibrations bands of the functional groups of 24D and of the ZLH confirms the intercalation. SEM images are in agreement with the structural evolution observed by XRD and reveal the ribbon morphology of the nanohybrids. The release studies of 24D showed a rapid release of 94% for the first 100 min governed by the pseudo-second order kinetic model. - Graphical abstract: The phenomenon indicates that the optical energy gap is enlarged with the increase of molar concentrations in 2,4-dichlorophenoxy acetate anion content into ZnO to create a ZLH–24D nanohybrid. - Highlights: • Nanohybrid was synthesized from 2,4-dichlorophenoxy acetate with-Zinc LHD, using wet chemistry. • Characterized using SEM, TEM, EDX, FTIR, XRD and TGA. • Ribbon-shaped 24D–Zn-layered hydroxide nanoparticles with (003) diffractions of 2.5 nm phase were synthesized.

  10. Chloride adsorption by calcined layered double hydroxides in hardened Portland cement paste

    KAUST Repository

    Yoon, Seyoon

    2014-06-01

    This study investigated the feasibility of using calcined layered double hydroxides (CLDHs) to prevent chloride-induced deterioration in reinforced concrete. CLDHs not only adsorbed chloride ions in aqueous solution with a memory effect but also had a much higher binding capacity than the original layered double hydroxides (LDHs) in the cement matrix. We investigated this adsorption in hardened cement paste in batch cultures to determine adsorption isotherms. The measured and theoretical binding capacities (153 mg g -1 and 257 mg g-1, respectively) of the CLDHs were comparable to the theoretical capacity of Friedel\\'s salt (2 mol mol-1 or 121 mg g-1), which belongs to the LDH family among cementitious phases. We simulated chloride adsorption by CLDHs through the cement matrix using the Fickian model and compared the simulation result to the X-ray fluorescence (XRF) chlorine map. Based on our results, it is proposed that the adsorption process is governed by the chloride transport through the cement matrix; this process differs from that in an aqueous solution. X-ray diffraction (XRD) analysis showed that the CLDH rebuilds the layered structure in a cementitious environment, thereby demonstrating the feasibility of applying CLDHs to the cement and concrete industries. © 2014 Published by Elsevier B.V. All rights reserved.

  11. Mg-Al layered double hydroxide intercalated with porphyrin anions: molecular simulations and experiments.

    Science.gov (United States)

    Kovár, Petr; Pospísil, Miroslav; Káfunková, Eva; Lang, Kamil; Kovanda, Frantisek

    2010-02-01

    Molecular modeling in combination with powder X-ray diffraction (XRD) provided new information on the organization of the interlayer space of Mg-Al layered double hydroxide (LDH) containing intercalated porphyrin anions [5,10,15,20-tetrakis(4-sulfonatophenyl)porphyrin (TPPS)]. Anion-exchange and rehydration procedures were used for the preparation of TPPS-containing LDH with an Mg/Al molar ratio of 2. Molecular modeling was carried out in the Cerius(2) and Materials Studio modeling environment. Three types of models were created in order to simulate the experimental XRD patterns of LDH intercalates with a TPPS loading of 70-80% with respect to the theoretical anion exchange capacity (AEC). The models represent single-phase systems with a 100% TPPS loading in the interlayer space (Type 1) and models represent the coexistence of two phases corresponding to the total exchange from 75 to 92% (Type 2). To cover other possible arrangements, models with the coexistence of both TPPS and NO(3)(-) anions in the same interlayer space were calculated (Type 3). The models are described and compared with experimental data. In all cases, guest TPPS anions are tilted with respect to the hydroxide layers, and are horizontally shifted to each other by up to one-half of the TPPS diameter. According to the energy characteristics and simulated XRD, the most probable arrangement is of Type 2, where some layers are saturated with TPPS anions and others are filled with original NO(3)(-) anions.

  12. Synthesis of layered double hydroxide nanosheets by coprecipitation using a T-type microchannel reactor

    Energy Technology Data Exchange (ETDEWEB)

    Pang, Xiujiang; Sun, Meiyu; Ma, Xiuming [State Key Laboratory Base of Eco-chemical Engineering, College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042 (China); Hou, Wanguo, E-mail: wghou@sdu.edu.cn [Key Laboratory of Colloid and Interface Chemistry (Ministry of Education), Shandong University, Jinan 250100 (China)

    2014-02-15

    The synthesis of Mg{sub 2}Al–NO{sub 3} layered double hydroxide (LDH) nanosheets by coprecipitation using a T-type microchannel reactor is reported. Aqueous LDH nanosheet dispersions were obtained. The LDH nanosheets were characterized by X-ray diffraction, transmission electron microscopy, atomic force microscopy and particle size analysis, and the transmittance and viscosity of LDH nanosheet dispersions were examined. The two-dimensional LDH nanosheets consisted of 1–2 brucite-like layers and were stable for ca. 16 h at room temperature. In addition, the co-assembly between LDH nanosheets and dodecyl sulfate (DS) anions was carried out, and a DS intercalated LDH nanohybrid was obtained. To the best of our knowledge, this is the first report of LDH nanosheets being directly prepared in bulk aqueous solution. This simple, cheap method can provide naked LDH nanosheets in high quantities, which can be used as building blocks for functional materials. - Graphical abstract: Layered double hydroxide (LDH) nanosheets were synthesized by coprecipitation using a T-type microchannel reactor, and could be used as basic building blocks for LDH-based functional materials. Display Omitted - Highlights: • LDH nanosheets were synthesized by coprecipitation using a T-type microchannel reactor. • Naked LDH nanosheets were dispersed in aqueous media. • LDH nanosheets can be used as building blocks for functional materials.

  13. Incorporation of fluorophosphate into zinc–aluminium–nitrate layered double hydroxide by ion exchange

    Indian Academy of Sciences (India)

    El Hassan Elkhattabi; Mohamed Badreddine; Moha Berraho; Ahmed Legrouri

    2012-08-01

    The intercalation of fluorophosphate (PO3F2-, FP) in the [Zn–Al] layered double hydroxides (LDHs) was investigated. A nitrate precursor was prepared by coprecipitaion at pH 9. An attempt to intercalate FP by direct coprecipitation reaction led to a poorly crystalline LDH phase. The effects of pH, aging time and anion concentration were studied and allowed to confirm that the best crystalline material, with high exchange extent, was obtained by carrying out the exchange at 25 °C in 0.1 M FP solution at pH 9 with at least 20 h of aging time.

  14. Mössbauer and XRD study of intercalated CaFe-layered double hydroxides

    Science.gov (United States)

    Sipiczki, Mónika; Kuzmann, Ernő; Pálinkó, István; Homonnay, Zoltán; Sipos, Pál; Kukovecz, Ákos; Kónya, Zoltán

    2014-04-01

    N-containing fully saturated (L-prolinate) or aromatic (indole-2-carboxylate) heterocyclic anions were immobilised in CaFe-layered double hydroxide with the dehydration-rehydration method from aqueous ethanol or acetone. The structure of the resulting organic-inorganic hybrids was characterised mainly with powder X-ray diffraction and 57Fe Mössbauer spectroscopy, and as supplementary analysis scanning electron microscopy, energy dispersive X-ray spectroscopy with elemental mapping and molecular modelling were also applied. It was found that the solvent mixture used for the synthesis caused enormous difference in the interlayer spacings of the obtained inorganic-organic hybrids.

  15. Removal of borate by coprecipitation with Mg/Al layered double hydroxide

    Science.gov (United States)

    Kurashina, Masashi; Inoue, Tatsuki; Tajima, Chihiro; Kanezaki, Eiji

    2015-03-01

    Borate has been used for various industrial products and excessive dose of boron is harmful to humans. We investigated the removal of borate by direct coprecipitation with Mg/Al layered double hydroxide. In this study, the maximum removal of boron was 90% when Mg 30 mmol and Al 15 mmol at pH = 10 were used for 498 mg/l as B. The boron adsorption isotherms could be fitted to Langmuir model. The calculated constant Ws, saturation limit of boron adsorption, is 25 ± 2 mg/g and it is larger than that of ion exchange reaction (Ws = 15±1 mg/g).

  16. Structure and thermal decomposition of sulfated β-cyclodextrin intercalated in a layered double hydroxide

    Science.gov (United States)

    Wang, Ji; Wei, Min; Rao, Guoying; Evans, David G.; Duan, Xue

    2004-01-01

    The sodium salt of hexasulfated β-cyclodextrin has been synthesized and intercalated into a magnesium-aluminum layered double hydroxide by ion exchange. The structure, composition and thermal decomposition behavior of the intercalated material have been studied by variable temperature X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), inductively coupled plasma emission spectroscopy (ICP), and thermal analysis (TG-DTA) and a model for the structure has been proposed. The thermal stability of the intercalated sulfated β-cyclodextrin is significantly enhanced compared with the pure form before intercalation.

  17. Anion-exchange membranes derived from quaternized polysulfone and exfoliated layered double hydroxide for fuel cells

    Science.gov (United States)

    Liu, Wan; Liang, Na; Peng, Pai; Qu, Rong; Chen, Dongzhi; Zhang, Hongwei

    2017-02-01

    Layered double hydroxides (LDH) are prepared by controlling urea assisted homogeneous precipitation conditions. Morphology and crystallinity of LDHs are confirmed by X-ray diffraction and scanning electron microscope. After LDHs are incorporated into quaternized polysulfone membranes, transmission electron microscope is used to observe the exfoliated morphology of LDH sheets in the membranes. The properties of the nanocomposite membranes, including water uptake, swelling ratio, mechanical property and ionic conductivity are investigated. The nanocomposite membrane containing 5% LDH sheets shows more balanced performances, exhibiting an ionic conductivity of 2.36×10-2 S cm-1 at 60 °C.

  18. Thermal Analysis On The Kinetics Of Magnesium-Aluminum Layered Double Hydroxides In Different Heating Rates

    Directory of Open Access Journals (Sweden)

    Hongbo Y.

    2015-06-01

    Full Text Available The thermal decomposition of magnesium-aluminum layered double hydroxides (LDHs was investigated by thermogravimetry analysis and differential scanning calorimetry (DSC methods in argon environment. The influence of heating rates (including 2.5, 5, 10, 15 and 20K/min on the thermal behavior of LDHs was revealed. By the methods of Kissinger and Flynn-Wall-Ozawa, the thermal kinetic parameters of activation energy and pre-exponential factor for the exothermic processes under non-isothermal conditions were calculated using the analysis of corresponding DSC curves.

  19. Preparation of Layered Double Hydroxide-Immobilized Lipase for High Yield and Optically Active (-)-Menthyl butyrate

    Institute of Scientific and Technical Information of China (English)

    Siti; Salhah; Othman; Mahiran; Basri; Mohd.Zobir; Hussein; Mohd; Basyaruddin; Abdul; Rahman; Raja; Noor; Zaliha; Raja; Abdul; Rahman; Abu; Bakar; Salleh; Salina; Mat; Radzi; Azwani; Sofia; Ahmad; Khiar

    2007-01-01

    1 Results Layered Double Hydroxide (LDH) finds extensive usage in the areas of pharmaceutical sciences and catalysis. In this study, a member of the LDH family, Mg/Al-hydrotalcite (HT), or the so-called anionic clay, was prepared at ratio 4 (HT) by co-precipitating through continuous agitation. X-ray diffraction pattern and thermogravimetric analysis of the material indicated that a pure HT had been successfully synthesized. This matrix was then used as support in the immobilization of lipase from Cand...

  20. Preparation and evaluation of PEGylated phospholipid membrane coated layered double hydroxide nanoparticles

    Directory of Open Access Journals (Sweden)

    Mina Yan

    2016-06-01

    Full Text Available The aim of the present study was to develop layered double hydroxide (LDH nanoparticles coated with PEGylated phospholipid membrane. By comparing the size distribution and zeta potential, the weight ratio of LDH to lipid materials which constitute the outside membrane was identified as 2:1. Transmission electron microscopy photographs confirmed the core-shell structure of PEGylated phospholipid membrane coated LDH (PEG-PLDH nanoparticles, and cell cytotoxicity assay showed their good cell viability on Hela and BALB/C-3T3 cells over the concentration range from 0.5 to 50 μg/mL.

  1. Direct decarbonation of micrometer-scale layered double hydroxides without morphology damage

    Institute of Scientific and Technical Information of China (English)

    Kong Li Xu; Guang Ming Chen; Jian Quan Shen

    2012-01-01

    A direct decarbonation route without obvious morphology damage was developed for large micrometer-scale layered double hydroxides (LDHs).First,we synthesized pure,hexagonal-shaped LDHs with lateral dimension of micrometer-size by the recently reported urea hydrolysis method.Then,using HNO3-NaNO3 mixed solution,the obtained LDH with carbonate anions in the interlayer (LDH_CO3) was directly decarbonated to its nitrate form,LDH_NO3,its morphology and particle size were still unchanged.Compared with the recently published two-step decarbonation method,the direct decarbonation reported herein is very convenient.

  2. Cobalt-based layered double hydroxides as oxygen evolving electrocatalysts in neutral electrolyte

    Science.gov (United States)

    Lin, Hong; Zhang, Ye; Wang, Gang; Li, Jian-Bao

    2012-06-01

    Co-M (M= Co, Ni, Fe, Mn) layered double hydroxides (LDHs) were successfully fabricated by a hexamethylenetetramine (HMT) pyrolysis method. Composite electrodes were made using a self-assembly fashion at inorganic/organic surface binder-free and were used to catalyze oxygen evolution reaction. Water oxidation can take place in neutral electrolyte operating with modest overpotential. The doping of other transitional metal cations affords mix valences and thus more intimate electronic interactions for reversible chemisorption of dioxygen molecules. The application of employing LDH materials in water oxidation process bodes well to facilitate future hydrogen utilization.

  3. Preparation and inhibition properties of molybdate intercalated ZnAlCe layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Huajie; Wang, Jihui, E-mail: jhwang@tju.edu.cn; Zhang, Yu; Hu, Wenbin

    2016-09-05

    ZnAlCe layered double hydroxide intercalated by molybdate (ZnAlCe−MoO{sub 4} LDH) was successfully synthesized by using co-precipitation method, and the morphology, structure of ZnAlCe−MoO{sub 4} LDH were observed and characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) techniques. The inhibition behavior of ZnAlCe−MoO{sub 4} LDH for Q235 steel in 3.5%NaCl solution was determined by polarization curves, electrochemical impedance spectroscopy (EIS), inductively coupled plasma mass spectrometer (ICP-MS) and X-ray photoelectron spectrometer (XPS) methods. The results shows that the synthesized ZnAlCe−MoO{sub 4} LDH has a lamellar structure with a particle size of 0.1–2.0 μm, an average thickness of 30 nm, and a basal plane spacing of 0.898 nm. Compared with the addition of ZnAl layered double hydroxide intercalated by nitrate (ZnAl−NO{sub 3} LDH) and ZnAl layered double hydroxide intercalated by molybdate (ZnAl−MoO{sub 4} LDH) in 3.5% NaCl solution, Q235 steel in 3.5%NaCl + ZnAlCe−MoO{sub 4} LDH solution has a lower corrosion current density, larger polarization resistance and a higher inhibition efficiency. The addition of ZnAlCe−MoO{sub 4} LDH will reduce the chloride concentration in 3.5% NaCl solution by the anion exchanged with molybdate, and improve the corrosion resistance of Q235 steel owing to the formation of passive film with the composition of ferrous or iron molybdate and deposition film with zinc and cerium hydroxides. - Highlights: • ZnAlCe−MoO{sub 4} LDH compound was successfully synthesized by co-precipitation method. • ZnAlCe−MoO{sub 4} LDH has a better inhibition effect to Q235 steel in 3.5%NaCl solution. • The Cl{sup −} ions in solution was partially exchanged with MoO{sub 4}{sup 2−} ions in host layers. • The passive film and deposition film were formed by the release of LDH compound.

  4. Zn-Al LAYERED DOUBLE HYDROXIDE PILLARED BY DIFFERENT DICARBOXYLATE ANIONS

    Directory of Open Access Journals (Sweden)

    S. Gago

    2004-12-01

    Full Text Available Zn-Al layered double hydroxides (LDHs intercalated by terephthalate (TPH and biphenyl-4,4'-dicarboxylate (BPH anions have been synthesized by direct co-precipitation from aqueous solution. The Zn/Al ratio in the final materials was 1.8. The products were characterized by powder X-ray diffraction, thermogravimetric analysis, FTIR and FT Raman spectroscopy, and MAS NMR spectroscopy. The basal spacing for the TPH-LDH intercalate was 14.62 Å, indicating that the guest anions stack to form a monolayer with the aromatic rings perpendicular to the host layers. For the LDH intercalate containing BPH anions, a basal spacing of at least 19.2 Å would be expected if the anions adopted an arrangement similar to that for the TPH anions. The observed spacing was 18.24 Å, suggesting that the anions are tilted slightly with respect to the host layers.

  5. Sono-assisted preparation of magnetic magnesium-aluminum layered double hydroxides and their application for removing fluoride.

    Science.gov (United States)

    Chang, Qing; Zhu, Lihua; Luo, Zhihong; Lei, Min; Zhang, Suicheng; Tang, Heqing

    2011-03-01

    A simple ultrasound-assisted co-precipitation method in combination with a calcination treatment was developed to prepare magnetic Mg-Al layered double hydroxides composite as an adsorbent material to remove fluoride ions from aqueous solutions. The application of ultrasound in the preparation process promoted the formation of the hydrotalcite-like phase and drastically shortened the time being required for preparation of the crystalline composite. It was found that the ultrasound irradiation assistance decreased the size of the composite particles and increased the specific surface area, being favorable to the improvement of the adsorption capacity. The composite prepared under the ultrasound irradiation exhibited fairly high maximum adsorption capacity of fluoride (47.7 mg g(-1)), which was 60% higher than that of the composite prepared without the ultrasound irradiation assistance with the same aging time. The thermodynamic and kinetic studies demonstrated that the adsorption of fluoride ions involved the reconstruction of the layered structure in the composite. In addition, the magnetic composite can be effectively and simply separated by using an external magnetic field, and then regenerated by desorption and calcination. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Mesoporous layer-by-layer ordered nanohybrids of layered double hydroxide and layered metal oxide: highly active visible light photocatalysts with improved chemical stability.

    Science.gov (United States)

    Gunjakar, Jayavant L; Kim, Tae Woo; Kim, Hyo Na; Kim, In Young; Hwang, Seong-Ju

    2011-09-28

    Mesoporous layer-by-layer ordered nanohybrids highly active for visible light-induced O(2) generation are synthesized by self-assembly between oppositely charged 2D nanosheets of Zn-Cr-layered double hydroxide (Zn-Cr-LDH) and layered titanium oxide. The layer-by-layer ordering of two kinds of 2D nanosheets is evidenced by powder X-ray diffraction and cross-sectional high resolution-transmission electron microscopy. Upon the interstratification process, the original in-plane atomic arrangements and electronic structures of the component nanosheets remain intact. The obtained heterolayered nanohybrids show a strong absorption of visible light and a remarkably depressed photoluminescence signal, indicating an effective electronic coupling between the two component nanosheets. The self-assembly between 2D inorganic nanosheets leads to the formation of highly porous stacking structure, whose porosity is controllable by changing the ratio of layered titanate/Zn-Cr-LDH. The resultant heterolayered nanohybrids are fairly active for visible light-induced O(2) generation with a rate of ∼1.18 mmol h(-1) g(-1), which is higher than the O(2) production rate (∼0.67 mmol h(-1) g(-1)) by the pristine Zn-Cr-LDH material, that is, one of the most effective visible light photocatalysts for O(2) production, under the same experimental condition. This result highlights an excellent functionality of the Zn-Cr-LDH-layered titanate nanohybrids as efficient visible light active photocatalysts. Of prime interest is that the chemical stability of the Zn-Cr-LDH is significantly improved upon the hybridization, a result of the protection of the LDH lattice by highly stable titanate layer. The present findings clearly demonstrate that the layer-by-layer-ordered assembly between inorganic 2D nanosheets is quite effective not only in improving the photocatalytic activity of the component semiconductors but also in synthesizing novel porous LDH-based hybrid materials with improved chemical

  7. Synthesis of nanocomposite 2-methyl-4-chlorophenoxyacetic acid with layered double hydroxide: physicochemical characterization and controlled release properties

    Energy Technology Data Exchange (ETDEWEB)

    Sarijo, Siti Halimah, E-mail: izaddinizaddin@yahoo.com; Ghazali, Sheikh Ahmad Izaddin Sheikh Mohd [Faculty of Applied Sciences, Universiti Teknologi MARA (Malaysia); Hussein, Mohd Zobir [Universiti Putra Malaysia, Department of Chemistry, Faculty of Science (Malaysia); Sidek, Norizzah Jaafar [Faculty of Applied Sciences, Universiti Teknologi MARA (Malaysia)

    2013-01-15

    A new organic-inorganic hybrid nanocomposite Zn-Al-MCPA-layered double hydroxide (ZAM) was prepared by intercalation of 2-methyl-4-chlorophenoxyacetic acid (MCPA) into Zn-Al-layered double hydroxide (ZAL) at various concentration of MCPA ranging from 0.1 to 0.7 M. The pH of the synthesis was kept constant at 7.5. Well-ordered hybrid nanocomposite was obtained with 0.4 M MCPA with an expansion of basal spacing from 8.9 Angstrom-Sign in the ZAL to 19.7 Angstrom-Sign in the resulting nanocomposite. The FTIR spectra of the nanocomposite show resemblance peaks of the MCPA and Zn-Al-layered double hydroxide indicating the inclusion of MCPA into the layered double hydroxide. The average particle size of ZAL and ZAM in this study was 115 and 128 nm, respectively. Percentage loading of MCPA was found to be 45.0 % (w/w), calculated based on the percentage of carbon in the sample. The release of MCPA into various aqueous solution was found to be dependent to the anion in the aqueous solution in the order of phosphate > sulfate > chloride with the percentage release of 80, 44, and 8%, respectively. This study shows that Zn-Al-layered double hydroxide can be used as a host carrier for herbicide, MCPA, with controlled release capability.

  8. Synthesis of nanocomposite 2-methyl-4-chlorophenoxyacetic acid with layered double hydroxide: physicochemical characterization and controlled release properties

    Science.gov (United States)

    Sarijo, Siti Halimah; Ghazali, Sheikh Ahmad Izaddin Sheikh Mohd; Hussein, Mohd Zobir; Sidek, Norizzah Jaafar

    2013-01-01

    A new organic-inorganic hybrid nanocomposite Zn-Al-MCPA-layered double hydroxide (ZAM) was prepared by intercalation of 2-methyl-4-chlorophenoxyacetic acid (MCPA) into Zn-Al-layered double hydroxide (ZAL) at various concentration of MCPA ranging from 0.1 to 0.7 M. The pH of the synthesis was kept constant at 7.5. Well-ordered hybrid nanocomposite was obtained with 0.4 M MCPA with an expansion of basal spacing from 8.9 Å in the ZAL to 19.7 Å in the resulting nanocomposite. The FTIR spectra of the nanocomposite show resemblance peaks of the MCPA and Zn-Al-layered double hydroxide indicating the inclusion of MCPA into the layered double hydroxide. The average particle size of ZAL and ZAM in this study was 115 and 128 nm, respectively. Percentage loading of MCPA was found to be 45.0 % (w/w), calculated based on the percentage of carbon in the sample. The release of MCPA into various aqueous solution was found to be dependent to the anion in the aqueous solution in the order of phosphate > sulfate > chloride with the percentage release of 80, 44, and 8 %, respectively. This study shows that Zn-Al-layered double hydroxide can be used as a host carrier for herbicide, MCPA, with controlled release capability.

  9. Rare earth and zinc layered hydroxide salts intercalated with the 2-aminobenzoate anion as organic luminescent sensitizer

    Energy Technology Data Exchange (ETDEWEB)

    Cursino, Ana Cristina Trindade, E-mail: anacursino@ufpr.br [CEPESQ – Research Centre of Applied Chemistry, Department of Chemistry, Universidade Federal do Paraná – P.O. Box 19081, 81531-980 Curitiba, PR (Brazil); Rives, Vicente, E-mail: vrives@usal.es [GIR-QUESCAT – Department of Inorganic Chemistry, Universidad de Salamanca, Plaza de la Merced S/N, 37998 Salamanca (Spain); Arizaga, Gregorio Guadalupe Carbajal, E-mail: gregoriocarbajal@yahoo.com.mx [Universidad de Guadalajara, Department of Chemistry, Boulevard Marcelino García Barragán 1421, C.P. 44430 Guadalajara, Jalisco (Mexico); Trujillano, Raquel, E-mail: rakel@usal.es [GIR-QUESCAT – Department of Inorganic Chemistry, Universidad de Salamanca, Plaza de la Merced S/N, 37998 Salamanca (Spain); Wypych, Fernando, E-mail: wypych@ufpr.br [CEPESQ – Research Centre of Applied Chemistry, Department of Chemistry, Universidade Federal do Paraná – P.O. Box 19081, 81531-980 Curitiba, PR (Brazil)

    2015-10-15

    Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The UV absorption ability was improved after intercalation/grafting in relation to that shown by the parent material. - Highlights: • Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide were synthesized. • Intercalated nitrate anions were exchanged by 2-aminobenzoate. • In all the 2-aminobenzoate containing compounds, the grafting reaction was detected. • The UV absorption ability was improved after the exchange reactions. • Rare earth hydroxide salts are potential matrixes to produce luminescent materials. - Abstract: Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The obtained compounds were characterized by powder X-ray diffraction (PXRD), Fourier transform infrared (FTIR) and ultraviolet visible (UV–vis) spectroscopies, fluorescence measurements and thermal analysis (TGA/DTA). The results from FTIR spectroscopy suggest a direct coordination of 2-aminobenzoate to the metal cations of the inorganic layered structure. The organic derivative products from the intercalation reactions absorb a broader range of UV-light in relation to that shown by the parent material; the photoluminescence measurements present a strong violet, blue and green luminescence under UV-light excitation for layered compounds with, Zn, Y and Tb, respectively. Rare earth hydroxide salts (RE-LHS) are potential alternative matrices for the immobilization of organic species to produce luminescent materials.

  10. Oxidation of Dodecanoate Intercalated Iron(II)–Iron(III) Layered Double Hydroxide to Form 2D Iron(III) (Hydr)oxide Layers

    DEFF Research Database (Denmark)

    Huang, Li‐Zhi; Ayala‐Luis, Karina B.; Fang, Liping;

    2013-01-01

    A planar trioctahedral iron(II)–iron(III) hydroxide (green rust, GR) intercalated with dodecanoate (GRC12) has been oxidized by dioxygen to produce the corresponding planar iron(III) (hydr)oxide. The formulae of GRC12 and the final iron(III) product (oxGRC12) were determined to be FeII2.00FeIII1...

  11. Organo-layered double hydroxides composite thin films deposited by laser techniques

    Energy Technology Data Exchange (ETDEWEB)

    Birjega, R. [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., 77125 Bucharest-Magurele (Romania); Vlad, A., E-mail: angela.vlad@gmail.com [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., 77125 Bucharest-Magurele (Romania); Matei, A.; Dumitru, M.; Stokker-Cheregi, F.; Dinescu, M. [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., 77125 Bucharest-Magurele (Romania); Zavoianu, R. [University of Bucharest, Faculty of Chemistry, Department of Chemical Technology and Catalysis, 4-12 Regina Elisabeta Bd., Bucharest 030018 (Romania); Raditoiu, V.; Corobea, M.C. [National R.& D. Institute for Chemistry and Petrochemistry, ICECHIM, 202 Splaiul Independentei Str., CP-35-274, 060021 Bucharest (Romania)

    2016-06-30

    Highlights: • PLD and MAPLE was successfully used to produce organo-layered double hydroxides. • The organic anions (dodecyl sulfate-DS) were intercalated in co-precipitation step. • Zn2.5Al-LDH (Zn/Al = 2.5) and Zn2.5Al-DS thin films obtained in this work could be suitable for further applications as hydrophobic surfaces. - Abstract: We used laser techniques to create hydrophobic thin films of layered double hydroxides (LDHs) and organo-modified LDHs. A LDH based on Zn-Al with Zn{sup 2+}/Al{sup 3+} ratio of 2.5 was used as host material, while dodecyl sulfate (DS), which is an organic surfactant, acted as guest material. Pulsed laser deposition (PLD) and matrix assisted pulsed laser evaporation (MAPLE) were employed for the growth of the films. The organic anions were intercalated in co-precipitation step. The powders were subsequently used either as materials for MAPLE, or they were pressed and used as targets for PLD. The surface topography of the thin films was investigated by atomic force microscopy (AFM), the crystallographic structure of the powders and films was checked by X-ray diffraction. FTIR spectroscopy was used to evidence DS interlayer intercalation, both for powders and the derived films. Contact angle measurements were performed in order to establish the wettability properties of the as-prepared thin films, in view of functionalization applications as hydrophobic surfaces, owing to the effect of DS intercalation.

  12. Sandwich-like graphene/polypyrrole/layered double hydroxide nanowires for high-performance supercapacitors

    Science.gov (United States)

    Li, Xuejin; Zhang, Yu; Xing, Wei; Li, Li; Xue, Qingzhong; Yan, Zifeng

    2016-11-01

    Electrode design in nanoscale is considered to be ultra-important to construct a superb capacitor. Herein, a sandwich-like composite was made by combining graphene/polypyrrole (GPPY) with nickel-aluminum layered double hydroxide nanowires (NiAl-NWs) via a facile hydrothermal method. This sandwich-like architecture is promising in energy storage applications due to three unique features: (1) the conductive GPPY substrate not only effectively prevents the layered double hydroxides species from aggregating, but also considerably facilitates the electron transmission; (2) the ultrathin NiAl-NWs ensure a maximum exposure of active Ni2+, which can improve the efficiency of rapid redox reactions even at high current densities; (3) the sufficient space between anisotropic NiAl-NWs can accommodate a large volume change of the nanowires to avoid their collapse or distortion during the reduplicative redox reactions. Keeping all these unique features in mind, when the as-prepared composite was applied to supercapacitors, it presented an enhanced capacitive performance in terms of high specific capacitance (845 F g-1), excellent rate performance (67% retained at 30 A g-1), remarkable cyclic stability (92% maintained after 5000 cycles) and large energy density (40.1 Wh·Kg-1). This accomplishment in the present work inspires an innovative strategy of nanoscale electrode design for high-rate performance supercapacitor electrodes containing pseuducapacitive metal oxide.

  13. Double layered hydroxides as potential anti-cancer drug delivery agents.

    Science.gov (United States)

    Riaz, Ufana; Ashraf, S M

    2013-04-01

    The emergence of nanotechnology has changed the scenario of the medical world by revolutionizing the diagnosis, monitoring and treatment of cancer. This nanotechnology has been proved miraculous in detecting cancer cells, delivering chemotherapeutic agents and monitoring treatment from non-specific to highly targeted killing of tumor cells. In the past few decades, a number of inorganic materials have been investigated such as calcium phosphate, gold, carbon materials, silicon oxide, iron oxide, and layered double hydroxide (LDH) for examining their efficacy in targeting drug delivery. The reason behind the selection of these inorganic materials was their versatile and unique features efficient in drug delivery, such as wide availability, rich surface functionality, good biocompatibility, potential for target delivery, and controlled release of the drug from these inorganic nanomaterials. Although, the drug-LDH hybrids are found to be quite instrumental because of their application as advanced anti-cancer drug delivery systems, there has not been much research on them. This mini review is set to highlight the advancement made in the use of layered double hydroxides (LDHs) as anti-cancer drug delivery agents. Along with the advantages of LDHs as anti-cancer drug delivery agents, the process of interaction of some of the common anti-cancer drugs with LDH has also been discussed.

  14. A study of thermally activated Mg–Fe layered double hydroxides as potential environmental catalysts

    Directory of Open Access Journals (Sweden)

    MILICA S. HADNAĐEV-KOSTIĆ

    2010-09-01

    Full Text Available Layered double hydroxides (LDHs and mixed oxides derived after thermal decomposition of LDHs with different Mg–Fe contents were investigated. These materials were chosen because of the possibility to tailor their various properties, such as ion-exchange capability, redox and acid–base and surface area. Layered double hydroxides, [Mg1-xFex(OH2](CO3x/2×mH2O (where x presents the content of trivalent ions, x = M(III/(M(II + M(III were synthesized using the low supersaturation precipitation method. The influence of different Mg/Fe ratios on the structure and surface properties of the LDH and derived mixed oxides was investigated in correlation to their catalytic properties in the chosen test reaction (Fischer–Tropsch synthesis. It was determined that the presence of active sites in the mixed oxides is influenced by the structural properties of the initial LDH and by the presence of additional Fe phases. Furthermore, a synthesis outside the optimal range for the synthesis of single phase LDHs leads to the formation of metastable, multiphase systems with specific characteristics and active sites.

  15. Preparation and properties of blends composed of lignosulfonated layered double hydroxide/plasticized starch and thermoplastics.

    Science.gov (United States)

    Privas, Edwige; Leroux, Fabrice; Navard, Patrick

    2013-07-01

    Layered double hydroxide prepared with lignosulfonate (LDH/LS) can be easily dispersed down to the nanometric scale in thermoplastic starch, at concentration of 1 up to 4 wt% of LDH/LS. They can thus be used as a bio-based reinforcing agent of thermoplastic starch. Incorporation of LDH/LS in starch must be done using LDH/LS slurry instead of powder on order to avoid secondary particles aggregation, the water of the paste being used as the starch plasticizer. This reinforced starch was used for preparing a starch-polyolefine composite. LDH/LS-starch nanocomposites were mixed in a random terpolymer of ethylene, butyl acrylate (6%) and maleic anhydride (3%) at concentrations of 20 wt% and 40 wt%. With a 20% loading of (1 wt% LDH/LS in thermoplastic starch), the ternary copolymer is partially bio-based while keeping nearly its original processability and mechanical properties and improving oxygen barrier properties. The use of layered double hydroxides is also removing most odours linked to the lignin phase.

  16. Organo/layered double hydroxide nanohybrids used to remove non ionic pesticides.

    Science.gov (United States)

    Chaara, D; Bruna, F; Ulibarri, M A; Draoui, K; Barriga, C; Pavlovic, I

    2011-11-30

    The preparation and characterization of organo/layered double hydroxide nanohybrids with dodecylsulfate and sebacate as interlayer anion were studied in detail. The aim of the modification of the layered double hydroxides (LDHs) was to change the hydrophilic character of the interlayer to hydrophobic to improve the ability of the nanohybrids to adsorb non-ionic pesticides such as alachlor and metolachlor from water. Adsorption tests were conducted on organo/LDHs using variable pH values, contact times and initial pesticide concentrations (adsorption isotherms) in order to identify the optimum conditions for the intended purpose. Adsorbents and adsorption products were characterized several physicochemical techniques. The adsorption test showed that a noticeable increase of the adsorption of the non-ionic herbicides was produced. Based on the results, the organo/LDHs could be good adsorbents to remove alachlor and metolachlor from water. Different organo/LDHs complexes were prepared by a mechanical mixture and by adsorption. The results show that HTSEB-based complex displays controlled release properties that reduce metolachlor leaching in soil columns compared to a technical product and the other formulations. The release was dependent on the nature of the adsorbent used to prepare the complexes. Thus, it can be concluded that organo/LDHs might act as suitable supports for the design of pesticide slow release formulations with the aim of reducing the adverse effects derived from rapid transport losses of the chemical once applied to soils.

  17. Efficient drug delivery using SiO2-layered double hydroxide nanocomposites.

    Science.gov (United States)

    Li, Li; Gu, Zi; Gu, Wenyi; Liu, Jian; Xu, Zhi Ping

    2016-05-15

    MgAl-layered double hydroxide (MgAl-LDH) nanoparticles have great potentials in drug and siRNA delivery. In this work, we used a nanodot-coating strategy to prepare SiO2 dot-coated layered double hydroxide (SiO2@MgAl-LDH) nanocomposites with good dispersibility and controllable size for drug delivery. The optimal SiO2@MgAl-LDH nanocomposite was obtained by adjusting synthetic parameters including the mass ratio of MgAl-LDH to SiO2, the mixing temperature and time. The optimal SiO2@MgAl-LDH nanocomposite was shown to have SiO2 nanodots (10-15nm in diameter) evenly deposited on the surface of MgAl-LDHs (110nm in diameter) with the plate-like morphology and the average hydrodynamic diameter of 170nm. We further employed SiO2@MgAl-LDH nanocomposite as a nanocarrier to deliver methotrexate (MTX), a chemotherapy drug, to the human osteosarcoma cell (U2OS) and found that MTX delivered by SiO2@MgAl-LDH nanocomposite apparently inhibited the U2OS cell growth.

  18. Layered double hydroxide-based nanomaterials as highly efficient catalysts and adsorbents.

    Science.gov (United States)

    Li, Changming; Wei, Min; Evans, David G; Duan, Xue

    2014-11-01

    Layered double hydroxides (LDHs) are a class of anion clays consisting of brucite-like host layers and interlayer anions, which have attracted increasing interest in the fields of catalysis/adsorption. By virtue of the versatility in composition, morphology, and architecture of LDH materials, as well as their unique structural properties (intercalation, topological transformation, and self-assembly with other functional materials), LDHs display great potential in the design and fabrication of nanomaterials applied in photocatalysis, heterogeneous catalysis, and adsorption/separation processes. Taking advantage of the structural merits and various control synthesis strategies of LDHs, the active center structure (e.g., crystal facets, defects, geometric and electronic states, etc.) and macro-nano morphology can be facilely manipulated for specific catalytic/adsorbent processes with largely enhanced performances. In this review, the latest advancements in the design and preparation of LDH-based functional nanomaterials for sustainable development in catalysis and adsorption are summarized.

  19. Atomistic simulation of nanoporous layered double hydroxide materials and their properties. I. Structural modeling

    Science.gov (United States)

    Kim, Nayong; Kim, Yongman; Tsotsis, Theodore T.; Sahimi, Muhammad

    2005-06-01

    An atomistic model of layered double hydroxides, an important class of nanoporous materials, is presented. These materials have wide applications, ranging from adsorbents for gases and liquid ions to nanoporous membranes and catalysts. They consist of two types of metallic cations that are accommodated by a close-packed configuration of OH- and other anions in a positively charged brucitelike layer. Water and various anions are distributed in the interlayer space for charge compensation. A modified form of the consistent-valence force field, together with energy minimization and molecular dynamics simulations, is utilized for developing an atomistic model of the materials. To test the accuracy of the model, we compare the vibrational frequencies, x-ray diffraction patterns, and the basal spacing of the material, computed using the atomistic model, with our experimental data over a wide range of temperature. Good agreement is found between the computed and measured quantities.

  20. Interlayer Structure of Bioactive Molecule, 2-Aminoethanesulfonate, Intercalated into Calcium-Containing Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Tae-Hyun Kim

    2012-01-01

    Full Text Available We have successfully intercalated 2-aminoethanesulfonate, a well-known biomolecule taurine, into calcium-containing layered double hydroxides via optimized solid phase intercalation. According to X-ray diffraction patterns and infrared spectroscopy, it was revealed that the intercalated taurine molecules were each directly coordinated to other calcium cation and arranged in a zig-zag pattern. Scanning electron microscopy showed that the particle size and morphology of the LDHs were not affected by the solid phase intercalation, and the surface of intercalates was covered by organic moieties. From ninhydrin amine detection tests, we confirmed that most of the taurine molecules were well stabilized between the calcium-containing LDH layers.

  1. Modification of nano-sized layered double hydroxides by long-chain organic aliphatic surfactants

    Directory of Open Access Journals (Sweden)

    RAMASAMY ANBARASAN

    2008-03-01

    Full Text Available The inter-layer anion of layered double hydroxides (LDH with a hydrotalcite (HT-like structure was ion-exchanged with various organic surfactants, particularly with long chain aliphatic surfactants. After the ion-exchange process, the basal spacing of the LDH was increased and the increase of the basal spacing depended on various factors, such as the intercalation capacity functionality and orientation capability of the surfactant. Of the employed surfactants, stearic acid intercalated LDH showed the highest increase of the basal spacing, which was confirmed by XRD analysis. FTIR results supported the interaction of the surfactants with the LDH. In addition, an increase in the thermal stability of the dodecanedioic acid intercalated HT was evidenced by the TGA method.

  2. Immobilization of HRP Enzyme on Layered Double Hydroxides for Biosensor Application

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    Zouhair M. Baccar

    2011-01-01

    Full Text Available We present a new biosensor for hydrogen peroxide (H2O2 detection. The biosensor was based on the immobilization of horseradish peroxidase (HRP enzyme on layered double hydroxides- (LDH- modified gold surface. The hydrotalcite LDH (Mg2Al was prepared by coprecipitation in constant pH and in ambient temperature. The immobilization of the peroxidase on layered hybrid materials was realized via electrostatic adsorption autoassembly process. The detection of hydrogen peroxide was successfully observed in PBS buffer with cyclic voltammetry and the chronoamperometry techniques. A limit detection of 9 μM of H2O2 was obtained with a good reproducibility. We investigate the sensitivity of our developed biosensor for H2O2 detection in raw milk.

  3. PREPARATION OF POLY(METHYL METHACRYLATE)/LAYERED DOUBLE HYDROXIDES NANOCOMPOSITES via in situ SOLUTION POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    An exfoliated layered double hydroxides/poly(methyl methacrylate) (LDHs/PMMA) nanocomposite was prepared by in situ solution polymerization of methyl methacrylate (MMA) in the presence of 4-vinylbenzenesulfonate intercalated LDHs(MgAl-VBS LDHs). MgAl-VBS LDHs was prepared by the ion exchange method, and the structure and composition of the MgAl-VBS LDHs were determined by X-ray diffraction (XRD), infrared spectroscopy and elemental analysis. XRD and transmission electron microscopy (TEM) were employed to examine the structure of LDHs/PMMA nanocomposite. It was indicated that the LDHs layers were well exfoliated and dispersed in the PMMA matrix. The grafting of PMMA onto LDHs was confirmed by the extraction result and the weight fraction of grafted PMMA increased as the weight fraction of LDHs in the nanocomposites increased.

  4. Zn-Co layered double hydroxide modified hematite photoanode for enhanced photoelectrochemical water splitting

    Science.gov (United States)

    Xu, Dongyu; Rui, Yichuan; Li, Yaogang; Zhang, Qinghong; Wang, Hongzhi

    2015-12-01

    Zinc-cobalt layered double hydroxide (LDH) was electrodeposited on Ti-doped hematite photoanodes for the first time, and a significant enhanced performance for photoelectrochemical water splitting was demonstrated over the composite photoanodes. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and electrochemical impedance spectroscopy (EIS) were characterized with the resulted photoanodes. With the electrodepositing treatment, the photocurrent density increased from 1.27 mA/cm2 for pristine hematite to 1.73 mA/cm2 for modified materials at 1.23 V vs. RHE (i.e. 36% improvement). The photocurrent improvement is mainly attributed to a suppression of electron-hole recombination and reduced overpotential for water oxidation at the hematite-electrolyte interface due to the formation of Zn-Co LDH layer on hematite.

  5. Synthesis of layered double hydroxide nanosheets by coprecipitation using a T-type microchannel reactor

    Science.gov (United States)

    Pang, Xiujiang; Sun, Meiyu; Ma, Xiuming; Hou, Wanguo

    2014-02-01

    The synthesis of Mg2Al-NO3 layered double hydroxide (LDH) nanosheets by coprecipitation using a T-type microchannel reactor is reported. Aqueous LDH nanosheet dispersions were obtained. The LDH nanosheets were characterized by X-ray diffraction, transmission electron microscopy, atomic force microscopy and particle size analysis, and the transmittance and viscosity of LDH nanosheet dispersions were examined. The two-dimensional LDH nanosheets consisted of 1-2 brucite-like layers and were stable for ca. 16 h at room temperature. In addition, the co-assembly between LDH nanosheets and dodecyl sulfate (DS) anions was carried out, and a DS intercalated LDH nanohybrid was obtained. To the best of our knowledge, this is the first report of LDH nanosheets being directly prepared in bulk aqueous solution. This simple, cheap method can provide naked LDH nanosheets in high quantities, which can be used as building blocks for functional materials.

  6. Chloride adsorption by calcined layered double hydroxides in hardened Portland cement paste

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Seyoon [School of Engineering, Kings College, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Moon, Juhyuk, E-mail: juhyuk.moon@stonybrook.edu [Civil Engineering Program, Department of Mechanical Engineering, State University of New York at Stony Brook, New York 11794 (United States); Bae, Sungchul [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States); Duan, Xiaonan [Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853 (United States); Giannelis, Emmanuel P. [Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853 (United States); Center for Refining and Petrochemicals, The Research Institute, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Monteiro, Paulo M. [Department of Civil and Environmental Engineering, University of California, Berkeley, CA 94720 (United States)

    2014-06-01

    This study investigated the feasibility of using calcined layered double hydroxides (CLDHs) to prevent chloride-induced deterioration in reinforced concrete. CLDHs not only adsorbed chloride ions in aqueous solution with a memory effect but also had a much higher binding capacity than the original layered double hydroxides (LDHs) in the cement matrix. We investigated this adsorption in hardened cement paste in batch cultures to determine adsorption isotherms. The measured and theoretical binding capacities (153 mg g{sup −1} and 257 mg g{sup −1}, respectively) of the CLDHs were comparable to the theoretical capacity of Friedel's salt (2 mol mol{sup −1} or 121 mg g{sup −1}), which belongs to the LDH family among cementitious phases. We simulated chloride adsorption by CLDHs through the cement matrix using the Fickian model and compared the simulation result to the X-ray fluorescence (XRF) chlorine map. Based on our results, it is proposed that the adsorption process is governed by the chloride transport through the cement matrix; this process differs from that in an aqueous solution. X-ray diffraction (XRD) analysis showed that the CLDH rebuilds the layered structure in a cementitious environment, thereby demonstrating the feasibility of applying CLDHs to the cement and concrete industries. - Highlights: • We examine the adsorption equilibrium and kinetics of CLDH in the hydrated cement. • CLDH capacity to bind chloride ions in the hydrated cement paste is determined. • We model chloride adsorption by CLDH through the cement matrix. • CLDH reforms the layered structure with ion adsorption in the cement matrix.

  7. Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

    Science.gov (United States)

    Djebbi, Mohamed Amine; Braiek, Mohamed; Namour, Philippe; Ben Haj Amara, Abdesslem; Jaffrezic-Renault, Nicole

    2016-11-01

    Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However, MgAl LDH shows better performance than ZnAl LDH, due to the presence of magnesium cations in the layers. Following the structural, morphological and electrochemical behavior studies of both synthesized LDHs, the prepared LDH modified electrodes were tested through microbial fuel cell configuration, revealing a remarkable, potential new pathway for high-performance and cost-effective electrode use in electrochemical power devices.

  8. Ultrafast switching of an electrochromic device based on layered double hydroxide/Prussian blue multilayered films

    Science.gov (United States)

    Liu, Xiaoxi; Zhou, Awu; Dou, Yibo; Pan, Ting; Shao, Mingfei; Han, Jingbin; Wei, Min

    2015-10-01

    Electrochromic materials are the most important and essential components in an electrochromic device. Herein, we fabricated high-performance electrochromic films based on exfoliated layered double hydroxide (LDH) nanosheets and Prussian blue (PB) nanoparticles via the layer-by-layer assembly technique. X-ray diffraction and UV-vis absorption spectroscopy indicate a periodic layered structure with uniform and regular growth of (LDH/PB)n ultrathin films (UTFs). The resulting (LDH/PB)n UTF electrodes exhibit electrochromic behavior arising from the reversible K+ ion migration into/out of the PB lattice, which induces a change in the optical properties of the UTFs. Furthermore, an electrochromic device (ECD) based on the (LDH/PB)n-ITO/0.1 M KCl electrolyte/ITO sandwich structure displays superior response properties (0.91/1.21 s for coloration/bleaching), a comparable coloration efficiency (68 cm2 C-1) and satisfactory optical contrast (45% at 700 nm), in comparison with other inorganic material-based ECDs reported previously. Therefore, this work presents a facile and cost-effective strategy to immobilize electrochemically active nanoparticles in a 2D inorganic matrix for potential application in displays, smart windows and optoelectronic devices.Electrochromic materials are the most important and essential components in an electrochromic device. Herein, we fabricated high-performance electrochromic films based on exfoliated layered double hydroxide (LDH) nanosheets and Prussian blue (PB) nanoparticles via the layer-by-layer assembly technique. X-ray diffraction and UV-vis absorption spectroscopy indicate a periodic layered structure with uniform and regular growth of (LDH/PB)n ultrathin films (UTFs). The resulting (LDH/PB)n UTF electrodes exhibit electrochromic behavior arising from the reversible K+ ion migration into/out of the PB lattice, which induces a change in the optical properties of the UTFs. Furthermore, an electrochromic device (ECD) based on the (LDH

  9. Preparation of hydroxide ion conductive KOH–layered double hydroxide electrolytes for an all-solid-state iron–air secondary battery

    Directory of Open Access Journals (Sweden)

    Taku Tsuneishi

    2014-06-01

    Full Text Available Anion conductive solid electrolytes based on Mg–Al layered double hydroxide (LDH were prepared for application in an all-solid-state Fe–air battery. The ionic conductivity and the conducting ion species were evaluated from impedance and electromotive force measurements. The ion conductivity of LDH was markedly enhanced upon addition of KOH. The electromotive force in a water vapor concentration cell was similar to that of an anion-conducting polymer membrane. The KOH–LDH obtained was used as a hydroxide ion conductive electrolyte for all-solid-state Fe–air batteries. The cell performance of the Fe–air batteries was examined using a mixture of KOH–LDH and iron-oxide-supported carbon as the negative electrode.

  10. Double-Shelled Nanocages with Cobalt Hydroxide Inner Shell and Layered Double Hydroxides Outer Shell as High-Efficiency Polysulfide Mediator for Lithium-Sulfur Batteries.

    Science.gov (United States)

    Zhang, Jintao; Hu, Han; Li, Zhen; Lou, Xiong Wen David

    2016-03-14

    Lithium-sulfur (Li-S) batteries have been considered as a promising candidate for next-generation electrochemical energy-storage technologies because of their overwhelming advantages in energy density. Suppression of the polysulfide dissolution while maintaining a high sulfur utilization is the main challenge for Li-S batteries. Here, we have designed and synthesized double-shelled nanocages with two shells of cobalt hydroxide and layered double hydroxides (CH@LDH) as a conceptually new sulfur host for Li-S batteries. Specifically, the hollow CH@LDH polyhedra with complex shell structures not only maximize the advantages of hollow nanostructures for encapsulating a high content of sulfur (75 wt %), but also provide sufficient self-functionalized surfaces for chemically bonding with polysulfides to suppress their outward dissolution. When evaluated as cathode material for Li-S batteries, the CH@LDH/S composite shows a significantly improved electrochemical performance.

  11. Molecular modeling of layered double hydroxide intercalated with benzoate, modeling and experiment.

    Science.gov (United States)

    Kovár, Petr; Pospísil, M; Nocchetti, M; Capková, P; Melánová, Klára

    2007-08-01

    The structure of Zn4Al2 Layered Double Hydroxide intercalated with benzencarboxylate (C6H5COO-) was solved using molecular modeling combined with experiment (X-ray powder diffraction, IR spectroscopy, TG measurements). Molecular modeling revealed the arrangement of guest molecules, layer stacking, water content and water location in the interlayer space of the host structure. Molecular modeling using empirical force field was carried out in Cerius(2) modeling environment. Results of modeling were confronted with experiment that means comparing the calculated and measured diffraction pattern and comparing the calculated water content with the thermogravimetric value. Good agreement has been achieved between calculated and measured basal spacing: d(calc) = 15.3 A and d(exp) = 15.5 A. The number of water molecules per formula unit (6H2O per Zn4Al2(OH)12) obtained by modeling (i.e., corresponding to the energy minimum) agrees with the water content estimated by thermogravimetry. The long axis of guest molecules are almost perpendicular to the LDH layers, anchored to the host layers via COO- groups. Mutual orientation of benzoate ring planes in the interlayer space keeps the parquet arrangement. Water molecules are roughly arranged in planes adjacent to host layers together with COO- groups.

  12. Multilayer films of layered double hydroxide/polyaniline and their ammonia sensing behavior

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Dong-Mei; Guan, Mei-Yu; Xu, Qing-Hong; Guo, Ying, E-mail: guoying@mail.buct.edu.cn

    2013-11-15

    Highlights: • (ZnAl-LDH/PANI){sub n} multilayer films have been fabricated via a layer-by-layer assembly way. • The multilayer films have relatively ordered morphology and controllable thickness. • The multilayer films show extremely high selectivity to ammonia at room temperature. -- Abstract: This paper reports the fabrication of layered double hydroxide (LDH)/conductive polymer multilayer films by alternate assembly of exfoliated ZnAl-LDH nanosheets and polyaniline (PANI) on silicon wafer substrates using the layer-by-layer (LBL) deposition technology. UV–vis absorption spectroscopy indicates a stepwise and regular growth of the (LDH/PANI){sub n} multilayer films upon increasing deposition cycles. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrate that the surfaces of the films are microscopy smooth and uniform with a thickness of 2 nm per bilayer. Furthermore, the resulting (LDH/PANI){sub n} multilayer films possess high selectively response to ammonia at room temperature. The presence of LDH nanosheets plays a critical role on the gas sensing for the pure PANI film has very low response to ammonia. The LBL assembly process based on LDH combines the conducting polymer and nano-inorganic material, which provides opportunities to develop new inorganic–organic films for gas sensing.

  13. Universal biomimetic preparation and immobilization of layered double hydroxide films and adsorption behavior

    Science.gov (United States)

    Zhou, Wei; Zhang, Wenpeng; Chen, Zilin

    2017-01-01

    Preparation and immobilization of layered double hydroxides (LDHs) film onto multiple substrates is important and challenging in functional materials fields by date. In this work, a simple and universal polydopamine (PD)-based layer-by-layer assembly strategy was developed for the immobilization of LDHs film onto surfaces such as polypropylene chip, glass slides and metal coins. The surface of substrates was firstly modified by polydopamine functionalization, and then LDHs film was synthesized via urea method and directly immobilized on the PD layer by in situ growing strategy in one step. The PD layer as well as the final LDHs film was characterized by energy dispersive X-ray spectroscopy, scanning electron microscope, infrared spectroscopy, X-ray diffraction pattern and X-ray photoelectron spectra. It has been demonstrated the formation of the dense and homogeneous nanoscaled LDHs film with 400 nm thickness. Adsorption behavior of the fabricated NiAl-LDHs film toward anionic dyes and pharmaceuticals was further assessed. To demonstrate their extensive application, fast and high efficient adsorption of anionic dyes and pharmaceuticals was achieved by NiAl-LDHs-modified polypropylene centrifugal tube.

  14. Water types and their relaxation behavior in partially rehydrated CaFe-mixed binary oxide obtained from CaFe-layered double hydroxide in the 155-298 K temperature range.

    Science.gov (United States)

    Bugris, Valéria; Haspel, Henrik; Kukovecz, Ákos; Kónya, Zoltán; Sipiczki, Mónika; Sipos, Pál; Pálinkó, István

    2013-10-29

    Heat-treated CaFe-layered double hydroxide samples were equilibrated under conditions of various relative humidities (11%, 43% and 75%). Measurements by FT-IR and dielectric relaxation spectroscopies revealed that partial to full reconstruction of the layered structure took place. Water types taking part in the reconstruction process were identified via dielectric relaxation measurements either at 298 K or on the flash-cooled (to 155 K) samples. The dynamics of water molecules at the various positions was also studied by this method, allowing the flash-cooled samples to warm up to 298 K.

  15. The in vitro sustained release profile and antitumor effect of etoposide-layered double hydroxide nanohybrids

    Directory of Open Access Journals (Sweden)

    Qin LL

    2013-05-01

    Full Text Available Lili Qin,1 Mei Wang,2 Rongrong Zhu,3 Songhui You,1 Ping Zhou,1 Shilong Wang31Department of Physical Education, Tongji University, Shanghai, People's Republic of China; 2Department of Chemistry, Tongji University, Shanghai, People's Republic of China; 3School of Life Science and Technology, Tongji University, Shanghai, People's Republic of ChinaAbstract: Magnesium-aluminum layered double hydroxides intercalated with antitumor drug etoposide (VP16 were prepared for the first time using a two-step procedure. The X-ray powder diffraction data suggested the intercalation of VP16 into layers with the increased basal spacing from 0.84–1.18 nm was successful. Then, it was characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy, thermogravimetry and differential thermal analysis, and transmission electron microscopy. The prepared nanoparticles, VP16-LDH, showed an average diameter of 62.5 nm with a zeta potential of 20.5 mV. Evaluation of the buffering effect of VP16-LDH indicated that the nanohybrids were ideal for administration of the drugs that treat human stomach irritation. The loading amount of intercalated VP16 was 21.94% and possessed a profile of sustained release. The mechanism of VP16-LDH release in the phosphate buffered saline solution at pH 7.4 is likely controlled by the diffusion of VP16 anions from inside to the surface of LDH particles. The in vitro cytotoxicity and antitumor assays indicated that VP16-LDH hybrids were less toxic to GES-1 cells while exhibiting better antitumor efficacy on MKN45 and SGC-7901 cells. These results imply that VP16-LDH is a potential antitumor drug for a broad range of gastric cancer therapeutic applications.Keywords: layered double hydroxides, etoposide, drug delivery, antitumor effect, sustained release

  16. Modular Polyoxometalate-Layered Double Hydroxide Composites as Efficient Oxidative Catalysts.

    Science.gov (United States)

    Chen, Yang; Yao, Zhixiao; Miras, Haralampos N; Song, Yu-Fei

    2015-07-20

    The exploitation of intercalation techniques in the field of two-dimensional layered materials offers unique opportunities for controlling chemical reactions in confined spaces and developing nanocomposites with desired functionality. In this study, the exploitation of the novel and facile "one-pot" anion-exchange method for the functionalization of layered double hydroxides (LDHs) is demonstrated. As a proof-of-concept, we demonstrate the intercalation of a series of polyoxometalate (POM) clusters, Na3[PW12O40]⋅15 H2O (Na3PW12), K6[P2W18O62]⋅14 H2O (K6P2W18), and Na9LaW10O36⋅32 H2O (Na9LaW10) into tris(hydroxymethyl)aminomethane (Tris)-modified layered double hydroxides (LDHs) under ambient conditions without the necessity of degassing CO2. Investigation of the resultant intercalated materials of Tris-LDHs-PW12 (1), Tris-LDH-P2W18 (2), and Tris-LDH-LaW10 (3) for the degradation of methylene blue (MB), rhodamine B (RB) and crystal violet (CV) has been carried out, where Tris-LDH-PW12 reveals the best performance in the presence of H2O2. Additionally, degradation of a mixture of RB, MB and CV by Tris-LDH-PW12 follows the order of CV>MB>RB, which is directly related to the designed accessible area of the interlayer space. Also, the composite can be readily recycled and reused at least ten cycles without measurable decrease of activity.

  17. Accessing the biocompatibility of layered double hydroxide by intramuscular implantation: histological and microcirculation evaluation

    Science.gov (United States)

    Cunha, Vanessa Roberta Rodrigues; de Souza, Rodrigo Barbosa; da Fonseca Martins, Ana Maria Cristina Rebello Pinto; Koh, Ivan Hong Jun; Constantino, Vera Regina Leopoldo

    2016-01-01

    Biocompatibility of layered double hydroxides (LDHs), also known as hydrotalcite-like materials or double metal hydroxides, was investigated by in vivo assays via intramuscular tablets implantation in rat abdominal wall. The tablets were composed by chloride ions intercalated into LDH of magnesium/aluminum (Mg2Al-Cl) and zinc/aluminum (Zn2Al-Cl). The antigenicity and tissue integration capacity of LDHs were assessed histologically after 7 and 28 days post-implantation. No fibrous capsule nearby the LDH was noticed for both materials as well any sign of inflammatory reactions. Sidestream Dark Field imaging, used to monitor in real time the microcirculation in tissues, revealed overall integrity of the microcirculatory network neighboring the tablets, with no blood flow obstruction, bleeding and/or increasing of leukocyte endothelial adhesion. After 28 days Mg2Al-Cl promoted multiple collagen invaginations (mostly collagen type-I) among its fragments while Zn2Al-Cl induced predominantly collagen type–III. This work supports previous results in the literature about LDHs compatibility with living matter, endorsing them as functional materials for biomedical applications. PMID:27480483

  18. A kinetic and mechanistic study into the formation of the Cu-Cr layered double hydroxide.

    Science.gov (United States)

    Williams, Gareth R; Clout, Alexander; Burley, Jonathan C

    2013-06-14

    The formation of the layered double hydroxide [Cu2Cr(OH)6]Cl·yH2O from the reaction between CuO and aqueous CrCl3·6H2O was explored using synchrotron X-ray diffraction and ex situ analyses. The use of hard X-rays permitted time-resolved in situ studies to be performed as the reaction proceeded under a range of conditions. Additional information was obtained from ex situ experiments in which aliquots of the reaction mixture were removed, quenched, and subsequently analysed by laboratory X-ray diffraction, IR, UV-visible, and atomic emission spectroscopies. On the basis of these data, it is proposed that the reaction involves three steps. First, the solid CuO starting material is hydrolysed to give Cu(OH)2 chains, releasing Cu(2+) ions into solution. The Cu hydroxide chains subsequently condense with aqueous Cr(3+) species, Cl(-) ions and water molecules to give a hydrated form of the LDH. This material then extrudes some water to form a phase with a reduced interlayer spacing.

  19. Mechanochemical synthesis of Cu-Al and methyl orange intercalated Cu-Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Qu, Jun, E-mail: forsjun@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); He, Xiaoman; Chen, Min; Hu, Huimin [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Zhang, Qiwu, E-mail: zhangqw@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Liu, Xinzhong [College of Ecological Environment and Urban Construction, Fujian University of Technology, Fuzhou 350118 China (China)

    2017-04-15

    In this study, a mechanochemical route to synthesize a Cu-Al layered double hydroxide (LDH) and a methyl orange (MO) intercalated one (MO-LDH) was introduced, in which basic cupric carbonate (Cu{sub 2}(OH){sub 2}CO{sub 3}) and aluminum hydroxide (Al(OH){sub 3}) with Cu/Al molar ratio at 2/1 was first dry ground for 2 h and then agitated in water or methyl orange solution for another 4 h to obtain the LDH and MO-LDH products without any heating operation. The prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermogravimetry (TG), Differential scanning calorimetry (DSC) and Scanning electron microscopy (SEM). The products showed high crystallinity phase of Cu-Al and MO intercalated Cu-Al LDH with no evident impurities, proving that the craft introduced here was facile and effective. The new idea can be applied in other fields to produce organic-inorganic composites. - Highlights: • A facile mechanochemical route to synthesize Cu-Al and MO intercalated Cu-Al LDH. • The products possesses high crystalline of LDH phase with no impure phases. • The dry milling process induces the element substitution between the raw materials. • The agitation operation helps the grain growth of LDH.

  20. Phosphor Dysprosium-Doped Layered Double Hydroxides Exchanged with Different Organic Functional Groups

    Directory of Open Access Journals (Sweden)

    David Ricardo Martínez Vargas

    2013-01-01

    Full Text Available The layers of a Zn/Al layered double hydroxide (LDH were doped with Dy3+ cations. Among some compositions, the Zn2+ : Al3+ : Dy3+ molar ratio equal to 30 : 9 : 1 presented a single crystalline phase. Organic anions with carboxylic, amino, sulfate, or phosphate functional groups were intercalated as single layers between LDH layers as confirmed by X-ray diffraction and infrared spectroscopy. Photoluminescence spectra of the nitrate intercalated LDH showed a wide emission band with strong intensity in the yellow region (around 574 nm, originated due to symmetry distortion of the octahedral coordination in dysprosium centers. Moreover, a broad red band emission was also detected apparently due to the presence of zinc oxide. The distorted symmetry of the dysprosium coordination environment, also confirmed by X-ray photoelectron spectroscopy analysis, was modified after the intercalation with phenyl phosphonate (PP, aspartate (Asp, adipate (Adip, and serinate (Ser anions; the emission as measured from PL spectra of these LDH was more intense in the blue region (ca. 486 nm, thus indicating an increase in symmetry of dysprosium octahedrons. The red emission band from zinc oxide kept the same intensity after intercalation of dodecyl sulfate (DDS. An additional emission of unknown origin at λ = 767 nm was present in all LDHs.

  1. Dual nutraceutical nanohybrids of folic acid and calcium containing layered double hydroxides

    Science.gov (United States)

    Kim, Tae-Hyun; Oh, Jae-Min

    2016-01-01

    Dual nutraceutical nanohybrids consisting of organic nutrient, folic acid (FA), and mineral nutrient, calcium, were prepared based on layered double hydroxide (LDH) structure. Among various hybridization methods such as coprecipitation, ion exchange, solid phase reaction and exfoliation-reassembly, it was found that exfoliation-reassembly was the most effective in terms of intercalation of FA moiety between Ca-containing LDH layers. X-ray diffraction patterns and infrared spectra indicated that FA molecules were well stabilized in the interlayer space of LDHs through electrostatic interaction. From the atomic force and scanning electron microscopic studies, particle thickness of LDH was determined to be varied with tens, a few and again tens of nanometers in pristine, exfoliated and reassembled state, respectively, while preserving particle diameter. The result confirmed layer-by-layer hybrid structure of FA and LDHs was obtained by exfoliation-reassembly. Solid UV-vis spectra showed 2-dimensional molecular arrangement of FA moiety in hybrid, exhibiting slight red shift in n→π* and π→π* transition. The chemical formulae of FA intercalated Ca-containing LDH were determined to Ca1.30Al(OH)4.6FA0.74·3.33H2O and Ca1.53Fe(OH)5.06FA2.24·9.94H2O by inductively coupled plasma-atomic emission spectroscopy, high performance liquid chromatography and thermogravimetry, showing high nutraceutical content of FA and Ca.

  2. Intracellular release of fluorescein anion from layered double hydroxide nanoparticles indicating endosomal escape

    Science.gov (United States)

    Tanaka, M.; Aisawa, S.; Hidetoshi, H.; Narita, E.; Dong, Q.; Yin, S.; Sato, T.

    2013-12-01

    In recent years, layered double hydroxide (LDH) has been attempted to be applied to a molecular container due to their anion exchange ability, low cytotoxicity and good biocompatibility. In this paper, we investigated the intracellular behaviour of LDH particles in mammalian cells after internalization. Nanoparticles of fluorescein (Fluo) intercalated LDH, Fluo/LDH, were prepared by the coprecipitation followed by subsequent hydrothermal treatment. As-prepared Fluo/LDH particles have the LDH structure and morphology of hexagonal sheet of 100 nm on the average. In addition, Fluo/LDH also exhibited high green fluorescence and low cytotoxicity. By a confocal laser scanning microscopy, the dim green fluorescence was observed throughout cells, including the nucleus. This result indicated that Fluo/LDH released guest anion (Fluo) from LDH structure inside cells. Furthermore, because the fluorescence was observed throughout the cell, Fluo was not retained within endosome structure, i.e., Fluo/LDH was dissolved to release Fluo from endosome.

  3. Novel inorganic host layered double hydroxides intercalated with guest organic inhibitors for anticorrosion applications.

    Science.gov (United States)

    Poznyak, S K; Tedim, J; Rodrigues, L M; Salak, A N; Zheludkevich, M L; Dick, L F P; Ferreira, M G S

    2009-10-01

    Zn-Al and Mg-Al layered double hydroxides (LDHs) loaded with quinaldate and 2-mercaptobenzothiazolate anions were synthesized via anion-exchange reaction. The resulting compounds were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy/energy-dispersive X-ray spectroscopy. Spectrophotometric measurements demonstrated that the release of organic anions from these LDHs into the bulk solution is triggered by the presence of chloride anions, evidencing the anion-exchange nature of this process. The anticorrosion capabilities of LDHs loaded with organic inhibitors toward the AA2024 aluminum alloy were analyzed by electrochemical impedance spectroscopy. A significant reduction of the corrosion rate is observed when the LDH nanopigments are present in the corrosive media. The mechanism by which the inhibiting anions can be released from the LDHs underlines the versatility of these environmentally friendly structures and their potential application as nanocontainers in self-healing coatings.

  4. Layered Double Hydroxide Nanoclusters: Aqueous, Concentrated, Stable, and Catalytically Active Colloids toward Green Chemistry.

    Science.gov (United States)

    Tokudome, Yasuaki; Morimoto, Tsuyoshi; Tarutani, Naoki; Vaz, Pedro D; Nunes, Carla D; Prevot, Vanessa; Stenning, Gavin B G; Takahashi, Masahide

    2016-05-24

    Increasing attention has been dedicated to the development of nanomaterials rendering green and sustainable processes, which occur in benign aqueous reaction media. Herein, we demonstrate the synthesis of another family of green nanomaterials, layered double hydroxide (LDH) nanoclusters, which are concentrated (98.7 g/L in aqueous solvent), stably dispersed (transparent sol for >2 weeks), and catalytically active colloids of nano LDHs (isotropic shape with the size of 7.8 nm as determined by small-angle X-ray scattering). LDH nanoclusters are available as colloidal building blocks to give access to meso- and macroporous LDH materials. Proof-of-concept applications revealed that the LDH nanocluster works as a solid basic catalyst and is separable from solvents of catalytic reactions, confirming the nature of nanocatalysts. The present work closely investigates the unique physical and chemical features of this colloid, the formation mechanism, and the ability to act as basic nanocatalysts in benign aqueous reaction systems.

  5. Co–Fe Prussian Blue Analogue Intercalated into Diamagnetic Mg–Al Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Cuijuan Zhang

    2016-04-01

    Full Text Available A heterostructure of diamagnetic magnesium‒aluminium layered double hydroxides (Mg‒Al LDHs and photomag‐ netic cobalt‒iron Prussian Blue analogue (Co‒Fe PBA was designed, synthesized and then designated as LDH‒PB. The cyanide-bridged Co‒Fe PBA was two-dimensionally intercalated into the Mg‒Al LDH template by the stepwise anion exchange method. LDH‒PB showed ferrimagnetic properties with in-plane antiferromagnetic exchange interactions, as well as small photo-induced magnetization by visible light illumination due to the low dimensional structures and the characteristic photo-induced electronic states of the mixed valence of FeIII(low spin, S = 1/2‒CN‒ CoII(high spin, S = 3/2‒NC‒FeII (low spin, S = 0.

  6. Preparation and characterization of trans-RhCl(CO)(TPPTS) 2-intercalated layered double hydroxides

    Science.gov (United States)

    Zhang, Xian; Wei, Min; Pu, Min; Li, Xianjun; Chen, Hua; Evans, David G.; Duan, Xue

    2005-09-01

    trans-RhCl(CO)(TPPTS) 2 (TPPTS= tris( m-sulfonatophenyl)phosphine) has been intercalated into Zn-Al layered double hydroxides (LDHs) by the method of ion exchange. The structure, composition and thermal stability of the composite material have been characterized by powder X-ray diffraction, Fourier transform infrared and 31P solid-state magic-angle spinning nuclear magnetic resonance spectroscopy, elemental analysis, thermogravimetry, and differential thermal analysis. The geometry of trans-RhCl(CO)(TPPTS) 2 was fully optimized using the PM3 semiempirical molecular orbital method, and a schematic model for the intercalated species has been proposed. The thermal stability of trans-RhCl(CO)(TPPTS) 2 is significantly enhanced by intercalation, which suggests that such materials may have prospective application as the basis of a supported catalyst system for the hydroformylation of higher olefins.

  7. Study on the adsorption kinetics of orthophosphate anions on layer double hydroxide

    Institute of Scientific and Technical Information of China (English)

    PENG Shuchuan; L(U) Lü; WANG Jin; HAN Lu; CHEN Tianhu; JIANG Shaotong

    2009-01-01

    A kinetic study was conducted on the adsorption of orthophosphate anions on layer double hydroxide (LDH). The adsorption has proved itself to be a spontaneous endothermic process and is large in capacity and rate. The adsorption isotherm correlates well with the Freundlich model, and a rise in temperature will lead to an increase in adsorption efficiency. Additionally, the results suggested that the adsorption is an entropy-increasing process and is in good agreement with the pseudo-second order kinetics. The free energy (ΔG) of adsorption of orthophosphate onto LDH varies within the range of -1.75- -3.34 kJ/mol, the enthalpy (ΔH) varies by 7.96 kJ/mol and the entropy (ΔS) by 33.59 kJ/mol. The adsorption activation energy is 8.3 kJ/mol, showing that the adsorption of orthophosphate onto LDH is determined to be a physical adsorption.

  8. Sepiocite, sepiolite-like nanoclay derived from hydrotalcite-like layered double hydroxide.

    Science.gov (United States)

    Park, Dae-Hwan; Jang, Myung Wook; Shul, Yong-Gun; Choy, Jin-Ho

    2011-01-01

    Sepiocite, a synthetic sepiolite-like nanoclay, was derived from hydrotalcite-like Mg2Al(CO3)0.5-layered double hydroxide (LDH) under phase transformation at 270 +/- 3 degrees C. The crystal structure of sepiocite is conceptually very similar to that of sepiolite derived from montmorillonite clay because sepiocite is formed through the alternation of the blocks and tunnels along the crystallographic c-axis, with a partial dehydroxylation of the octahedral Mg-(OH)-Al configuration into tetrahedral ones. Three important findings regarding sepiocite were arrived at: (i) its high specific surface area of 128.25 m2/g with an average particle size of 200 nm, which is approimately equal to 3.5 times larger than the specific surface area of the pristine LDH (34.21 m2/g); (ii) its non-swelling property; and (iii) its strongly reduced anion-exchange capacity.

  9. Synthesis of nanocomposite coating based on TiO2/ZnAl layer double hydroxides

    Directory of Open Access Journals (Sweden)

    V. Jovanov

    2017-02-01

    Full Text Available The aim of this investigation was the synthesis of nanocomposite coatings based on Zn-Al layered double hydroxides (Zn-Al LDH and TiO2. The Zn-Al LDH material, which acted as the catalyst support of the active TiO2 component (in the content of 3 and 10 wt. %, was synthesized by a low super saturation co-precipitation method. The interaction between the Zn-Al LDH and the active TiO2 component was accomplished by using vacuum evaporation prior to the mechanical activation and only by mechanical activation. The final suspension based on Zn-Al LDH and 10wt. % TiO2, impregnated only by mechanical activation, showed the optimal characteristics from the aspect of particle size distribution and XRD analysis. These properties had a positive effect on the functional properties of the coatings (photocatalytic activity and self-cleaning efficiency after the water rinsing procedure.

  10. Hydrothermal Synthesis of Nanorods and Nanowires of Mg/Al Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    ZHAO Yun; JIAO Qing-ze; DING Xue-jia; ZHANG Li-qun; LIU Yuan-yuan

    2007-01-01

    @@ Layered double hydroxides (LDHs) are a class of synthetic anion clays, characterized by the formula[MⅡ1-xMⅢx (OH)2]x+ (An- )x/n·yH2O (where M =metal and A = anion, usually carbonate)[1-3]. A large number of LDHs with a wide variety of M Ⅱ-M Ⅲ cation pairs including M Ⅰ-M Ⅲ ( e. g. , Li-Al ) and M Ⅱ-MⅣ( e. g. , Co-Ti) have been reported. Thus the identities of the cations(MⅠ , MⅡ , MⅢ and MⅣ) and the interlayer anion (An-) together with the value of the stoichiometric coefficient (x) may vary widely, giving rise to a large class of isostructural materials.

  11. Layered Double Hydroxide as a Vehicle to Increase Toxicity of Gallate Ions against Adenocarcinoma Cells

    Directory of Open Access Journals (Sweden)

    Jenny Arratia-Quijada

    2016-07-01

    Full Text Available The antineoplasic activity of gallic acid has been reported. This compound induces apoptosis and inhibits the growth of several neoplasic cells. However, this molecule is easily oxidized and degraded in the body. The aim of this work was to intercalate gallate ions into layered double hydroxide (LDH nanoparticles under controlled conditions to reduce oxidation of gallate and to evaluate its toxicity against the A549 adenocarcinoma cell line. An isopropanol medium under nitrogen atmosphere was adequate to intercalate gallate ions with a lesser oxidation degree as detected by electron spin resonance spectroscopy. Concentrations of the hybrid LDH-gallate nanoparticles between 0.39 and 25 µg/mL reduced the cell viability to 67%, while the value reached with the pure gallic acid and LDH was 90% and 78%, respectively, thus proving that the combination of gallate ions with the inorganic nanoparticles increases the toxicity potential within this dose range.

  12. Large Scale Synthesis of NiCo Layered Double Hydroxides for Superior Asymmetric Electrochemical Capacitor

    Science.gov (United States)

    Li, Ruchun; Hu, Zhaoxia; Shao, Xiaofeng; Cheng, Pengpeng; Li, Shoushou; Yu, Wendan; Lin, Worong; Yuan, Dingsheng

    2016-01-01

    We report a new environmentally-friendly synthetic strategy for large-scale preparation of 16 nm-ultrathin NiCo based layered double hydroxides (LDH). The Ni50Co50-LDH electrode exhibited excellent specific capacitance of 1537 F g-1 at 0.5 A g-1 and 1181 F g-1 even at current density as high as 10 A g-1, which 50% cobalt doped enhances the electrical conductivity and porous and ultrathin structure is helpful with electrolyte diffusion to improve the material utilization. An asymmetric ultracapacitor was assembled with the N-doped graphitic ordered mesoporous carbon as negative electrode and the NiCo LDH as positive electrode. The device achieves a high energy density of 33.7 Wh kg-1 (at power density of 551 W kg-1) with a 1.5 V operating voltage.

  13. Synthesis and photoluminescence of red emitting phosphors of europium complex intercalated layered double hydroxide

    Science.gov (United States)

    Gao, Xiaorui; Gao, Zhen; Yin, Xiaoru; Xie, Juan

    2015-12-01

    An inorganic-organic red emitting phosphor, europium ethylenediaminetetraacetate complex ([Eu(EDTA)]-) anions intercalated Mg/Al and Zn/Al layered double hydroxides (LDHs) were synthesized through an ion exchange method. X-ray powder diffraction (XRD) results exhibit that a nearly vertical arrangement of [Eu(EDTA)]- anions with the maximal dimension in the gallery is adopted. Measurement of the excitation and emission spectra show that the two materials display high red luminescence from Eu3+ ions. Furthermore, Mg/Al LDH containing europium complex has higher luminescence intensity than Zn/Al LDH, which probably was related with more inversion asymmetry sites of Eu3+ occurring in the Mg/Al LDH.

  14. A Simple Approach for the Synthesis of Gold Nanoparticles Mediated by Layered Double Hydroxide

    Directory of Open Access Journals (Sweden)

    Aires da Conceição Silva

    2013-01-01

    Full Text Available The present work introduces a new procedure to obtain gold nanoparticles (AuNPs. AuNPs (77–213 nm were obtained in the absence of any classical reducing agents in a medium containing Mg2+/Al3+ layered double hydroxide (LDH and N,N-dimethylformamide. XRD analysis showed the presence of crystalline phases of gold in the Au/LDH composite. The 2θ values of peaks corresponding to the LDH interlayer distance indicated that metallic NPs were deposited on the surface of the material. Furthermore, atomic force microscopy (AFM analysis showed that AuNPs tend to agglomerate in a nonclassical halter-like shape.

  15. Photostability enhancement of azoic dyes adsorbed and intercalated into Mg-Al-layered double hydroxide

    Science.gov (United States)

    Liu, Pengfei; Liu, Pei; Zhao, Kongcao; Li, Lei

    2015-11-01

    Two azoic dyes 4-aminoazobenzene-4-sulfonic (AS) and ethyl orange (EO) were adsorbed on or intercalated into Mg-Al-CO3 layered double hydroxide (LDH) for photostability enhancement. Fluorescence analysis results showed that the photostability of two dyes could be greatly improved after being adsorbed on the surface of Mg-Al-CO3-LDH matrix. Furthermore, photostability of adsorbed dyes was superior to that of intercalated dyes. It was suggested that AS or EO was adsorbed on LDHs surface through a strong chemisorption interaction, resulting in the enhancement of photostability. After the UV irradiation under N2 atmosphere, the absorbed dyes not only show great increase of fluorescence intensity but also exhibited high stability against UV irradiation. This work provides a feasible approach to enhance the photostability of azoic dye confined in an inorganic two-dimensional (2D) matrix via changing the microenvironment, which may be considered to be a promising method of improving photostability of solid fluorescent materials.

  16. Preparation and regulating cell adhesion of anion-exchangeable layered double hydroxide micropatterned arrays.

    Science.gov (United States)

    Yao, Feng; Hu, Hao; Xu, Sailong; Huo, Ruijie; Zhao, Zhiping; Zhang, Fazhi; Xu, Fujian

    2015-02-25

    We describe a reliable preparation of MgAl-layered double hydroxide (MgAl-LDH) micropatterned arrays on gold substrate by combining SO3(-)-terminated self-assembly monolayer and photolithography. The synthesis route is readily extended to prepare LDH arrays on the SO3(-)-terminated polymer-bonded glass substrate amenable for cell imaging. The anion-exchangeable MgAl-LDH micropattern can act both as bioadhesive region for selective cell adhesion and as nanocarrier for drug molecules to regulate cell behaviors. Quantitative analysis of cell adhesion shows that selective HepG2 cell adhesion and spreading are promoted by the micropatterned MgAl-LDH, and also suppressed by methotrexate drug released from the LDH interlayer galleries.

  17. Wetting behavior and drag reduction of superhydrophobic layered double hydroxides films on aluminum

    Science.gov (United States)

    Zhang, Haifeng; Yin, Liang; Liu, Xiaowei; Weng, Rui; Wang, Yang; Wu, Zhiwen

    2016-09-01

    We present a novel method to fabricate Zn-Al LDH (layered double hydroxides) film with 3D flower-like micro-and nanostructure on the aluminum foil. The wettability of the Zn-Al LDH film can be easily changed from superhydrophilic to superhydrophobic with a simple chemical modification. The as-prepared superhydrophobic surfaces have water CAs (contact angles) of 165 ± 2°. In order to estimate the drag reduction property of the surface with different adhesion properties, the experimental setup of the liquid/solid friction drag is proposed. The drag reduction ratio for the as-prepared superhydrophobic sample is 20-30% at low velocity. Bearing this in mind, we construct superhydrophobic surfaces that have numerous technical applications in drag reduction field.

  18. Effect of Layered Double Hydroxides on Ultraviolet Aging Resistance of SBS Modifi ed Bitumen Membrane

    Institute of Scientific and Technical Information of China (English)

    XU Song; YU Jianying; XUE Lihui; SUN Yubin; XIE Dong

    2015-01-01

    Layered double hydroxides (LDHs)/styrene-butadiene-styrene (SBS) copolymer modified bitumen was prepared by melt blending. The effect of LDHs on the ultraviolet (UV) aging behavior of SBS modifi ed bitumen was investigated. The changes of chemical structures of modifi ed bitumen before and after UV aging were characterized by Fourier transform infrared spectroscopy (FTIR). The results show that LDHs obviously reduce the variation of softening point and low temperaturefl exibility of SBS modifi ed bitumen under different UV radiation intensities, which indicates that the UV aging resistance performance of SBS modifi ed bitumen is improved effectively by LDHs. Compared with SBS modifi ed bitumen, the changes of carbonyl, sulfoxide and butadienyl of LDHs/SBS modified bitumen decrease significantly after UV aging according to FTIR analysis, demonstrating that the oxidation and degradation reactions of SBS modifi ed bitumen were restrained effectively by adding LDHs.

  19. Fatigue Properties of Layered Double Hydroxides Modified Asphalt and Its Mixture

    Directory of Open Access Journals (Sweden)

    Xing Liu

    2014-01-01

    Full Text Available This study investigated the influence of layered double hydroxides (LDHs on the fatigue properties of asphalt mixture. In this paper, different aging levels (thin film oven test (TFOT and ultraviolet radiation aging (UV aging for short of bitumen modified with various mass ratios of the LDHs were investigated. The TFOT and UV aging process were used to simulate short-term field thermal-oxidative aging and long-term field light UV aging of bitumen, respectively. The influences of LDHs on the fatigue properties of LDHs were evaluated by dynamic shear rheometer (DSR and indirect tensile fatigue test. Results indicated that the introduction of LDHs could change the fatigue properties of bitumen under a stress control mode. The mixture with modified bitumen showed better fatigue resistance than the mixture with base bitumen. The results illustrated that the LDHs would be alternative modifiers used in the bitumen to improve the lifetime of asphalt pavements.

  20. APPLICATIONS OF LAYERED DOUBLE HYDROXIDES IN REMOVING OXYANIONS FROM OIL REFINING AND COAL MINING WASTEWATER

    Energy Technology Data Exchange (ETDEWEB)

    Song Jin; Paul Fallgren

    2006-03-01

    Western Research Institute (WRI), in conjunction with the U.S. Department of Energy (DOE), conducted a study of using the layered double hydroxides (LDH) as filter material to remove microorganisms, large biological molecules, certain anions and toxic oxyanions from various waste streams, including wastewater from refineries. Results demonstrate that LDH has a high adsorbing capability to those compounds with negative surface charge. Constituents studied include model bacteria, viruses, arsenic, selenium, vanadium, diesel range hydrocarbons, methyl tert-butyl ether (MTBE), mixed petroleum constituents, humic materials and anions. This project also attempted to modify the physical structure of LDH for the application as a filtration material. Flow characterizations of the modified LDH materials were also investigated. Results to date indicate that LDH is a cost-effective new material to be used for wastewater treatment, especially for the treatment of anions and oxyanions.

  1. Migration of nanosized layered double hydroxide platelets from polylactide nanocomposite films

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Katiyar, Vimal; Plackett, David

    2011-01-01

    Melt-extruded L-polylactide (PLA) nanocomposite films were prepared from commercially available PLA and laurate-modified Mg–Al layered double hydroxide (LDH-C12). Three films were tested for total migration as well as specific migration of LDH, tin, laurate and low molecular weight PLA oligomers...... (OLLA). This is the first reported investigation on the migration properties of PLA-LDH nanocomposite films. The tests were carried out as part of an overall assessment of the suitability of such films for use as food contact materials (FCM). Total migration was determined according to a European...... standard method. All three films showed migration of nanosized LDH, which was quantified using acid digestion followed by inductively coupled plasma mass spectrometric (ICP–MS) detection of 26Mg. Migration of LDH from the films was also confirmed by examining migrates using transmission electron microscopy...

  2. Layered double hydroxide nanosheet as a two-dimensional support of dense platinum nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Hyo Gyoung; Cho, Se Hee; Ji, Hong Geun [H and A PharmaChem, R and D center, Bucheon (Korea, Republic of); Lee, Jong Hyeon [Dept. of Chemistry, The Catholic University of Korea, Bucheon (Korea, Republic of)

    2017-02-15

    Transition metal nanoparticles (NPs) with a narrow size distribution have been intensively synthesized on various solid supports for anti-agglomeration, and high catalytic activity and selectivity. Layered double hydroxides (LDH) are currently attracting intense interest in the field of heterogeneous catalysis as catalyst supports. In order to obtain a well-crystallized LDH nanosheet, the as-synthesize d carbonate form of LDH was hydrothermally treated according to a reported procedure, and further reacted by anion-exchange with an aqueous solution of NaNO{sub 3} and acetate buffer to give the nitrate form of LDH. Dense and uniform Pt NPs were synthesized on the exfoliated LDH nanosheets through precursor exchange and thermal reduction of the precursor ions. In this nanocomposite, the Pt Nps were uniformly grown on the surface of the LDH nano sheet and the average size of Pt Nps was 2nm.

  3. Poly I-lactide-layered double hydroxide nanocomposites via in situ polymerization of I-lactide

    DEFF Research Database (Denmark)

    Katiyar, Vimal; Gerds, N.; Koch, C.B.;

    2010-01-01

    The use of clay nanofillers offers a potential route to improved barrier properties in polylactide films. Magnesium–aluminium layered double hydroxides (LDHs) are interesting in this respect and we therefore explored synthesis of PLA-LDH nanocomposites by ring-opening polymerization. This method...... is attractive because it should ensure good dispersion of LDH in the polymer. The effect of adding either LDH carbonate (LDH-CO3) or laurate-modified LDH (LDH-C12) was investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy revealed that exfoliated nanocomposites were...... obtained when using LDH-C12 but that LDH-CO3 gave a partly phase-separated morphology. Thermogravimetric analysis showed that PLA-LDH combinations exhibited higher degradation onset temperatures and differential scanning calorimetry confirmed that LDHs can act as nucleating agents. However, PLA molecular...

  4. Removal of guar and humus from water by layered double hydroxides.

    Science.gov (United States)

    Jin, Song; Cui, Kangping; Fallgren, Paul H; Urynowicz, Michael A; Jian, Jiazhong

    2009-01-01

    Natural organic matter such as guar and humus are recalcitrant to conventional pretreatment technologies and can potentially foul processes such as membranes during water treatment. An innovative method of using synthetic layered double hydroxides (LDH) was investigated for removing common natural organic matter in the form of guar gum (GG) and humic acid (HA) from water. Adsorption isotherms were evaluated with Langmuir and Freundlich models. Results show the affinity of GG and HA to LDH to be 11.31 and 9.33 mg g(-1) LDH, respectively. Kinetic isotherms indicate that the sorbing rates of LDH to GG and HA increase with initial GG and HA concentrations, fitting a pseudo-second order model. This study demonstrate that LDH may be an effective material in removing GG and HA from waters and offer an alternative to conventional pretreatment technologies for the mitigation fouling of membrane and other systems in water treatment.

  5. Interstratified nanohybrid assembled by alternating cationic layered double hydroxide nanosheets and anionic layered titanate nanosheets with superior photocatalytic activity.

    Science.gov (United States)

    Lin, Bizhou; Sun, Ping; Zhou, Yi; Jiang, Shaofeng; Gao, Bifen; Chen, Yilin

    2014-09-15

    Oppositely charged 2D inorganic nanosheets of ZnAl-layered double hydroxide and layered titanate were successfully assembled into an interstratified nanohybrid through simply mixing the corresponding nanosheet suspensions. Powder X-ray diffraction and high-resolution transmission electron microscope clearly revealed that the component nanosheets in the as-obtained nanohybrid ZnAl-Ti3O7 retain the 2D sheet skeletons of the pristine materials and that the two kinds of nanosheets are well arranged in a layer-by-layer alternating fashion with a basal spacing of about 1.3 nm, coincident with the thickness summation of the two component nanosheets. The effective interfacial heterojunction between them and the high specific surface area resulted in that the nanohybrid exhibits a superior photocatalytic activity in the degradation of methylene blue with a reaction constant k of 2.81 × 10(-2)min(-1), which is about 9 and 4 times higher than its precursors H2Ti3O7 and ZnAl-LDH, respectively. Based on UV-vis, XPS and photoelectrochemical measurements, a proposed photoexcitation model was provided to understand its photocatalytic behavior.

  6. Mixed oxides derived from layered double hydroxides as novel catalysts for phenol photodegradation

    Science.gov (United States)

    Puscasu, C. M.; Carja, G.; Mureseanu, M.; Zaharia, C.

    2017-08-01

    The removal of organic pollutants is nowadays a very challenging aspect of the environmental research. There are strong interests to develop novel semiconducting photocatalysts able to efficiently promote advanced oxidation reactions. The development of photocatalysts based on the mixtures of mixed oxides derived from layered double hydroxides (LDHs) - a family of naturally occurring anionic clays - might offer novel environmental-friendly solutions for the cost effective removal of organic pollutants. This work presents ZnO/ZnAl2O4, ZnO/Zn2TiO4 and ZnO/ZnCr2O4 as novel photocatalytic formulations for phenol degradation under UV irradiation. They were obtained by the controlled thermal treatment of the layered double hydroxides matrices (LDHs), as precursors materials, type ZnM-LDH (M = Al3+, Cr3+ or Ti4+). The LDHs were synthesized by the co-precipitation method at a constant pH. Controlled calcination at 650°C gives rise to solutions of mixed metal oxides. The structural and nanoarchitectonics characteristics of the studied catalysts were described by: XRD, SEM/TEM and TG/DTG techniques. Results show that in the photocatalytic process of the phenol degradation from aqueous solutions, ZnO/ZnCr2O4 and ZnO/ZnAl2O4 showed the best performance degrading ∼98% of phenol after 3.5 hs and 5 hs, respectively; while ZnO/Zn2TiO4 has degraded almost 80 % after 7.5 hs of UV irradiation. These results open new opportunities in the development of new cost effective photoresponsive formulations able to facilitate the photo-degradation of the organic pollution as “green” solution for removal of dangerous pollutants.

  7. Absorption of the selenite anion from aqueous solutions by thermally activated layered double hydroxide.

    Science.gov (United States)

    Liu, Rui; Frost, Ray L; Martens, Wayde N

    2009-03-01

    The presence of selenite or selenate in potable water is a health hazard especially when consumed over a long period of time. Its removal from potable water is of importance. This paper reports technology for the removal of selenite from water through the use of thermally activated layered double hydroxides. Mg/Al hydrotalcites with selenite in the interlayer were prepared at different times from 0.5 to 20 h through ion exchange. X-ray diffraction of the MgAlSeO3 hydrotalcites indicates that the selenite anion entered the interlayer spacing of Mg/Al hydrotalcite and MgAlSeO3 hydrotalcite was formed. Raman spectra proved the presence of selenite anion in the hydrotalcite interlayer as the counter anion. The band intensity and width of MgAlSeO3 hydrotalcite in the region of 3800-3000 cm(-1) increase with the adsorption of selenite by the Mg/Al hydrotalcite. The characteristic bands of free selenite anions in the MgAlSeO3 hydrotalcites are located between the region between 850 and 800 cm(-1). The Raman spectra of the lower wave number region of 550-500 cm(-1) show a shift toward higher wave numbers with adsorption of the selenite. An estimation of the amount of selenite anion removed by the thermally activated layered double hydroxide was obtained through the measurement of the intensity of the selenite Raman bands at 814 and 835 cm(-1) resulting from the amount of selenite anion remaining in solution. Thermally activated LDHs provide a mechanism for removing selenite anions from aqueous solutions.

  8. Facile synthesis of methotrexate intercalated layered double hydroxides: Particle control, structure and bioassay explore

    Energy Technology Data Exchange (ETDEWEB)

    Tian, De-Ying; Liu, Zhen-Lei [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China); Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China); Li, Xiao-Dong [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China); Shenzhen Research Institute of Xiamen University, Shenzhen 518057 (China)

    2014-12-01

    To study the influence of particle size on drug efficacy and other properties, a series of methotrexate intercalated layered double hydroxides (MTX/LDHs) were synthesized through the traditional coprecipitation method, using a mixture of water and polyethylene glycol (PEG-400) as the solvent. To adjust the particle size of MTX/LDHs, the dropping way, the volume ratio of water to PEG-400 and different hydrothermal treatment time changed accordingly, and the results indicate that the particle size can be controlled between 90 and 140 nm. Elemental C/H/N and inductive coupled plasma (ICP) analysis indicated that different synthesis conditions almost have no effect on the compositions of the nanohybrids. X-ray diffraction (XRD) patterns manifested the successful intercalation of MTX anions into the LDH interlayers, and it's also found out that different volume ratios of water to PEG-400 and variable dropping way can affect the crystallinity of the final samples, i.e., the volume ratio of 3:1 and pH decreasing are proved to be optimum conditions. Furthermore, both antiparallel monolayer and bilayers adopting different orientations are suggested for four samples from XRD results. Fourier transform infrared spectroscopy (FTIR) investigations proved the coexistence of CO{sub 3}{sup 2−} and MTX anions in the interlayer of the nanohybrids. MTX/LDH particles exhibited hexagonal platelet morphology with round corner and different dropping ways can affect the morphology greatly. Moreover, a DSC study indicated that longer time treatment can weaken the bond between the MTX anions and LDH layers. The kinetic release profiles told us that larger MTX/LDH particles have enhanced the ability of LDH layers to protect interlayer molecules. At last, the bioassay study indicated that the nanohybrids with larger diameters have higher tumor suppression efficiency. - Graphical abstract: A series of methotrexate intercalated layered double hydroxides were synthesized by changing the

  9. Layered double hydroxides as supports for intercalation and sustained release of antihypertensive drugs

    Science.gov (United States)

    Xia, Sheng-Jie; Ni, Zhe-Ming; Xu, Qian; Hu, Bao-Xiang; Hu, Jun

    2008-10-01

    Zn/Al layered double hydroxides (LDHs) were intercalated with the anionic antihypertensive drugs Enalpril, Lisinopril, Captopril and Ramipril by using coprecipitation or ion-exchange technique. TG-MS analyses suggested that the thermal stability of Ena -, Lis - (arranged with monolayer, resulted from X-ray diffraction (XRD) and Fourier transform infrared spectra (FT-IR) analysis was enhanced much more than Cap - and Ram - (arranged with bilayer). The release studies show that the release rate of all samples markedly decreased in both pH 4.25 and 7.45. However, the release time of Ena -, Lis - were much longer compared with Cap -, Ram - in both pH 4.25 and 7.45, it is possible that the intercalated guests, arranged with monolayer in the interlayer, show lesser repulsive force and strong affinity with the LDH layers. And the release data followed both the Higuchi-square-root law and the first-order equation well. Based on the analysis of batch release, intercalated structural models as well as the TG-DTA results, we conclude that for drug-LDH, stronger the affinity between intercalated anions and the layers is, better the thermal property and the stability to the acid attack of drug-LDH, and the intercalated anions are easier apt to monolayer arrangement within the interlayer, were presented.

  10. Removal of Remazol Blue 19 from wastewater by zinc-aluminium-chloride-layered double hydroxides

    Science.gov (United States)

    Elkhattabi, El Hassan; Lakraimi, Mohamed; Badreddine, Mohamed; Legrouri, Ahmed; Cherkaoui, Omar; Berraho, Moha

    2013-06-01

    Layered double hydroxides (LDHs), also called anionic clays, consist of cationic brucite-like layers and exchangeable interlayer anions. These hydrotalcite-like compounds, with Zn and Al in the layers and chloride in the interlayer space, were prepared following the coprecipitation method at constant pH. The affinity of this material for Remazol Blue 19, RB19 [ 2- (3- (4- Amino- 9,10- dihydro- 3- sulpho- 9,10- dioxoanthracen- 4- yl) aminobenzenesulphonyl) vinyl) disodiumsulphate], was studied as a function of contact time, pH of the solutions LDH dose and the RB19/[Zn-Al-Cl] mass ratio. It was found that 48 h is enough time for the equilibrium state to be reached with maximum RB19 retention at pH of 9 for an LDH dose equal to 100 mg and with an RB19/[Zn-Al-Cl] mass ratio higher than 3. The adsorption isotherm, described by the Langmuir model, is of L-type. The results demonstrate that RB19 retention on LDHs occurs by adsorption on external surface when RB19/[Zn-Al-Cl] mass ratio is equal or <3 and by both adsorption and interlayer ion exchange for ratios higher than 3. A mechanism for removal of RB19 anion has been confirmed by X-ray diffraction, IR spectroscopy and TG analysis (TG and DTG curves).

  11. Multilayer films of layered double hydroxide/polyaniline and their ammonia sensing behavior.

    Science.gov (United States)

    Xu, Dong-Mei; Guan, Mei-Yu; Xu, Qing-Hong; Guo, Ying

    2013-11-15

    This paper reports the fabrication of layered double hydroxide (LDH)/conductive polymer multilayer films by alternate assembly of exfoliated ZnAl-LDH nanosheets and polyaniline (PANI) on silicon wafer substrates using the layer-by-layer (LBL) deposition technology. UV-vis absorption spectroscopy indicates a stepwise and regular growth of the (LDH/PANI)n multilayer films upon increasing deposition cycles. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrate that the surfaces of the films are microscopy smooth and uniform with a thickness of 2 nm per bilayer. Furthermore, the resulting (LDH/PANI)n multilayer films possess high selectively response to ammonia at room temperature. The presence of LDH nanosheets plays a critical role on the gas sensing for the pure PANI film has very low response to ammonia. The LBL assembly process based on LDH combines the conducting polymer and nano-inorganic material, which provides opportunities to develop new inorganic-organic films for gas sensing.

  12. Controlled synthesis of layered double hydroxide nanoplates driven by screw dislocations.

    Science.gov (United States)

    Forticaux, Audrey; Dang, Lianna; Liang, Hanfeng; Jin, Song

    2015-05-13

    Layered double hydroxides (LDHs) are a family of two-dimensional (2D) materials with layered crystal structures that have found many applications. Common strategies to synthesize LDHs lead to a wide variety of morphologies, from discrete 2D nanosheets to nanoflowers. Here, we report a study of carefully controlled LDH nanoplate syntheses using zinc aluminum (ZnAl) and cobalt aluminum (CoAl) LDHs as examples and reveal their crystal growth to be driven by screw dislocations. By controlling and maintaining a low precursor supersaturation using a continuous flow reactor, individual LDH nanoplates with well-defined morphologies were synthesized on alumina-coated substrates, instead of the nanoflowers that result from uncontrolled overgrowth. The dislocation-driven growth was further established for LDH nanoplates directly synthesized using the respective metal salt precursors. Atomic force microscopy revealed screw dislocation growth spirals, and under transmission electron microscopy, thin CoAl LDH nanoplates displayed complex contrast contours indicative of strong lattice strain caused by dislocations. These results suggest the dislocation-driven mechanism is generally responsible for the growth of 2D LDH nanostructures, and likely other materials with layered crystal structures, which could help the rational synthesis of well-defined 2D nanomaterials with improved properties.

  13. Reductive dehalogenation by layered iron(II)-iron(III) hydroxides and related iron(II) containing solids

    DEFF Research Database (Denmark)

    Yin, Weizhao

    In the present PhD project, novel synthesis and modifications of layered Fe(II)-Fe(III) hydroxides (green rusts, GRs) were investigated with focus on improved dehalogenation of carbon tetrachloride by using modified green rusts and/or altered reaction conditions. The Ph.D. project has comprised: 1...

  14. Folic acid conjugated self-assembled layered double hydroxide nanoparticles for high-efficacy-targeted drug delivery.

    Science.gov (United States)

    Yan, Li; Chen, Wei; Zhu, Xiaoyue; Huang, Longbiao; Wang, Zhigang; Zhu, Guangyu; Roy, V A L; Yu, K N; Chen, Xianfeng

    2013-12-04

    Enhanced selectivity and efficacy is important for advanced drug delivery. Herein, a novel type of folic acid conjugated self-assembled layered double hydroxide nanoparticles is reported. These nanoparticles have a drug loading capacity of 27 wt% and are able to enter cell nuclei and dramatically improve the efficacy of MTX.

  15. Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

    Energy Technology Data Exchange (ETDEWEB)

    Djebbi, Mohamed Amine, E-mail: mohamed.djebbi@etu.univ-lyon1.fr [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Braiek, Mohamed [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Namour, Philippe [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Irstea, 5 rue de la Doua, 69100 Villeurbanne (France); Ben Haj Amara, Abdesslem [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Jaffrezic-Renault, Nicole [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France)

    2016-11-15

    Highlights: • MgAl and ZnAl LDH nanosheets were chemically synthesized and deposited over carbon electrode materials. • Catalytic performance of both LDHs was investigated for Fe(II) reduction reaction. • Satisfactory results have been achieved with the MgAl LDH material. • MgAl and ZnAl LDH modified carbon felt were applied in MFC as an efficient anode catalyst. • The LDH-modified anode significantly increased power performance of MFC. - Abstract: Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However

  16. Dual nutraceutical nanohybrids of folic acid and calcium containing layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Tae-Hyun; Oh, Jae-Min, E-mail: jaemin.oh@yonsei.ac.kr

    2016-01-15

    Dual nutraceutical nanohybrids consisting of organic nutrient, folic acid (FA), and mineral nutrient, calcium, were prepared based on layered double hydroxide (LDH) structure. Among various hybridization methods such as coprecipitation, ion exchange, solid phase reaction and exfoliation-reassembly, it was found that exfoliation-reassembly was the most effective in terms of intercalation of FA moiety between Ca-containing LDH layers. X-ray diffraction patterns and infrared spectra indicated that FA molecules were well stabilized in the interlayer space of LDHs through electrostatic interaction. From the atomic force and scanning electron microscopic studies, particle thickness of LDH was determined to be varied with tens, a few and again tens of nanometers in pristine, exfoliated and reassembled state, respectively, while preserving particle diameter. The result confirmed layer-by-layer hybrid structure of FA and LDHs was obtained by exfoliation-reassembly. Solid UV–vis spectra showed 2-dimensional molecular arrangement of FA moiety in hybrid, exhibiting slight red shift in n→π* and π→π* transition. The chemical formulae of FA intercalated Ca-containing LDH were determined to Ca{sub 1.30}Al(OH){sub 4.6}FA{sub 0.74}·3.33H{sub 2}O and Ca{sub 1.53}Fe(OH){sub 5.06}FA{sub 2.24}·9.94H{sub 2}O by inductively coupled plasma-atomic emission spectroscopy, high performance liquid chromatography and thermogravimetry, showing high nutraceutical content of FA and Ca. - Highlights: • We successfully intercalated FA molecules into Ca-containing LDHs. • Exfoliation-reassembly was proven to be the most effective. • The interaction between LDH and FA were studied by FT-IR and UV–vis spectra. • Thermal stability of FA were enhanced by electrostatic interaction with LDH layers.

  17. Superhydrophobic and UV-blocking cotton fabrics prepared by layer-by-layer assembly of organic UV absorber intercalated layered double hydroxides

    Science.gov (United States)

    Zhao, Yan; Xu, Zhiguang; Wang, Xungai; Lin, Tong

    2013-12-01

    A dual-functional coating with both superhydrophobic and UV-blocking properties was prepared on cotton fabric using a hybrid layered double hydroxide (LDH) nanoplatelet intercalated with 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid (HMBS) molecules and an electrostatic layer-by-layer (LbL) assembly technique. The thermal stability of HMBS was greatly enhanced by the host-guest interaction with LDH layers. The as-prepared HMBS@LDH hybrid had a nearly neutral surface charge. To make it carry enough charge for the electrostatic LbL assembly, the HMBS@LDH nanoplatelet was further modified with 3-aminopropyltriethoxy silane. The nanoscale roughness generated by LDH nanoplatelets, together with low-surface-energy fluoroalkylsilane, endowed cotton fabrics with superhydrophobicity. The HMBS@LDH coating showed up to four-fold increase in the UV protection ability of cotton fabrics.

  18. Nitrogen doping in atomic layer deposition grown titanium dioxide films by using ammonium hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Kaeaeriaeinen, M.-L., E-mail: marja-leena.kaariainen@lut.fi; Cameron, D.C.

    2012-12-30

    Titanium dioxide films have been created by atomic layer deposition using titanium chloride as the metal source and a solution of ammonium hydroxide in water as oxidant. Ammonium hydroxide has been used as a source of nitrogen for doping and three thickness series have been deposited at 350 Degree-Sign C. A 15 nm anatase dominated film was found to possess the highest photocatalytic activity in all film series. Furthermore almost three times better photocatalytic activity was discovered in the doped series compared to undoped films. The doped films also had lower resistivity. The results from X-ray photoemission spectroscopy showed evidence for interstitial nitrogen in the titanium dioxide structure. Besides, there was a minor red shift observable in the thickest samples. In addition the film conductivity was discovered to increase with the feeding pressure of ammonium hydroxide in the oxidant precursor. This may indicate that nitrogen doping has caused the decrease in the resistivity and therefore has an impact as an enhanced photocatalytic activity. The hot probe test showed that all the anatase or anatase dominant films were p-type and all the rutile dominant films were n-type. The best photocatalytic activity was shown by anatase-dominant films containing a small amount of rutile. It may be that p-n-junctions are formed between p-type anatase and n-type rutile which cause carrier separation and slow down the recombination rate. The combination of nitrogen doping and p-n junction formation results in superior photocatalytic performance. - Highlights: Black-Right-Pointing-Pointer We found all N-doped and undoped anatase dominating films p-type. Black-Right-Pointing-Pointer We found all N-doped and undoped rutile dominating films n-type. Black-Right-Pointing-Pointer We propose that p-n junctions are formed in anatase-rutile mixture films. Black-Right-Pointing-Pointer We found that low level N-doping has increased TiO{sub 2} conductivity. Black

  19. Preparation of poly(ethylene terephthalate/layered double hydroxide nanocomposites by in-situ polymerization and their thermal property

    Directory of Open Access Journals (Sweden)

    Q. Jiao

    2012-06-01

    Full Text Available Terephthalate (TA intercalated layered double hydroxides (LDHs were synthesized using hydroxides as raw materials, and poly(ethylene terephthalate (PET/LDH nanocomposites with different contents of TA intercalated LDHs were prepared by in-situ polymerization. The structure, morphology and thermal property of PET/LDH nanocomposites were investigated. The TA intercalated LDHs were partially exfoliated and well dispersed in PET matrix. The PET/LDH nanocomposites exhibit enhanced thermal stability relative to pure PET, confirmed by the thermogravimetric analysis results. The results of differential scanning calorimetry suggest that LDH nanoparticles could effectively promote the nucleation and crystallization of PET.

  20. Highly stable layered double hydroxide colloids: a direct aqueous synthesis route from hybrid polyion complex micelles.

    Science.gov (United States)

    Layrac, Géraldine; Destarac, Mathias; Gérardin, Corine; Tichit, Didier

    2014-08-19

    Aqueous suspensions of highly stable Mg/Al layered double hydroxide (LDH) nanoparticles were obtained via a direct and fully colloidal route using asymmetric poly(acrylic acid)-b-poly(acrylamide) (PAA-b-PAM) double hydrophilic block copolymers (DHBCs) as growth and stabilizing agents. We showed that hybrid polyion complex (HPIC) micelles constituted of almost only Al(3+) were first formed when mixing solutions of Mg(2+) and Al(3+) cations and PAA3000-b-PAM10000 due to the preferential complexation of the trivalent cations. Then mineralization performed by progressive hydroxylation with NaOH transformed the simple DHBC/Al(3+) HPIC micelles into DHBC/aluminum hydroxide colloids, in which Mg(2+) ions were progressively introduced upon further hydroxylation leading to the Mg-Al LDH phase. The whole process of LDH formation occurred then within the confined environment of the aqueous complex colloids. The hydrodynamic diameter of the DHBC/LDH colloids could be controlled: it decreased from 530 nm down to 60 nm when the metal complexing ratio R (R = AA/(Mg + Al)) increased from 0.27 to 1. This was accompanied by a decrease of the average size of individual LDH particles as R increased (for example from 35 nm at R = 0.27 down to 17 nm at R = 0.33), together with a progressive favored intercalation of polyacrylate rather than chloride ions in the interlayer space of the LDH phase. The DHBC/LDH colloids have interesting properties for biomedical applications, that is, high colloidal stability as a function of time, stability in phosphate buffered saline solution, as well as the required size distribution for sterilization by filtration. Therefore, they could be used as colloidal drug delivery systems, especially for hydrosoluble negatively charged drugs.

  1. Dynamics of Intercalation/De-Intercalation of Rhodamine B during the Polymorphic Transformation of CdAl Layered Double Hydroxide to the Brucite-Like Cadmium Hydroxide

    KAUST Repository

    Saliba, Daniel

    2016-06-23

    Cadmium-Aluminum layered double hydroxide (CdAl LDH) is thermodynamically unstable and transforms to Cd(OH)2 and Al(OH)3 in a short period of time. We present a reaction-diffusion framework that enables us to use in situ steady-state fluorescence spectroscopy to study the kinetics of intercalation of a fluorescent probe (Rhodamine B (RhB)) during the formation of the CdAl LDH and its de-intercalation upon the conversion of the LDH phase to the β phase (Cd(OH)2). The method involves the diffusion of sodium hydroxide into a hydrogel gel matrix containing the aluminum and cadmium ions as well as the species we wish to incorporate in the interlayers of the LDH. The existence of RhB between the LDH layers and its expel during the transition into the β phase are proved via fluorescence microscopy, XRD and ssNMR. The activation energies of intercalation and de-intercalation of RhB are computed and show dependence on the cationic ratio of the corresponding LDH. We find that the energies of de- intercalation are systematically higher than those of intercalation proving that the dyes are stabilized due to the probe-brucite sheets interactions.

  2. Engineering of (10-hydroxycamptothecin intercalated layered double hydroxide)@liposome nanocomposites with excellent water dispersity

    Science.gov (United States)

    Zhang, Yongfang; Wu, Xiaowen; Mi, Yuwei; Li, Haiping; Hou, Wanguo

    2017-09-01

    A hierarchical nanocomposite of 10-hydroxycamptothecin (HCPT), a nonionic and lipophilic anticancer drug, intercalated layered double hydroxide (LDH) encapsulated in liposomes was constructed. HCPT molecules were first incorporated into sodium cholate (Ch) micelles, and the resultant negatively charged HCPT-loaded Ch micelles were then co-assembled with positively charged LDH single-layer nanosheets, forming a HCPT/Ch intercalated LDH (HCPT-Ch-LDH) host-gest nanohybrid. The nanohybrid particles were further coated with liposomes (LSs), gaining a core-shell nanocomposite, denoted as (HCPT-Ch-LDH)@LS. The so-obtained samples were characterized using TEM, SAXS, FT-IR, DLS, and elemental analyses. Special emphasis was placed on the effect of liposome-coating for the HCPT-Ch-LDH on its water dispersity and drug-release. The results showed that the nanocomposite has excellent water dispersity and enhanced drug sustained-release performance in comparison with the HCPT-Ch-LDH, demonstrating that the liposome-coating for drug-LDH nanohybrids is an effective strategy to enhance their water dispersity and sustained-release performances. This work provides an effective strategy for engineering of LDH-based delivery systems for nonionic and lipophilic drugs.

  3. A novel method to get methotrexatum/layered double hydroxides intercalation compounds and their release properties

    Science.gov (United States)

    Qi, Fenglin; Zhang, Xiaoqing; Li, Shuping

    2013-08-01

    In this context, the methotrexatum/layered double hydroxides (MTX/LDHs) intercalation compounds have been synthesized by a mechanochemical-hydrothermal method, which involves a grinding process and subsequent hydrothermal treatment. The influence of R (molar ratio of Mg2+ to Al3+ to MTX) values on the structure and morphology of the intercalation compounds and their release properties were investigated systematically. The resulting compounds were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), inductively coupled plasma (ICP), thermogravimetric (TG) and differential scanning calorimetry (DSC) analysis. All the results indicate that R value has significant influence on the intercalation of MTX anions into LDH interlayer and the optimal R value is 2:1:0.5. Furthermore, four dissolution-diffusion kinetic models were used to fit the in vitro release of MTX from LDH layers. The release process can be divided into two stages: firstly surface diffusion and secondly intraparticle diffusion. The study also revealed that the properties of the intercalation compounds is comparable to that obtained from standard methods such as co-precipitation method, but with time, solvent and energy saving.

  4. Surface-charging behavior of Zn-Cr layered double hydroxide.

    Science.gov (United States)

    Rojas Delgado, R; Arandigoyen Vidaurre, M; De Pauli, C P; Ulibarri, M A; Avena, M J

    2004-12-15

    A Zn-Cr layered double hydroxide (LDH) having the formula Zn(2)Cr(OH)(6)Cl(0.7)(CO(3))(0.15)2.1H(2)O was synthesized and characterized by powder X-ray diffraction, infrared spectroscopy, acid-base potentiometric titration, mass titration, electrophoretic mobility, and modeling of the electrical double layer. Adsorption of alizarin was also performed in order to show some particular features of the HDL. Net hydroxyl adsorption, which increases with increasing pH and decreasing supporting electrolyte concentration, takes place above pH 5. The electrophoretic mobility of the particles was always positive and it decreased when the pH was higher than 9. An isoelectric point of 12 could be estimated by extrapolating the data. The modified MUSIC model was used to estimate deprotonation constants of surface groups and different adsorption models were compared. Good fit of hydroxyl adsorption and electrophoresis could be achieved by considering both OH(-)/Cl(-) exchange at structural sites and proton desorption from surface hydroxyl groups. The modeling, in agreement with alizarin adsorption, indicates that most of the structural positive charge of the LDH is screened at the surface by exchanged anions and negatively charged surface groups. It also suggests that only structural charge sites initially neutralized by chloride ions are active for anion exchange. The remaining sites are blocked by carbonate and do not participate in the exchange.

  5. Synthesis and Characterization of Camptothecin Intercalated into Mg/AI Layered Double Hydroxide

    Institute of Scientific and Technical Information of China (English)

    LIU,Chun-Xia; HOU,Wan-Guo; LI,Yan; LI,Li-Fang

    2008-01-01

    The intercalation of camptothecin(CPT)into a layered inorganic host,Mg-Al layered double hydroxide(LDH),was carried out using a coprecipitation method tO obtain CPT-LDH nanohybrids.It Was found that the intercalated amounts(Ain)of CPrr-LDH nanohybrids were remarkably dependent on the molar ratios(Rc,M)of CPT tO metal ions in raw materials.The Ain value increases with the RC/M value increasing.According to the gallery heights of CPT-LDH and sizes of CPT molecule,a probably morphology of CPT molecules in the gallery of LDH was suggested that the horizontal-arranged monolayer and vertical-arranged bilayer of CPT molecules coexisted in the interlayer region of LDH.An interesting result was found that the gallery height corresponding to the bilayer of CPT-LDH sample with a high Ain value was remarkably Iower than that with low Ain value.111e/n vitro CPT release examinations from the nanohybrids showed that the CPT-LDH nanohybrids were a potential drug controlled release system.The kinetic analysis showed that the release kinetics of CPT from the nanohybrids obeyed the pseudo-first order kinetic model and the diffusion Of CPT through the LDH particle Of CPT played an important role in controlling the drug release rate.

  6. Synthesis and in situ mechanism of nuclei growth of layered double hydroxides

    Indian Academy of Sciences (India)

    H S Panda; R Srivastava; D Bahadur

    2011-12-01

    A host–guest material such as layered double hydroxide (LDH) has generated immense interest in current research due to its technological importance, whereby its dimension significantly affect its mechanical and other physical properties. The purpose of this study was to prepare Mg/Al-LDHs by systematically varying the molar concentration of cations, aging time and pH. The prepared LDHs were characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, thermal analysis and transmission electron microscopy to confirm their formation and morphology. We qualitatively observed a new growth route for LDH system which is dissimilar to the existing growth mechanism. The rate of growth is shown to be slower than the well known Ostwald ripening process. This unusual behaviour is due to the formation of effective passivation layer by Na+ ions around the generated LDHs nuclei. This suggested growth mechanism will be helpful in further controlling the particle size of other LDH, which may be useful for various future applications.

  7. Potential for Layered Double Hydroxides-Based, Innovative Drug Delivery Systems

    Directory of Open Access Journals (Sweden)

    Kai Zhang

    2014-04-01

    Full Text Available Layered Double Hydroxides (LDHs-based drug delivery systems have, for many years, shown great promises for the delivery of chemical therapeutics and bioactive molecules to mammalian cells in vitro and in vivo. This system offers high efficiency and drug loading density, as well as excellent protection of loaded molecules from undesired degradation. Toxicological studies have also found LDHs to be biocompatible compared with other widely used nanoparticles, such as iron oxide, silica, and single-walled carbon nanotubes. A plethora of bio-molecules have been reported to either attach to the surface of or intercalate into LDH materials through co-precipitation or anion-exchange reaction, including amino acid and peptides, ATPs, vitamins, and even polysaccharides. Recently, LDHs have been used for gene delivery of small molecular nucleic acids, such as antisense, oligonucleotides, PCR fragments, siRNA molecules or sheared genomic DNA. These nano-medicines have been applied to target cells or organs in gene therapeutic approaches. This review summarizes current progress of the development of LDHs nanoparticle drug carriers for nucleotides, anti-inflammatory, anti-cancer drugs and recent LDH application in medical research. Ground breaking studies will be highlighted and an outlook of the possible future progress proposed. It is hoped that the layered inorganic material will open up new frontier of research, leading to new nano-drugs in clinical applications.

  8. Potential for layered double hydroxides-based, innovative drug delivery systems.

    Science.gov (United States)

    Zhang, Kai; Xu, Zhi Ping; Lu, Ji; Tang, Zhi Yong; Zhao, Hui Jun; Good, David A; Wei, Ming Qian

    2014-01-01

    Layered Double Hydroxides (LDHs)-based drug delivery systems have, for many years, shown great promises for the delivery of chemical therapeutics and bioactive molecules to mammalian cells in vitro and in vivo. This system offers high efficiency and drug loading density, as well as excellent protection of loaded molecules from undesired degradation. Toxicological studies have also found LDHs to be biocompatible compared with other widely used nanoparticles, such as iron oxide, silica, and single-walled carbon nanotubes. A plethora of bio-molecules have been reported to either attach to the surface of or intercalate into LDH materials through co-precipitation or anion-exchange reaction, including amino acid and peptides, ATPs, vitamins, and even polysaccharides. Recently, LDHs have been used for gene delivery of small molecular nucleic acids, such as antisense, oligonucleotides, PCR fragments, siRNA molecules or sheared genomic DNA. These nano-medicines have been applied to target cells or organs in gene therapeutic approaches. This review summarizes current progress of the development of LDHs nanoparticle drug carriers for nucleotides, anti-inflammatory, anti-cancer drugs and recent LDH application in medical research. Ground breaking studies will be highlighted and an outlook of the possible future progress proposed. It is hoped that the layered inorganic material will open up new frontier of research, leading to new nano-drugs in clinical applications.

  9. Zn-Co layered double hydroxide modified hematite photoanode for enhanced photoelectrochemical water splitting

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Dongyu [State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620 (China); Rui, Yichuan [College of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620 (China); Li, Yaogang [Engineering Research Center of Advanced Glasses Manufacturing Technology, MOE, Donghua University, Shanghai 201620 (China); Zhang, Qinghong, E-mail: zhangqh@dhu.edu.cn [State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620 (China); Engineering Research Center of Advanced Glasses Manufacturing Technology, MOE, Donghua University, Shanghai 201620 (China); Wang, Hongzhi, E-mail: wanghz@dhu.edu.cn [State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620 (China)

    2015-12-15

    Graphical abstract: - Highlights: • A facile way to fabricate earth-abundant α-Fe{sub 2}O{sub 3}/Zn-Co LDH composite photoanode via electrodeposition was presented. • The highest photocurrent 1.73 mA/cm{sup 2} at 1.23 V vs RHE was achieved by 60 s electrodeposition (i.e., 36% increment). • EIS indicated the enhanced charge transfer rate comes from improvement of water oxidation. - Abstract: Zinc-cobalt layered double hydroxide (LDH) was electrodeposited on Ti-doped hematite photoanodes for the first time, and a significant enhanced performance for photoelectrochemical water splitting was demonstrated over the composite photoanodes. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and electrochemical impedance spectroscopy (EIS) were characterized with the resulted photoanodes. With the electrodepositing treatment, the photocurrent density increased from 1.27 mA/cm{sup 2} for pristine hematite to 1.73 mA/cm{sup 2} for modified materials at 1.23 V vs. RHE (i.e. 36% improvement). The photocurrent improvement is mainly attributed to a suppression of electron–hole recombination and reduced overpotential for water oxidation at the hematite-electrolyte interface due to the formation of Zn-Co LDH layer on hematite.

  10. Mg-Fe-mixed oxides derived from layered double hydroxides: A study of the surface properties

    Directory of Open Access Journals (Sweden)

    Marinković-Nedučin Radmila P.

    2011-01-01

    Full Text Available The influence of surface properties on the selectivity of the synthesized catalysts was studied, considering that their selectivity towards particular hydrocarbons is crucial for their overall activity in the chosen Fischer- -Tropsch reaction. Magnesium- and iron-containing layered double hydroxides (LDH, with the general formula: [Mg1-xFex(OH2](CO3x/2?mH2O, x = = n(Fe/(n(Mg+n(Fe, synthesized with different Mg/Fe ratio and their thermally derived mixed oxides were investigated. Magnesium was chosen because of its basic properties, whereas iron was selected due to its well-known high Fischer-Tropsch activity, redox properties and the ability to form specific active sites in the layered LDH structure required for catalytic application. The thermally less stable multiphase system (synthesized outside the optimal single LDH phase range with additional Fe-phase, having a lower content of surface acid and base active sites, a lower surface area and smaller fraction of smaller mesopores, showed higher selectivity in the Fischer-Tropsch reaction. The results of this study imply that the metastability of derived multiphase oxides structure has a greater influence on the formation of specific catalyst surface sites than other investigated surface properties.

  11. Mg-Al layered double hydroxide-methotrexate nanohybrid drug delivery system: evaluation of efficacy.

    Science.gov (United States)

    Chakraborty, Jui; Roychowdhury, Susanta; Sengupta, Somoshree; Ghosh, Swapankumar

    2013-05-01

    Mg-Al layered double hydroxide nanoparticles were synthesized by one-pot co-precipitation method and anticancerous drug methotrexate was incorporated into it by in-situ ion exchange. The LDH-MTX nanohybrid produced moderately stable suspension in water, as predicted by zeta potential measurement. X-ray diffraction revealed that the basal spacing increased to nearly twice the same for pristine LDH on MTX intercalation. Thermogravimetric analyses confirmed an increase in thermal stability of the intercalated drug in the LDH framework. A striking enhancement in efficacy/sensitivity of MTX on the HCT-116 cells was obtained when intercalated within the LDH layers, as revealed by the attainment of half maximal inhibitory concentration of LDH-MTX nanohybrid by 48 h, whereas, bare MTX required 72 h for the same. The MTX release from MgAl-LDH-MTX hybrids in phosphate buffer saline at pH7.4 followed a relatively slow, first order kinetics and was complete within 8 days following diffusion and crystal dissolution mechanism.

  12. In Situ Hybridization of Pulp Fibers Using Mg-Al Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Carl-Erik Lange

    2015-04-01

    Full Text Available Inorganic Mg2+ and Al3+ containing layered double hydroxide (LDH particles were synthesised in situ from aqueous solution onto chemical pulp fibers of pine (Pinus sylvestris. High super saturated (hss solution with sodium carbonate produced LDH particles with an average diameter of 100–200 nm. Nano-size (70 nm LDH particles were found from fibers external surface and, to a lesser degree, from the S2 cell wall after synthesis via low super saturated (lss route. The synthesis via slow urea hydrolysis (Uhyd yielded micron and clay sized LDH (2–5 μm and enabled efficient fiber densification via mineralization of S2 fiber wall layer as indicated by TEM and compliance analysis. The Uhyd method decreased fiber compliance up to 50%. Reduction in the polymerisation degree of cellulose was observed with capillary viscometry. Thermogravimetric analysis showed that the hybridization with LDH reduced the exothermic heat, indicating, that this material can be incorporated in flame retardant applications. Fiber charge was assessed by Fibers 2015, 3 104 adsorption expermients with methylene blue (MB and metanil yellow (MY. Synthesis via lss route retained most of the fibres original charge and provided the highest capacity (10 μmol/g for anionic MY, indicating cationic character of hybrid fibers. Our results suggested that mineralized fibers can be potentially used in advanced applications such as biocomposites and adsorbent materials.

  13. Synthesis, structure and photocatalytic activity of calcined Mg-Al-Ti-layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Hosni, Khaled; Abdelkarim, Omar; Srasra, Ezzeddine [Centre National des Recherches en Sciences des Matériaux (CNRSM), Soliman (Turkey); Frini-Srasra, Najoua [Faculté des Sciences de Tunis (FST), Tunis (Turkey)

    2015-01-15

    Mg-Al-Ti layered double hydroxides (LDH), consisting of di-, tri- and tetra-valent cations with different Al{sup 3+}/Ti{sup 4+} ratio, have been synthesized by co-precipitation which was demonstrated as efficient visible-light photocatalysts. The structure and chemical composition of the compound were characterized by PXRD, FT-IR, SAA, N{sub 2} adsorption-desorption isotherms, and DSC techniques. It is found that no hydrotalcites structure were formed for Ti{sup 4+}/(Ti{sup 4+}+ Al{sup 3+})>0.5 and the substitution of Ti(IV) for Al(III) in the layer increases the thermal stability of the resulting LDH materials. The calcined sample containing titanium showed relatively high adsorption capacity for MB as compared to that without titanium. Results show that the pseudo-second-order kinetic model and the Langmuir were found to correlate the experimental data well. The photocatalytic activity was evaluated for the degradation of the methylene blue. The photocatalytic activity increased with the increase of the Al/Ti cationic ratio. 71% of the dye could be removed by the Mg/Al/Ti-LDH with the cationic ratio Al/Ti=0 : 1 and calcined at 500 .deg. C.

  14. In situ dielectric measurements of Zn?Al layered double hydroxide with anionic nitrate ions

    Science.gov (United States)

    Ahmed, Abdullah Ahmed Ali; Talib, Zainal Abidin; Hussein, Mohd Zobir bin; Zakaria, Azmi

    2012-08-01

    Zn-Al-NO3-layered double hydroxide (Zn-Al-NO3-LDH) was prepared by the co-precipitation method with a ratio of Zn/Al = 4 and at a constant pH of 7. Powder XRD patterns showed the characteristic peaks of layered structure of the LDH sample. Thermogravimetric analysis (TGA) and infrared spectra of the sample were investigated. Because of the existence of water molecules and anionic NO3- in the interlayer of the LDH, the in situ dielectric spectroscopy of the LDH can be described by an anomalous low frequency dispersion using the second type of Universal Power Law. Novel measurements of activation energy of LDH have been obtained at five different frequencies. The energy value increased from 0.05 eV at 1 MHz to 0.37 eV at 134 Hz. The conductivity spectra of sample were studied as a function in temperature of the in situ measurements. The ionic conductivity (dc) of LDH increased as the in situ temperature increased.

  15. Visions of Reconstruction: Layers of Moving Images

    NARCIS (Netherlands)

    Paalman, Floris Jan Willem

    2015-01-01

    abstractAfter WWII, films accompanied the reconstruction of Europe’s destroyed cities. Many contained historical footage. How was this material used, to articulate visions of reconstruction, what happened to the material later on, and how do the films relate to municipal film archives? This question

  16. Photocatalytic property and structural stability of CuAl-based layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Lv, Ming; Liu, Haiqiang, E-mail: Liuhaiqiang1980@126.com

    2015-07-15

    Three types of CuMAl layered double hydroxides (LDHs, M=Mg, Zn, Ni) were successfully synthesized by coprecipitation. Powder X-ray diffraction (XRD), inductively coupled plasma atomic emission spectrometry (ICP-AES) and UV–Vis diffuse reflectance spectrum (UV–vis) were used to confirm the formation of as-synthesized solids with good crystal structure. The photocatalytic activity of those LDH materials for CO{sub 2} reduction under visible light was investigated. The experimental results show that CuNiAl-LDHs with narrowest band gap and largest surface areas behave highest efficiency for methanol generation under visible light compared with CuMgAl-LDHs and CuZnAl-LDHs. The CuNiAL-LDH showed high yield for methanol production i.e. 0.210 mmol/g h, which was high efficient. In addition, the influence of the different M{sup 2+} on the structures and stability of the CuMAl-LDHs was also investigated by analyzing the geometric parameters, electronic arrangement, charge populations, hydrogen-bonding, and binding energies by density functional theory (DFT) analysis. The theoretical calculation results show that the chemical stability of LDH materials followed the order of CuMgAl-LDHs>CuZnAl-LDHs>CuNiAl-LDHs, which is just opposite with the photocatalytic activity and band gaps of three materials. - Graphical abstract: The host–guest calculation models and XRD patterns of CuMAl-LDHs: CuMgAl-LDHs (a), CuZnAl-LDHs (b) and CuNiAl-LDHs (c). - Highlights: • Three types of CuMAl layered double hydroxides (LDHs, M=Mg, Zn, Ni) has been synthesized. • CuMgNi shows narrower band gap and more excellent textural properties than other LDHs. • The band gap: CuMgAl

  17. Electrospun fibers of layered double hydroxide/biopolymer nanocomposites as effective drug delivery systems

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yue-E.; Zhu Hong; Chen Dan; Wang Ruiyu [State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200433 (China); Tjiu, Weng Weei [Institute of Materials Research and Engineering, A-STAR (Agency for Science, Technology and Research), 3 Research Link, Singapore 117602 (Singapore); Liu Tianxi, E-mail: txliu@fudan.edu.cn [State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200433 (China)

    2012-06-15

    Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on a combination of LDH-IBU with two kinds of biopolymers (i.e. PCL and PLA), to act as effective drug delivery systems. Ibuprofen (IBU) is chosen as a model drug, which is intercalated in MgAl-LDH by coprecipitation. Poly(oxyethylene-b-oxypropylene-b-oxyethylene) (Pluronic) is also added into PLA-based fibers as hydrophilicity enhancer and release modulator. LDH-IBU nanoparticles are uniformly dispersed throughout the nanocomposite fibers, as evidenced by transmission electron microscopy (TEM) observations. In vitro drug release studies show that initial IBU liberation from LDH-IBU/PCL composite fibers is remarkably slower than that from IBU/PCL fibers due to the sustained release property of LDH-IBU and heterogeneous nucleation effect of LDH-IBU on PCL chain segments. Surprisingly, the initial IBU release from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers is faster than that from the corresponding IBU/PLA and IBU/PLA/Pluronic fibers. This effect can be attributed to the strong interaction between alkyl groups in IBU molecules and methyl substituent groups of PLA as well as the hydrophilicity of LDH-IBU, which lead to an easier diffusion of water with a faster release of IBU from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers. - Graphical abstract: Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on the combination of LDHs with two kinds of biopolymers (i.e. PCL and PLA). LDH-IBU nanoparticles are uniformly dispersed throughout all the electrospun nanocomposite fibers even at a high loading level of 5 wt%. By combining the tunable drug release property of LDHs and electrospinning technique, the new drug delivery system is anticipated for effective loading and sustained release of drugs

  18. Treatment with coated layer double hydroxide clays decreases the toxicity of copper-contaminated water.

    Science.gov (United States)

    Blake, Deanne; Nar, Mangesh; D'Souza, Nandika Anne; Glenn, J Brad; Klaine, Stephen J; Roberts, Aaron P

    2014-05-01

    Copper is a common pollutant found in watersheds that exerts toxic effects on both invertebrates and vertebrates. Layer double hydroxide (LDH) clays are able to adsorb a wide range of contaminants through ion-exchange mechanisms. Coating LDH clays with various materials alters the aggregation of clay particles into the nano-size range, thus increasing relative surface area and offering great potential for contaminant remediation. The goal of this study was to determine if treatment with coated LDH clays decreases the toxicity of copper-containing solutions to Daphnia magna. Four LDH clays with different coatings used to alter hydrophobicity were as follows: used: Na(+) montmorillonite, Zn-Al LDH-nitrate, Zn-Al LDH-stearate, and Zn-Al LDH-carbonate. It was determined that coated LDH clays decreased copper toxicity by decreasing bioavailability and that smaller aggregate sizes decreased bioavailability the most. 96 h LC50 values increased by as much as 4.2 times with the treatment of the solutions with 100 mg/L LDH clay. Copper analysis of the clay and solutions indicated that the clays work by decreasing copper bioavailability by way of a binding mechanism. Coated LDH clays hold promise as a small-scale remediation tool or as an innovative tool for toxicity identification and evaluation characterization of metals.

  19. Bacteria encapsulated in layered double hydroxides: towards an efficient bionanohybrid for pollutant degradation.

    Science.gov (United States)

    Halma, Matilte; Mousty, Christine; Forano, Claude; Sancelme, Martine; Besse-Hoggan, Pascale; Prevot, Vanessa

    2015-02-01

    A soft chemical process was successfully used to immobilize Pseudomonas sp. strain ADP (ADP), a well-known atrazine (herbicide) degrading bacterium, within a Mg2Al-layered double hydroxide host matrix. This approach is based on a simple, quick and ecofriendly direct coprecipitation of metal salts in the presence of a colloidal suspension of bacteria in water. It must be stressed that by this process the mass ratio between inorganic and biological components was easily tuned ranging from 2 to 40. This ratio strongly influenced the biological activity of the bacteria towards atrazine degradation. The better results were obtained for ratios of 10 or lower, leading to an enhanced atrazine degradation rate and percentage compared to free cells. Moreover the biohybrid material maintained this biodegradative activity after four cycles of reutilization and 3 weeks storage at 4°C. The ADP@MgAl-LDH bionanohybrid materials were completely characterized by X-ray diffraction (XRD), FTIR spectroscopy, thermogravimetric analysis and scanning and transmission electronic microscopy (SEM and TEM) evidencing the successful immobilization of ADP within the inorganic matrix. This synthetic approach could be readily extended to other microbial whole-cell immobilization of interest for new developments in biotechnological systems.

  20. Antibacterial carboxymethyl cellulose/Ag nanocomposite hydrogels cross-linked with layered double hydroxides.

    Science.gov (United States)

    Yadollahi, Mehdi; Namazi, Hassan; Aghazadeh, Mohammad

    2015-08-01

    This paper deals with the preparation of antibacterial nanocomposite hydrogels through the combination of carboxy methyl cellulose (CMC), layered double hydroxides (LDH), and silver nanoparticles (AgNPs). CMC-LDH hydrogels were prepared by intercalating CMC into different LDHs. Then, Ag/CMC-LDH nanocomposite hydrogels were prepared through in situ formation of AgNPs within the CMC-LDHs. XRD analysis confirmed the intercalating CMC into the LDH sheets and formation of intercalated structures, as well as formation of AgNPs within the CMC-LDHs. SEM and TEM micrographs indicated well distribution of AgNPs within the Ag/CMC-LDHs. The prepared hydrogels showed a pH sensitive swelling behavior. The Ag/CMC-LDH nanocomposite hydrogels have rather higher swelling in different aqueous solutions in comparison with CMC-LDHs. The antibacterial activity of CMC-LDHs increased considerably after formation of AgNPs and was stable for more than one month. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Methotrexatum intercalated layered double hydroxides: statistical design, mechanism explore and bioassay study.

    Science.gov (United States)

    Wang, Xiao-Feng; Liu, Su-Qing; Li, Shu-Ping

    2015-04-01

    A series of methotrexatum intercalated layered double hydroxide (MTX/LDH for short) hybrids have been synthesized by a mechanochemical-hydrothermal method, the statistical experiments are planned and conducted to find out the critical factor influencing the physicochemical properties. Four variables, i.e., addition of NaOH solution, grinding duration, hydrothermal temperature and time, are chosen to play as the examined factors in the orthogonal design. Furthermore, three respective levels, i.e., high, medium and low levels, are conducted in the design. The resulting hybrids are then characterized by X-ray diffraction (XRD) patterns, transmission electron microscope (TEM) graphs and Zeta potentials. XRD diffractions indicate that MTX anions have been successfully intercalated into LDH interlayers and the amount of NaOH solution can change the gallery height greatly. The information from TEM graphs and Zeta potentials state that the increase of alkali solution gives rise to regular morphology and the increase of Zeta potentials. As a result of the statistical analysis, addition of alkali solution is the major factor affecting the morphology and drug-loading capacity. At last, the mechanism of particle growth is explored emphatically, and the anticancer efficacy of some MTX/LDH hybrids is estimated by MTT assay on A549 cells as well.

  2. Comparative study of the coprecipitation methods for the preparation of Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Crepaldi Eduardo L.

    2000-01-01

    Full Text Available Coprecipitation is the method most frequently applied to prepare Layered Double Hydroxides (LDHs. Two variations of this method can be used, depending on the pH control conditions during the precipitation step. In one case the pH values are allowed to vary while in the other they are kept constant throughout coprecipitation. Although research groups have their preferences, no systematic comparison of the two variations of the coprecipitation method is available in the literature. On this basis, the objective of the present study was to compare the properties of LDHs prepared using the two forms of pH control in the coprecipitation method. The results showed that even though coprecipitation is easier to perform under conditions of variable pH values, materials with more interesting properties, from the point of view of technological applications, are obtained at constant pH. Higher crystallinity, smaller particle size, higher specific surface area and higher average pore diameter were found for materials obtained by coprecipitation at constant pH, when compared to the materials obtained at variable pH.

  3. Controlled supramolecular structure of guanosine monophosphate in the interlayer space of layered double hydroxide

    Directory of Open Access Journals (Sweden)

    Gyeong-Hyeon Gwak

    2016-12-01

    Full Text Available Guanosine monophosphates (GMPs were intercalated into the interlayer space of layered double hydroxides (LDHs and the molecular arrangement of GMP was controlled in LDHs. The intercalation conditions such as GMP/LDH molar ratio and reaction temperature were systematically adjusted. When the GMP/LDH molar ratio was 1:2, which corresponds to the charge balance between positive LDH sheets and GMP anions, GMP molecules were well-intercalated to LDH. At high temperature (100 and 80 °C, a single GMP molecule existed separately in the LDH interlayer. On the other hand, at lower temperature (20, 40 and 60 °C, GMPs tended to form ribbon-type supramolecular assemblies. Differential scanning calorimetry showed that the ribbon-type GMP assembly had an intermolecular interaction energy of ≈101 kJ/mol, which corresponds to a double hydrogen bond between guanosine molecules. Once stabilized, the interlayer GMP orientations, single molecular and ribbon phase, were successfully converted to the other phase by adjusting the external environment by stoichiometry or temperature control.

  4. Preparation of layered double hydroxide/chlorophyll a hybrid nano-antennae: a key step.

    Science.gov (United States)

    Sommer Márquez, Alicia E; Lerner, Dan A; Fetter, Geolar; Bosch, Pedro; Tichit, Didier; Palomares, Eduardo

    2014-07-21

    In the first step to obtain an efficient nano-antenna in a bottom-up approach, new hybrid materials were synthesized using a set of layered double hydroxides (LDHs) with basic properties and pure chlorophyll a (Chl a). The stability of the adsorbed monolayer of Chl a was shown to be dependent on the nature and the ratio of the different metal ions present in the LDHs tested. The hybrid materials turned out to be adequate for stabilizing Chl a on Mg/Al LDHs for more than a month under ambient conditions while a limited catalytic decomposition was observed for the Ni/Al LDHs leading to the formation of pheophytin. These changes were followed by namely XRD, DR-UV-vis and fluorescence spectroscopies of the hybrid antennae and of the solutions obtained from their lixiviation with acetone or diethylether. On Mg/Al hydrotalcites the stability of the adsorbed Chl a was equivalent for values of the metal atom ratio ranging from 2 to 4. The latter hybrids should constitute a good basis to form efficient nanoscale light harvesting units following intercalation of selected dyes. This work describes an efficient preparation of Chl a that allows scale-up as well as the obtention of a stable Chl a monolayer on the surface of various LDHs.

  5. NONISOTHERMAL CRYSTALLIZATION AND MORPHOLOGY OF POLY(BUTYLENE SUCCINATE)/LAYERED DOUBLE HYDROXIDE NANOCOMPOSITES

    Institute of Scientific and Technical Information of China (English)

    Mei-qiu Zhan; Guang-yi Chen; Zhi-yong Wei; Yu-mei Shi; Wan-xi Zhang

    2013-01-01

    Biodegradable poly(butylene succinate) (PBS) and layered double hydroxide (LDH) nanocomposites were prepared via melt blending in a twin-screw extruder.The morphology and dispersion of LDH nanoparticles within PBS matrix were characterized by transmission electron microscopy (TEM),which showed that LDH nanoparticles were found to be well distributed at the nanometer level.The nonisothermal crystallization behavior of nanocomposites was extensively studied using differential scanning calorimetry (DSC) technique at various cooling rates.The crystallization rate of PBS was accelerated by the addition of LDH due to its heterogeneous nucleation effect; however,the crystallization mechanism and crystal structure of PBS remained almost unchanged.In kinetics analysis of nonisothermal crystallization,the Ozawa approach failed to describe the crystallization behavior of PBS/LDH nanocomposites,whereas both the modified Avrami model and the Mo method well represented the crystallization behavior of nanocomposites.The effective activation energy was estimated as a function of the relative degree of crystallinity using the isoconversional analysis.The subsequent melting behavior of PBS and PBS/LDH nanocomposites was observed to be dependent on the cooling rate.The POM showed that the small and less perfect crystals were formed in nanocomposites.

  6. Aluminium substitution in iron(II III)-layered double hydroxides: Formation and cationic order

    Science.gov (United States)

    Ruby, Christian; Abdelmoula, Mustapha; Aissa, Rabha; Medjahdi, Ghouti; Brunelli, Michela; François, Michel

    2008-09-01

    The formation and the modifications of the structural properties of an aluminium-substituted iron(II-III)-layered double hydroxide (LDH) of formula Fe4IIFe(2-6y)IIIAl6yIII (OH) 12 SO 4, 8H 2O are followed by pH titration curves, Mössbauer spectroscopy and high-resolution X-ray powder diffraction using synchrotron radiation. Rietveld refinements allow to build a structural model for hydroxysulphate green rust, GR(SO 42-), i.e. y=0, in which a bilayer of sulphate anions points to the Fe 3+ species. A cationic order is proposed to occur in both GR(SO 42-) and aluminium-substituted hydroxysulphate green rust when yhydroxides. Adsorption of more soluble Al III species onto the initially formed ferric oxyhydroxide may be responsible for this slowdown of crystal growth. Therefore, the insertion of low aluminium amount ( y˜0.01) could be an interesting way for increasing the surface reactivity of iron(II-III) LDH that maintains constant the quantity of the reactive Fe II species of the material.

  7. Computer simulation of interlayer arrangement in cinnamate intercalated layered double hydroxides

    Science.gov (United States)

    Greenwell, H. C.; Jones, W.; Newman, S. P.; Coveney, P. V.

    2003-02-01

    The interlayer arrangements of Mg-Al layered double hydroxides (LDHs) containing trans-cinnamate anions have been studied using molecular dynamics computer simulations. A modified version of the Dreiding forcefield was used to perform simulations of models with Mg/Al ratios of 2,3 and 6. For each Mg/Al ratio, two hydration states of 20 and 30 wt% water content were modelled. Close contacts between the olefinic carbons of the anion were analysed in an attempt to rationalize the potential outcome of the [2+2] photo-induced dimerization of the anions. In all instances, except for the model with Mg/Al=6 and 20 wt% water, the arrangement of the dimer pairs showed that syn-head-to-tail dimer formation was unfavourable. Preferred orientation of dimer pairs towards formation of head-to-head dimers was observed to undergo a transition from strongly favouring the syn-head-to-head dimer at low Mg/Al ratios to greater selectivity for the anti-head-to-head dimer with increasing Mg/Al ratio. The model with Mg/Al=6 and 20 wt% water content was observed to have a very disordered interlayer arrangement, with preference towards anion-pair arrangements favouring syn-head-to-tail dimer formation. The model with Mg/Al=6 and 30 wt% water content was predicted to exhibit only trans- cis isomerisation.

  8. Study on the adsorption of DNA on the layered double hydroxides (LDHs)

    Science.gov (United States)

    Li, Bin; Wu, Pingxiao; Ruan, Bo; Liu, Paiyu; Zhu, Nengwu

    2014-03-01

    Four kinds of layered double hydroxides (LDHs) were prepared by chemical coprecipitation method and used as DNA adsorbents. Multiple characterization tools such as power X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and Standard electronic modules (SEM) were employed to characterize the LDHs. By examining the effect of initial concentration, solution pH, adsorption experiments were carried out to investigate the adsorption capacities of LDHs for DNA. The results revealed that the LDHs with Mg/Al = 3 had higher ability on adsorbing the DNA and were not affected by pH values. The LDHs exhibited excellent adsorption properties and completely adsorbed DNA within 2 h. The adsorption equilibrium data were fitted to the Langmuir and Freundlich models, showing that the Langmuir model which represented monolayer adsorption had better correlation with the adsorption linear equation. In addition, Circular dichroism (CD) spectrum, UV-vis spectorscopy and agarose gel electrophoresis revealed the integrity of DNA structure, suggesting that there had no damage on the DNA structure during the adsorption process.

  9. Layered Double Hydroxide Modified by PEGylated Hyaluronic Acid as a Hybrid Nanocarrier for Targeted Drug Delivery

    Institute of Scientific and Technical Information of China (English)

    董岸杰; 李雪; 王伟伟; 韩尚聪; 刘鉴锋; 刘金剑; 赵军强; 许舒欣; 邓联东

    2016-01-01

    In recent years, organic-inorganic hybrid nanocarriers are explored for effective drug delivery and pref-erable disease treatments. In this study, using 5-fluorouracil(5-FU)as electronegative model drug, a new type of organic-inorganic hybrid drug delivery system(LDH/HA-PEG/5-FU)was conceived and manufactured by the ad-sorption of PEGylated hyaluronic acid(HA-PEG)on the surface of layered double hydroxide(LDH, prepared via hydrothermal method)and the intercalation of 5-FU in the interlamination of LDH via ion exchange strategy. The drug loading amount of LDH/HA-PEG/5-FU achieved as high as 34.2%. LDH, LDH/5-FU and LDH/HA-PEG/5-FU were characterized by FT-IR, XRD, TGA, laser particle size analyzer and SEM. With the benefit of pH-degradable feature of LDH and enzyme-degradable feature of HA, LDH/HA-PEG/5-FU showed pH-degradable and enzyme-degradable capacity inin vitro drug release. Moreover, the drug carrier LDH/HA-PEG contained biocom-patible PEG and tumor-targeted HA, resulting in lower cytotoxicity and better endocytosis compared with LDHin vitro. It was suggested that the organic-inorganic hybrid drug delivery system, which was endowed with the proper-ties of controlled release, low toxicity and tumor-targeting delivery for ameliorative cancer therapy, was advisable and might be applied further to fulfill other treatments.

  10. Synthesis and characterization of 10-hydroxycamptothecin - sebacate - layered double hydroxide nanocomposites

    Science.gov (United States)

    Pang, Xiujiang; Ma, Xiuming; Li, Dongxiang; Hou, Wanguo

    2013-02-01

    10-Hydroxycamptothecin (HCPT) as a hydrophobic anticancer drug brings many challenges in the clinical applications due to its poor water solubility and the presence of a chemically unstable lactone ring. In this work, the nanocomposites of HCPT intercalated layered double hydroxide (LDH) were prepared by a secondary intercalation method, and the encapsulated HCPT could keep the biologically active lactone form. A Zn-Al-NO3 LDH was pillared with sebacate anions by a co-precipitation method in an aqueous medium, and then HCPT was intercalated into the LDH's gallery via hydrophobic interaction in an ethanol medium. The parallel alkyl chains of perpendicularly arranged sebacate anions in the LDH gallery provide a hydrophobic space for the drug intercalation. The in vitro release kinetics of HCPT from the nanocomposites could be fitted with the pseudo-second-order kinetic model, and the diffusion of HCPT through the LDH particles played an important role in controlling the drug release. The nanocomposites can be considered as a potential drug delivery system.

  11. Polymer Coated CaAl-Layered Double Hydroxide Nanomaterials for Potential Calcium Supplement

    Directory of Open Access Journals (Sweden)

    Tae-Hyun Kim

    2014-12-01

    Full Text Available We have successfully prepared layered double hydroxide (LDH nanomaterials containing calcium and aluminum ions in the framework (CaAl-LDH. The surface of CaAl-LDH was coated with enteric polymer, Eudragit®L 100 in order to protect nanomaterials from fast dissolution under gastric condition of pH 1.2. The X-ray diffraction patterns, Fourier transform infrared spectroscopy, scanning electron and transmission electron microscopy revealed that the pristine LDH was well prepared having hydrocalumite structure, and that the polymer effectively coated the surface of LDH without disturbing structure. From thermal analysis, it was determined that only a small amount (less than 1% of polymer was coated on the LDH surface. Metal dissolution from LDH nanomaterials was significantly reduced upon Eudragit®L 100 coating at pH 1.2, 6.8 and 7.4, which simulates gastric, enteric and plasma conditions, respectively, and the dissolution effect was the most suppressed at pH 1.2. The LDH nanomaterials did not exhibit any significant cytotoxicity up to 1000 μg/mL and intracellular calcium concentration significantly increased in LDH-treated human intestinal cells. Pharmacokinetic study demonstrated absorption efficiency of Eudragit®L 100 coated LDH following oral administration to rats. Moreover, the LDH nanomaterials did not cause acute toxic effect in vivo. All the results suggest the great potential of CaAl-LDH nanomaterials as a calcium supplement.

  12. Nanocomposites of Magnetite and Layered Double Hydroxide for Recyclable Chromate Removal

    Directory of Open Access Journals (Sweden)

    Gyeong-Hyeon Gwak

    2016-01-01

    Full Text Available Nanocomposites containing magnetic iron oxide (magnetite nanoparticles and layered double hydroxide (LDH nanosheets were prepared by two different methods, exfoliation-reassembly and coprecipitation, for aqueous chromate adsorbent. According to X-ray diffraction, scanning electron microscopy, and atomic force microscopy, both nanocomposites were determined to develop different nanostructures; LDH nanosheets well covered magnetite nanoparticles with house-of-cards-like structure in exfoliation-reassembly method, while coprecipitation resulted in LDH particle formation along with magnetite nanoparticles. Zeta-potential measurement also revealed that the magnetite surface was effectively covered by LDH moiety in exfoliation-reassembly compared with coprecipitation. Time, pH, concentration dependent chromate adsorption tests, and magnetic separation experiments exhibited that both nanocomposites effectively adsorb and easily collect chromate. However, exfoliation-reassembly nanocomposite was determined to be slightly effective in chromate removal by ~10%. Chromate adsorbed nanocomposites could be regenerated by treating with bicarbonate and the regenerated nanocomposites preserved ~80% of chromate adsorption efficacy after three times of recycling.

  13. Methotrexate intercalated layered double hydroxides with the mediation of surfactants: Mechanism exploration and bioassay study

    Energy Technology Data Exchange (ETDEWEB)

    Dai, Chao-Fan; Tian, De-Ying; Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn; Li, Xiao-Dong

    2015-12-01

    Methotrexatum intercalated layered double hydroxides (MTX/LDHs) hybrids were synthesized by the co-precipitation method and three kinds of nonionic surfactants with different hydrocarbon chain lengths were used. The resulting hybrids were then characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM). XRD and FTIR investigations manifest the successful intercalation of MTX anions into the interlayer of LDHs. TEM graphs indicate that the morphology of the hybrids changes with the variation of the chain length of the surfactants, i.e., the particles synthesized using polyethylene glycol (PEG-7) present regular disc morphology with good monodispersity, while samples with the mediation of alkyl polyglycoside (APG-14) are heavily aggregated and samples with the addition of polyvinylpyrrolidone (PVP-10) exhibit irregular branches. Furthermore, the release and bioassay experiments show that monodisperse MTX/LDHs present good controlled-release and are more efficient in the suppression of the tumor cells. - Highlights: • Surfactants could be used to modify the dispersing state of MTX/LDHs hybrids. • Surfactants have great effect on the morphology of MTX/LDHs hybrids. • MTX/LDHs with good monodisperse degree are more efficient in the suppression of the tumor cells.

  14. Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z. [Department of Organic Chemistry, University of Szeged, Dóm tér 8, Szeged H-6720 (Hungary); Materials and Solution Structure Research Group, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, Szeged H-6720 (Hungary); Kukovecz, Á. [Department of Applied and Environmental Chemistry, University of Szeged, Rerrich Béla tér 1, Szeged H-6720 (Hungary); MTA-SZTE “Lendület” Porous Nanocomposites Research Group, Rerrich Béla tér 1, Szeged H-6720 (Hungary); Kónya, Z. [Department of Applied and Environmental Chemistry, University of Szeged, Rerrich Béla tér 1, Szeged H-6720 (Hungary); MTA-SZTE Reaction Kinetics and Surface Chemistry Research Group, Rerrich Béla tér 1, Szeged H-6720 (Hungary); Carlson, S. [MAX IV Laboratory, Ole Römers väg 1, Lund SE-223 63 (Sweden); Sipos, P. [Materials and Solution Structure Research Group, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, Szeged H-6720 (Hungary); Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, Szeged H-6720 (Hungary); and others

    2016-01-15

    A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.

  15. Vapor phase hydrogenation of furfural over nickel mixed metal oxide catalysts derived from layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Sulmonetti, Taylor P.; Pang, Simon H.; Claure, Micaela Taborga; Lee, Sungsik; Cullen, David A.; Agrawal, Pradeep K.; Jones, Christopher W.

    2016-05-01

    The hydrogenation of furfural is investigated over various reduced nickel mixed metal oxides derived from layered double hydroxides (LDHs) containing Ni-Mg-Al and Ni-Co-Al. Upon reduction, relatively large Ni(0) domains develop in the Ni-Mg-Al catalysts, whereas in the Ni-Co-Al catalysts smaller metal particles of Ni(0) and Co(0), potentially as alloys, are formed, as evidenced by XAS, XPS, STEM and EELS. All the reduced Ni catalysts display similar selectivities towards major hydrogenation products (furfuryl alcohol and tetrahydrofurfuryl alcohol), though the side products varied with the catalyst composition. The 1.1Ni-0.8Co-Al catalyst showed the greatest activity per titrated site when compared to the other catalysts, with promising activity compared to related catalysts in the literature. The use of base metal catalysts for hydrogenation of furanic compounds may be a promising alternative to the well-studied precious metal catalysts for making biomass-derived chemicals if catalyst selectivity can be improved in future work by alloying or tuning metal-oxide support interactions.

  16. The reduction of chromate ions by Fe(II layered hydroxides

    Directory of Open Access Journals (Sweden)

    S. Loyaux-Lawniczak

    1999-01-01

    Full Text Available The reduction of chromate ions by Fe(OH2 and the iron (II-iron (III hydroxysulphate green rust, GR(SO42-, was studied to evaluate whether such synthetic layered hydroxides and the corresponding natural green rust mineral could be involved in the natural attenuation of contaminated environments. The resulting Cr (III bearing phases, which would govern the subsequent behaviour of chromium, were clearly characterised. Both compounds proved to be very reactive and oxidised instantaneously while chromate ions were reduced to Cr (III as evidenced by X-ray photoelectron spectroscopy. Mass balance (ICP-AES demonstrated that the Fe/Cr ratio inside the solid end product was equal to the initial Fe/Cr ratio. The solid phases, analysed by X-ray diffraction, Raman and Mossbauer spectroscopies were identified as Cr-substituted poorly crystallised iron (III oxyhydroxides in both cases, more precisely δ-FeOOH when starting with Fe(OH2 and ferrihydrite when starting with GR(SO42-.

  17. Anion-intercalated layered double hydroxides modified test strips for detection of heavy metal ions.

    Science.gov (United States)

    Wang, Nan; Sun, Jianchao; Fan, Hai; Ai, Shiyun

    2016-01-01

    In this work, a novel approach for facile and rapid detection of heavy metal ions using anion-intercalated layered double hydroxides (LDHs) modified test strips is demonstrated. By intercalating Fe(CN)6(4-) or S(2-) anions into the interlayers of LDHs on the filter paper, various heavy metal ions can be easily detected based on the color change before and after reaction between the anions and the heavy metal ions. Upon the dropping of heavy metal ions solutions to the test strips, the colors of the test strips changed instantly, which can be easily observed by naked eyes. With the decrease of the concentration, the color depth changed obviously. The lowest detection concentration can be up to 1×10(-6) mol L(-1). Due to the easily intercalation of anions into the interlayer of the LDHs on test trips, this procedure provides a general method for the construction of LDHs modified test strips for detection of heavy metal ions. The stability of the prepared test strips is investigated. Furthermore, all the results were highly reproducible. The test strips may have potential applications in environmental monitoring fields.

  18. Ionic elastomers based on carboxylated nitrile rubber (XNBR and magnesium aluminum layered double hydroxide (hydrotalcite

    Directory of Open Access Journals (Sweden)

    A. Laskowska

    2014-06-01

    Full Text Available The presence of carboxyl groups in carboxylated nitrile butadiene rubber (XNBR allows it to be cured with different agents. This study considers the effect of crosslinking of XNBR by magnesium aluminum layered double hydroxide (MgAl-LDH, known also as hydrotalcite (HT, on rheometric, mechano-dynamical and barrier properties. Results of XNBR/HT composites containing various HT loadings without conventional curatives are compared with XNBR compound crosslinked with commonly used zinc oxide. Hydrotalcite acts as an effective crosslinking agent for XNBR, as is particularly evident from rheometric and Fourier transform infrared spectroscopy (FTIR studies. The existence of ionic crosslinks was also detected by dynamic mechanical analysis (DMA of the resulting composites. DMA studies revealed that the XNBR/HT composites exhibited two transitions – one occurring at low temperature is associated to the Tg of elastomer and the second at high temperature corresponds to the ionic transition temperature Ti. Simultaneous application of HT as a curing agent and a filler may deliver not only environmentally friendly, zinc oxide-free rubber product but also ionic elastomer composite with excellent mechanical, barrier and transparent properties.

  19. Structure and photoluminescence of Mg-Al-Eu ternary hydrotalcite-like layered double hydroxides

    Science.gov (United States)

    Chen, Yufeng; Li, Fei; Zhou, Songhua; Wei, Junchao; Dai, Yanfeng; Chen, Yiwang

    2010-09-01

    A series of Mg-Al-Eu ternary hydrotalcite-like layered double hydroxides (LDHs), with Eu/Al atomic ratios of ˜0.06 and Mg/(Al+Eu) atomic ratios ranging from 1.3 to 4.0, were synthesized by a coprecipitation method. The Mg-Al-Eu ternary LDHs were investigated by various techniques. X-ray diffraction (XRD) results indicated that the crystallinity of the ternary LDHs was gradually improved with the increase of Mg 2+/(Al 3++Eu 3+) molar ratio from 1.3/1 to 4/1, and all the samples were a single phase corresponding to LDH. The photoluminescent (PL) spectra of the ternary Mg-Al-Eu LDHs were described by the well-known 5D0- 7FJ transition ( J=1, 2, 3, 4) of Eu 3+ ions with the strongest emission for J=2, suggesting that the host LDH was favorable to the emissions of Eu 3+ ions. The asymmetry parameter ( R) relevant to 5D0- 7FJ transition ( J=1, 2) dependant of the atomic ratios of Mg 2+/(Al 3++Eu 3+) was discussed, and was consistent with the result of XRD.

  20. Potential Applications of Hybrid Layered Double Hydroxide (LDH Particles in Pulp and Paper Production

    Directory of Open Access Journals (Sweden)

    Sophia von Haartman

    2014-03-01

    Full Text Available Functionalization of papermaking pulp fibers using inorganic particles was investigated as a novel approach. Different layered double hydroxide (LDH particles were used in peroxide bleaching of thermomechanical pulp (TMP and in oxygen bleaching of eucalyptus kraft pulp. LDH particles were also tested as binding sites for optical brightening agents (OBA that are commonly used in paper production. The surface chemistry of LDH-treated pulps was examined using X-ray photoelectron spectroscopy (XPS and apparent contact angle with water. Adsorbed LDH was not detected by XPS on the fiber surfaces after the bleaching trials, but it had a clear impact on the processes. LDH particles modified with terephthalate anions decreased the consumption of hydrogen peroxide and increased opacity by 3 units in TMP. Unmodified LDH particles enhanced the selectivity in oxygen delignification of kraft pulp, leading to 10% gain in ISO brightness and reduction of 2 units in Kappa number in comparison with conventional processes. Paper strength properties were unaffected in the presented system. After bleaching with LDH, the amount of anionic groups on pulp surfaces was increased. Also, the retention of OBA onto TMP fibers was improved with modified LDH particles. LDH proved to have great potential for current and prospective applications in pulp and paper manufacture.

  1. Zinc layered hydroxide salts: intercalation and incorporation into low-density polyethylene

    Directory of Open Access Journals (Sweden)

    Silvia Jaerger

    2014-12-01

    Full Text Available In this study, polymer composites using low-density polyethylene (LDPE and layered hydroxide salts (LHS were synthesized. The following compositions of LHS were obtained Zn5(OH8(An-2/n.yH2O, where A was varied in order to obtain hydrophilic (A = NO3- or hydrophobic (A = DDS- - dodecyl sulfate or DBS- - dodecyl benzene sulfonate. Synthesis was carried out by co-precipitation in alkaline medium and drying, being followed by characterization via Fourier-transform infrared spectroscopy, thermogravimetric analysis, X-ray diffraction and scanning electron microscopy. A variable amount of filler was then incorporated into the LDPE via extrusion, which was then injection molded to obtain specimens for evaluating tensile properties (Young's modulus, tensile strength, strain at break and toughness. For comparison, the sodium salts of the surfactants (NaDDS and NaDBS were also used as fillers in LDPE. The X-ray diffraction results indicated that the hydrophobic LHS were exfoliated in the polymer matrix, whereas the hydrophilic LHS was only delaminated. In the LDPE composites, melting and crystallization temperatures were nearly constant, along with the crystallinity indexes. The mechanical properties were mainly varied when the organophilic LHS was used. Overall, fillers based on LHS, especially those containing hydrophobic anions, may be interesting alternatives in the production of reinforced thermoplastics.

  2. Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

    Science.gov (United States)

    Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z.; Kukovecz, Á.; Kónya, Z.; Carlson, S.; Sipos, P.; Pálinkó, I.

    2016-01-01

    A mechanochemical method (grinding the components without added water - dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution - wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic-inorganic nanocomposites: LDHs intercalated with amino acid anions.

  3. Composition and structure of an iron-bearing, layered double hydroxide (LDH) - Green rust sodium sulphate

    DEFF Research Database (Denmark)

    Christiansen, B. C.; Balic-Zunic, T.; Petit, P. O.

    2009-01-01

    Mixed-valent Fe(II),Fe(III)-layered hydroxide, known as green rust, was synthesized from slightly basic, sodium sulphate solutions in an oxygen-free glove box. Solution conditions were monitored with pH and Eh electrodes and optimized to ensure a pure sulphate green-rust phase. The solid...... with Fe(II) and Fe(III) in an ordered distribution. The interlayers contain sulphate, water and sodium in an arrangement characteristic for the nikischerite group. The crystal structure is highly disordered by slacking faults. The composition, formula and crystallographic parameters are: NaFe(II)(6)Fe......(III)(3)(SO4)(2)(OH)(18)center dot 12H(2)O, space group P-3, a = 9.528(6) angstrom, c = 10.968(8) angstrom and Z = 1. Green rust sodium sulphate, GR(Na,SO4) crystallizes in thin, hexagonal plates. Particles range from less than 50 nm to 2 mu m in diameter and are 40 nm thick or less. The material is redox...

  4. Phosphate recovery from wastewater using engineered superparamagnetic particles modified with layered double hydroxide ion exchangers.

    Science.gov (United States)

    Drenkova-Tuhtan, Asya; Mandel, Karl; Paulus, Anja; Meyer, Carsten; Hutter, Frank; Gellermann, Carsten; Sextl, Gerhard; Franzreb, Matthias; Steinmetz, Heidrun

    2013-10-01

    An innovative nanocomposite material is proposed for phosphate recovery from wastewater using magnetic assistance. Superparamagnetic microparticles modified with layered double hydroxide (LDH) ion exchangers of various compositions act as phosphate adsorbers. Magnetic separation and chemical regeneration of the particles allows their reuse, leading to the successful recovery of phosphate. Based upon the preliminary screening of different LDH ion exchanger modifications for phosphate selectivity and uptake capacity, MgFe-Zr LDH coated magnetic particles were chosen for further characterization and application. The adsorption kinetics of phosphate from municipal wastewater was studied in dependence with particle concentration, contact time and pH. Adsorption isotherms were then determined for the selected particle system. Recovery of phosphate and regeneration of the particles was examined via testing a variety of desorption solutions. Reusability of the particles was demonstrated for 15 adsorption/desorption cycles. Adsorption in the range of 75-97% was achieved in each cycle after 1 h contact time. Phosphate recovery and enrichment was possible through repetitive application of the desorption solution. Finally, a pilot scale experiment was carried out by treating 125 L of wastewater with the particles in five subsequent 25 L batches. Solid-liquid separation on this scale was carried out with a high-gradient magnetic filter (HGMF).

  5. Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides

    Directory of Open Access Journals (Sweden)

    Dessislava Kostadinova

    2016-12-01

    Full Text Available Increasing attention has been devoted to the design of layered double hydroxide (LDH-based hybrid materials. In this work, we demonstrate the intercalation by anion exchange process of poly(acrylic acid (PAA and three different hydrophilic random copolymers of acrylic acid (AA and n-butyl acrylate (BA with molar masses ranging from 2000 to 4200 g mol−1 synthesized by reversible addition-fragmentation chain transfer (RAFT polymerization, into LDH containing magnesium(II and aluminium(III intralayer cations and nitrates as counterions (MgAl-NO3 LDH. At basic pH, the copolymer chains (macroRAFT agents carry negative charges which allowed the establishment of electrostatic interactions with the LDH interlayer and their intercalation. The resulting hybrid macroRAFT/LDH materials displayed an expanded interlamellar domain compared to pristine MgAl-NO3 LDH from 1.36 nm to 2.33 nm. Depending on the nature of the units involved into the macroRAFT copolymer (only AA or AA and BA, the intercalation led to monolayer or bilayer arrangements within the interlayer space. The macroRAFT intercalation and the molecular structure of the hybrid phases were further characterized by Fourier transform infrared (FTIR and solid-state 13C, 1H and 27Al nuclear magnetic resonance (NMR spectroscopies to get a better description of the local structure.

  6. Layered Double Hydroxides: Potential Release-on-Demand Fertilizers for Plant Zinc Nutrition.

    Science.gov (United States)

    López-Rayo, Sandra; Imran, Ahmad; Bruun Hansen, Hans Chr; Schjoerring, Jan K; Magid, Jakob

    2017-10-02

    A novel zinc (Zn) fertilizer concept based on Zn-doped layered double hydroxides (Zn-doped Mg-Fe-LDHs) has been investigated. Zn-doped Mg-Fe-LDHs were synthesized, their chemical composition was analyzed, and their nutrient release was studied in buffered solutions with different pH values. Uptake of Zn by barley (Hordeum vulgare cv. Antonia) was evaluated in short- (8 weeks), medium- (11 weeks), and long-term (28 weeks) experiments in quartz sand and in a calcareous soil enriched with Zn-doped Mg-Fe-LDHs. The Zn release rate of the Zn-doped Mg-Fe-LDHs was described by a first-order kinetics equation showing maximum release at pH 5.2, reaching approximately 45% of the total Zn content. The Zn concentrations in the plants receiving the LDHs were between 2- and 9.5-fold higher than those in plants without Zn addition. A positive effect of the LDHs was also found in soil. This work documents the long-term Zn release capacity of LDHs complying with a release-on-demand behavior and serves as proof-of-concept that Zn-doped Mg-Fe-LDHs can be used as Zn fertilizers.

  7. Calcined Mg-Fe layered double hydroxide as an absorber for the removal of methyl orange

    Directory of Open Access Journals (Sweden)

    Chao Peng

    2015-05-01

    Full Text Available In this work, methyl orange (MO was effectively removed from aqueous solution with the calcined product of hydrothermal synthesized Mg/Fe layered double hydroxide (Mg/Fe-LDH. The structure, composition, morphology and textural properties of the Mg/Fe-LDH before and after adsorption were characterized by X-ray diffraction, Fourier transformation infrared spectroscopy, transmission electron microscopy, nitrogen adsorption apparatus and X-ray photoelectron spectroscopy. It was confirmed that MO had been absorbed by calcined Mg/Fe-LDH which had strong interactions with MO. The adsorption of MO onto the Mg/Fe-LDH was systematically investigated by batch tests. The adsorption capacity of the Mg/Fe-LDH toward MO was found to be 194.9 mg • g−1. Adsorption kinetics and isotherm studies revealed that the adsorption of MO onto Mg/Fe-LDH was a spontaneous and endothermic process. These results indicate that Mg/Fe-LDH is a promising material for the removal of MO.

  8. Functionalized layered double hydroxide nanoparticles conjugated with disulfide-linked polycation brushes for advanced gene delivery.

    Science.gov (United States)

    Hu, H; Xiu, K M; Xu, S L; Yang, W T; Xu, F J

    2013-06-19

    Layered double hydroxides (LDHs) have aroused great attention as potential nanosized drug delivery carriers, but independent inorganic LDH wrapped with DNA shows very low transfection efficiency. To manipulate and control the surface properties of LDH nanoparticles is of crucial importance in the designing of LDH-based drug carriers. In this work, surface-initiated atom transfer radical polymerization (ATRP) of 2-(dimethylamino)ethyl methacrylate (DMAEMA) is employed to tailor the functionality of LDH surfaces in a well-controlled manner and produce a series of well-defined novel gene delivery vectors (termed as LDH-PDs), where a flexible three-step method was first developed to introduce the ATRP initiation sites containing disulfide bonds onto LDH surfaces. In comparison the pristine LDH particles, the resultant LDH-PDs exhibited better ability to condense plasmid DNA (pDNA) and much higher levels to delivery genes in different cell lines including COS7 and HepG2 cell lines. Moreover, the LDH-PDs also could largely enhance cellular uptake. This present study demonstrates that functionalization of bioinorganic LDH with flexible polycation brushes is an effective means to produce new LDH-based gene delivery systems.

  9. From spent Mg/Al layered double hydroxide to porous carbon materials.

    Science.gov (United States)

    Laipan, Minwang; Zhu, Runliang; Chen, Qingze; Zhu, Jianxi; Xi, Yunfei; Ayoko, Godwin A; He, Hongping

    2015-12-30

    Adsorption has been considered as an efficient method for the treatment of dye effluents, but proper disposal of the spent adsorbents is still a challenge. This work attempts to provide a facile method to reutilize the spent Mg/Al layered double hydroxide (Mg/Al-LDH) after the adsorption of orange II (OII). Herein, the spent hybrid was carbonized under the protection of nitrogen, and then washed with acid to obtain porous carbon materials. Thermogravimetric analysis results suggested that the carbonization could be well achieved above 600°C, as mass loss of the spent hybrid gradually stabilized. Therefore, the carbonization process was carried out at 600, 800, and 1000°C, respectively. Scanning electron microscope showed that the obtained carbon materials possessed a crooked flaky morphology. Nitrogen adsorption-desorption results showed that the carbon materials had large BET surface area and pore volume, e.g., 1426 m(2)/g and 1.67 cm(3)/g for the sample carbonized at 800°C. Moreover, the pore structure and surface chemistry compositions were tunable, as they were sensitive to the temperature. Toluene adsorption results demonstrated that the carbon materials had high efficiency in toluene removal. This work provided a facile approach for synthesizing porous carbon materials using spent Mg/Al-LDH.

  10. Morphological control of layered double hydroxide through a biomimetic approach using carboxylic and sulfonic acids

    Directory of Open Access Journals (Sweden)

    Taishi Yokoi

    2015-09-01

    Full Text Available Layered double hydroxides (LDHs have intercalation properties and are used in various applications. The performances of the LDH materials can be improved by controlling crystal morphology. Morphology of inorganic crystals is controlled by organic molecules in biomineralization. Inspired by biomineralization, we investigated the effect of the addition of mono, di and triacids as morphological control agents on crystal morphology of LDH synthesized by the homogeneous precipitation method. Morphology of LDH was changed from hexagonal plate to stacked disc by addition of monoacids, namely acetic acid and methanesulfonic acid, in the reaction solution. Flower-shaped LDH crystals were formed in the presence of diacids and a triacid, namely succinic acid, 1,2-ethanedisulfonic acid and 1,2,3-propanetricarboxylic acid. We found that the morphology of the LDH crystals was controlled by the number of functional group on the morphological control agent rather than the type of functional group. These findings can contribute for the development of novel and functional LDH materials with precisely controlled morphology.

  11. Enhanced Anti-Metastatic Activity of Etoposide Using Layered Double Hydroxide Nano Particles.

    Science.gov (United States)

    Zhu, Yanjing; Wu, Youjun; Zhang, Haixia; Wang, Zhaoqi; Wang, Shilong; Qian, Yechang; Zhu, Rongrong

    2015-12-01

    Cell migration and invasion are integral to lung cancer metastasis. In this study, we investigated the combination of traditional chemotherapy and a layered double hydroxide (LDH) carrier as a new strategy for the inhibition of migration and invasion. To investigate the characteristics and possible mechanisms of VP16-LDH [the Mg-Al/LDH containing etoposide (VP16)], we used several experimental techniques, such as transmission electron microscopy (TEM) and fluorescent microscopy. The TEM, X-ray diffraction (XRD) and zeta potential results indicated that VP16 binds well with LDH, with an average size of 70 nm, and the drug delivery system was confirmed to have the desired quality of slow release by the in vitro release test results. Fluorescent images showed that the cellular uptake of VP16-LDH was a caveolae-mediated and energy-dependent process. Moreover, A549 cells treated with VP16-LDH (5 μg/ml, 10 μg/ml) demonstrated significant inhibition of cell migration and invasion compared with the cells treated with free VP16 at the same concentration. The inhibition of AKT, mTOR and STAT3 phosphorylation and p-β-catenin up-regulation in VP16-LDH-treated cells revealed a possible molecular mechanism via the mTOR/AKT and STAT pathways, through which VP16-LDH had a stronger inhibitory effect on migration than the drug alone.

  12. Dependence of bonding interactions in Layered Double Hydroxides on metal cation chemistry

    Science.gov (United States)

    Shamim, Mostofa; Dana, Kausik

    2016-12-01

    The evolution of various Infrared bands of Layered Double Hydroxides (LDH) with variable Zn:Al ratio was analyzed to correlate it with the changes in octahedral metal cation chemistry, interlayer carbonate anion and hydroxyl content of LDH. The synthesized phase-pure LDHs were crystallized as hexagonal 2H polytype with a Manasseite structure. The broad and asymmetric hydroxyl stretching region (2400-4000 cm-1) can be deconvoluted into four different bands. With increase in Zn2+:Al3+ metal ratio, the peak position of stretching frequencies of Al3+sbnd OH and carbonate-bridged hydroxyl (water) decrease almost linearly. Individual band's peak position and area under the curve have been successfully correlated with the carbonate and hydroxyl content of LDH. Due to lowering of symmetry of the carbonate anion, the IR-inactive peak νCsbnd O, symm at 1064 cm-1 becomes IR active. The peak position of metal-oxygen bands and carbonate bending modes are practically unaffected by the Zn2+:Al3+ ratio but the area under the individual M-O bands shows a direct correlation.

  13. Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides

    Science.gov (United States)

    Kostadinova, Dessislava; Cenacchi Pereira, Ana; Lansalot, Muriel; D’Agosto, Franck; Bourgeat-Lami, Elodie; Leroux, Fabrice; Taviot-Guého, Christine; Cadars, Sylvian

    2016-01-01

    Summary Increasing attention has been devoted to the design of layered double hydroxide (LDH)-based hybrid materials. In this work, we demonstrate the intercalation by anion exchange process of poly(acrylic acid) (PAA) and three different hydrophilic random copolymers of acrylic acid (AA) and n-butyl acrylate (BA) with molar masses ranging from 2000 to 4200 g mol−1 synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization, into LDH containing magnesium(II) and aluminium(III) intralayer cations and nitrates as counterions (MgAl-NO3 LDH). At basic pH, the copolymer chains (macroRAFT agents) carry negative charges which allowed the establishment of electrostatic interactions with the LDH interlayer and their intercalation. The resulting hybrid macroRAFT/LDH materials displayed an expanded interlamellar domain compared to pristine MgAl-NO3 LDH from 1.36 nm to 2.33 nm. Depending on the nature of the units involved into the macroRAFT copolymer (only AA or AA and BA), the intercalation led to monolayer or bilayer arrangements within the interlayer space. The macroRAFT intercalation and the molecular structure of the hybrid phases were further characterized by Fourier transform infrared (FTIR) and solid-state 13C, 1H and 27Al nuclear magnetic resonance (NMR) spectroscopies to get a better description of the local structure.

  14. Particle size- and number-dependent delivery to cells by layered double hydroxide nanoparticles.

    Science.gov (United States)

    Dong, Haiyan; Parekh, Harendra S; Xu, Zhi Ping

    2015-01-01

    It is well known that delivery efficiency to cells is highly dependent on particle size and the administered dose. However, there is a marked discrepancy in many reports, mainly due to the inconsistency in assessment of various parameters. In this particular research, we designed experiments using layered double hydroxide nanoparticles (LDH NPs) to specifically elucidate the effect of particle size, dose and dye loading manner on cellular uptake. Using the number of LDH NPs taken up by HCT-116 cells as the indicator of delivery efficiency, we found that (1) the size of sheet-like LDH in the range of 40-100 nm did not significantly affect their cellular uptake; (2) cellular uptake of 40 and 100 nm LDH NPs was increased proportionally to the number concentration below a critical value, but remained relatively constant beyond the critical value; and (3) the effect of the dye loading manner is mainly dependent on the loading capacity or yield. In particular, the loading capacity is determined by the NP specific surface area. This research may be extended to a larger size range to examine the size effect, but suggests that it is necessary to set up a protocol to evaluate the effects of NP's physicochemical properties on the cellular delivery efficiency.

  15. The unmediated choline sensor based on layered double hydroxides in hydrogen peroxide detection mode

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    In this work,we have developed a novel choline biosensor on the basis of immobilization of choline oxidase (ChOx) by the attractive materials layered double hydroxides (LDHs). Amperometric detection of choline was evaluated by holding the modified electrode at 0.5 V (vs. SCE). Due to the special properties of LDHs ([Zn3-Al-Cl]),such as chemical inertness,high porosity,and swelling property,the [Zn3-Al-Cl]/ChOx modified electrode exhibited an enhanced analytical performance. The biosensor provided a linear response to choline over a concentration range from 3.7 × 10-6 to 6.3 × 10-4 M with a low detection limit of 3 × 10-7 M based on S/N=3. The apparent Michaelis-Menten constant was calculated to be 1.38 mM. In addition,the interaction between ChOx and LDHs has also been investigated using FT-IR spectroscopy.

  16. Crosslinking to enhance colloidal stability and redispersity of layered double hydroxide nanoparticles.

    Science.gov (United States)

    Zuo, Huali; Gu, Zi; Cooper, Helen; Xu, Zhi Ping

    2015-12-01

    This article introduces a strategy for stabilizing and redispersing layered double hydroxide (LDH) nanoparticles by crosslinking bovine serum albumin (BSA) coated onto the surface. The strategy involves optimization of the amount of the crosslinking agent glutaraldehyde (GTA) to achieve minimal aggregation and ready redispersion. LDH nanoparticles were prepared by co-precipitation and hydrothermal treatment, with subsequent BSA coating at the BSA/LDH mass ratio of 5:2. BSA coated onto LDH nanoparticles was crosslinked with different amounts of GTA. Aggregation studies using dilution assays, dynamic light scattering, and zeta potential analysis indicated that severe aggregation at lower LDH nanoparticle concentrations can be prevented by proper crosslinking of BSA with GTA. The GTA-crosslinked BSA-coated nanoparticles showed excellent redispersity compared to the non-crosslinked nanoparticles. In vitro cytotoxicity and cell uptake were found to be minimally affected by GTA-crosslinking. The new strategy therefore provides a much more effective method for the prevention of LDH nanoparticle aggregation and improved LDH nanoparticle redispersion for use in a wide variety of bio-applications in vitro and in vivo.

  17. Leaching of iodide (I(-)) and iodate (IO3(-)) anions from synthetic layered double hydroxide materials.

    Science.gov (United States)

    Theiss, Frederick L; Ayoko, Godwin A; Frost, Ray L

    2016-09-15

    Several studies have previously demonstrated that layered double hydroxides (LDHs) show considerable potential for the adsorption of radioiodine from aqueous solution; however, few studies have demonstrated that these materials are able to store radioactive (131)I for an acceptable period. The leaching of iodide (I(-)) and iodate (IO3(-)) form Mg/Al LDHs has been carried out. Contact time appeared to be a more significant variable for the leaching of iodate (IO3(-)) compared to that of iodide (I(-)). Experimental results are fitted to the pseudo second order model, suggesting that diffusion is likely to be the rate-limiting step. The presence of carbonate in the leaching solution appeared to significantly increase the leaching of iodide (I(-)) as did the presence of chloride to a lesser extent. The maximum amount of iodate (IO3(-)) leached using ultrapure water as the leaching solution was 21% of the iodate (IO3(-)) originally present. The corresponding result for iodide (I(-)) was even lower at 3%.

  18. Chelator-Free Labeling of Layered Double Hydroxide Nanoparticles for in Vivo PET Imaging

    Science.gov (United States)

    Shi, Sixiang; Fliss, Brianne C.; Gu, Zi; Zhu, Yian; Hong, Hao; Valdovinos, Hector F.; Hernandez, Reinier; Goel, Shreya; Luo, Haiming; Chen, Feng; Barnhart, Todd E.; Nickles, Robert J.; Xu, Zhi Ping; Cai, Weibo

    2015-11-01

    Layered double hydroxide (LDH) nanomaterial has emerged as a novel delivery agent for biomedical applications due to its unique structure and properties. However, in vivo positron emission tomography (PET) imaging with LDH nanoparticles has not been achieved. The aim of this study is to explore chelator-free labeling of LDH nanoparticles with radioisotopes for in vivo PET imaging. Bivalent cation 64Cu2+ and trivalent cation 44Sc3+ were found to readily label LDH nanoparticles with excellent labeling efficiency and stability, whereas tetravalent cation 89Zr4+ could not label LDH since it does not fit into the LDH crystal structure. PET imaging shows that prominent tumor uptake was achieved in 4T1 breast cancer with 64Cu-LDH-BSA via passive targeting alone (7.7 ± 0.1%ID/g at 16 h post-injection; n = 3). These results support that LDH is a versatile platform that can be labeled with various bivalent and trivalent radiometals without comprising the native properties, highly desirable for PET image-guided drug delivery.

  19. Three-dimensional porous MXene/layered double hydroxide composite for high performance supercapacitors

    Science.gov (United States)

    Wang, Ya; Dou, Hui; Wang, Jie; Ding, Bing; Xu, Yunling; Chang, Zhi; Hao, Xiaodong

    2016-09-01

    In this work, an exfoliated MXene (e-MXene) nanosheets/nickel-aluminum layered double hydroxide (MXene/LDH) composite as supercapacitor electrode material is fabricated by in situ growth of LDH on e-MXene substrate. The LDH platelets homogeneously grown on the surface of the e-MXene sheets construct a three-dimensional (3D) porous structure, which not only leads to high active sites exposure of LDH and facile liquid electrolyte penetration, but also alleviates the volume change of LDH during the charge/discharge process. Meanwhile, the e -MXene substrate forms a conductive network to facilitate the electron transport of active material. The optimized MXene/LDH composite exhibits a high specific capacitance of 1061 F g-1 at a current density of 1 A g-1, excellent capacitance retention of 70% after 4000 cycle tests at a current density of 4 A g-1 and a good rate capability with 556 F g-1 retention at 10 A g-1.

  20. Calcined Mg-Fe layered double hydroxide as an absorber for the removal of methyl orange

    Energy Technology Data Exchange (ETDEWEB)

    Peng, Chao [School of Civil Engineering and Mechanics, Central South University of Forestry and Technology, Changsha 410004, Hunan (China); State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China); Dai, Jing [Key Laboratory of Advanced Technology for Special Functional Materials of Ministry of Education, Wuhan 430070 (China); Yu, Jianying, E-mail: Yujianyingwhut@163.com [State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China); Yin, Jian [School of Civil Engineering and Mechanics, Central South University of Forestry and Technology, Changsha 410004, Hunan (China)

    2015-05-15

    In this work, methyl orange (MO) was effectively removed from aqueous solution with the calcined product of hydrothermal synthesized Mg/Fe layered double hydroxide (Mg/Fe-LDH). The structure, composition, morphology and textural properties of the Mg/Fe-LDH before and after adsorption were characterized by X-ray diffraction, Fourier transformation infrared spectroscopy, transmission electron microscopy, nitrogen adsorption apparatus and X-ray photoelectron spectroscopy. It was confirmed that MO had been absorbed by calcined Mg/Fe-LDH which had strong interactions with MO. The adsorption of MO onto the Mg/Fe-LDH was systematically investigated by batch tests. The adsorption capacity of the Mg/Fe-LDH toward MO was found to be 194.9 mg • g{sup −1}. Adsorption kinetics and isotherm studies revealed that the adsorption of MO onto Mg/Fe-LDH was a spontaneous and endothermic process. These results indicate that Mg/Fe-LDH is a promising material for the removal of MO.

  1. Preparation and antibacterial activity of lysozyme and layered double hydroxide nanocomposites.

    Science.gov (United States)

    Yang, Qin-Zheng; Chang, Ying-Yue; Zhao, Hua-Zhang

    2013-11-01

    It is necessary to develop "green" disinfection technology which does not produce disinfection by-products. Lysozyme-layered double hydroxide nanocomposites (LYZ-LDHs) were prepared by intercalating LYZ in LDH for the first time. Their antibacterial activity was evaluated using staphylococcus aureus as a target. The bacteria removal mechanism was also studied. Characterization of LYZ-LDHs by X-ray diffraction and Fourier transform infrared spectroscopy indicated that LYZ was successfully intercalated in LDH, compressed and deformed without secondary structural change. LYZ-LDHs showed excellent bactericidal effectiveness against staphylococcus aureus. The antibacterial performance of LYZ-LDHs was found to be affected by the LYZ/LDH ratio and the pH of the bacteria-containing water. The bacteria removal efficiency of LYZ-LDHs with LYZ/LDH mass ratio of 0.8 was consistently above 94% over the pH range of 3-9. LYZ-LDHs adsorbed bacteria to their surface by LDH and then killed them by the immobilized LYZ. This new material integrated the bactericidal ability of LYZ and adsorption ability of LDH. Moreover, the antibacterial ability of LYZ-LDHs was persistent and not limited by the adsorption capacity.

  2. Layered double hydroxide functionalized textile for effective oil/water separation and selective oil adsorption.

    Science.gov (United States)

    Liu, Xiaojuan; Ge, Lei; Li, Wei; Wang, Xiuzhong; Li, Feng

    2015-01-14

    The removal of oil and organic pollutants from water is highly desired due to frequent oil spill accidents, as well as the increase of industrial oily wastewater. Here, superhydrophobic and superoleophilic textile has been successfully prepared for the application of effective oil/water separation and selective oil adsorption. This textile was fabricated by functionalizing the commercial textile with layered double hydroxide (LDH) microcrystals and low surface energy molecules. The LDH microcrystals were immobilized on the microfibers of the textile through an in situ growth method, and they formed a nestlike microstructure. The combination of the hierarchical structure and the low surface energy molecules made the textile superhydrophobic and superoleophilic. Further experiments demonstrated that the as-prepared textile not only can be applied as effective membrane materials for the separation of oil and water mixtures with high separation efficiency (>97%), but also can be used as a bag for the selective oil adsorption from water. Thus, such superhydrophobic and superoleophilic textile is a very promising material for the application of oil spill cleanup and industrial oily wastewater treatment.

  3. Starch Biocatalyst Based on α-Amylase-Mg/Al-Layered Double Hydroxide Nanohybrids.

    Science.gov (United States)

    Bruna, Felipe; Pereira, Marita G; Polizeli, Maria de Lourdes T M; Valim, João B

    2015-08-26

    The design of new biocatalysts through the immobilization of enzymes, improving their stability and reuse, plays a major role in the development of sustainable methodologies toward the so-called green chemistry. In this work, α-amylase (AAM) biocatalyst based on Mg3Al-layered double-hydroxide (LDH) matrix was successfully developed with the adsorption method. The adsorption process was studied and optimized as a function of time and enzyme concentration. The biocatalyst was characterized, and the mechanism of interaction between AAM and LDH, as well as the immobilization effects on the catalytic activity, was elucidated. The adsorption process was fast and irreversible, thus yielding a stable biohybrid material. The immobilized AAM partially retained its enzymatic activity, and the biocatalyst rapidly hydrolyzed starch in an aqueous solution with enhanced efficiency at intermediate loading values of ca. 50 mg/g of AAM/LDH. Multiple attachments through electrostatic interactions affected the conformation of the immobilized enzyme on the LDH surface. The biocatalyst was successfully stored in its dry form, retaining 100% of its catalytic activity. The results reveal the potential usefulness of a LDH compound as a support of α-amylase for the hydrolysis of starch that may be applied in industrial and pharmaceutical processes as a simple, environmentally friendly, and low-cost biocatalyst.

  4. Removal of bacteria and viruses from waters using layered double hydroxide nanocomposites

    Directory of Open Access Journals (Sweden)

    Song Jin et al

    2007-01-01

    Full Text Available We have identified synthetic layered double hydroxides (LDH nanocomposites as an effective group of material for removing bacteria and viruses from water. In this study, LDH nanocomposites were synthesized and tested for removing biological contaminants. LDH was used to remove MS2 and X174 (indicator viruses, and Escherichia coli (an indicator bacterium from synthetic groundwater and to remove mixed communities of heterotrophic bacteria from raw river water. Our results indicate that LDH composed of magnesium–aluminium or zinc–aluminium has a viral and bacterial adsorption efficiency ≥99% at viral concentrations between 5.9×106 and 9.1×106 plaque forming units (pfu/L and bacterial concentrations between 1.6×1010 and 2.6×1010 colony forming units (cfu/L when exposed to LDH in a slurry suspension system. Adsorption densities of viruses and bacteria to LDH in suspension ranged from 1.4×1010 to 2.1×1010 pfu/kg LDH and 3.2×1013–5.2×1013 cfu/kg LDH, respectively. We also tested the efficiency of LDH in removing heterotrophic bacteria from raw river water. While removal efficiencies were still high (87–99%, the adsorption capacities of the two kinds of LDH were 4–5 orders of magnitude lower than when exposed to synthetic groundwater, depending on if the LDH was in suspension or a packed column, respectively.

  5. Photocatalytic property and structural stability of CuAl-based layered double hydroxides

    Science.gov (United States)

    Lv, Ming; Liu, Haiqiang

    2015-07-01

    Three types of CuMAl layered double hydroxides (LDHs, M=Mg, Zn, Ni) were successfully synthesized by coprecipitation. Powder X-ray diffraction (XRD), inductively coupled plasma atomic emission spectrometry (ICP-AES) and UV-Vis diffuse reflectance spectrum (UV-vis) were used to confirm the formation of as-synthesized solids with good crystal structure. The photocatalytic activity of those LDH materials for CO2 reduction under visible light was investigated. The experimental results show that CuNiAl-LDHs with narrowest band gap and largest surface areas behave highest efficiency for methanol generation under visible light compared with CuMgAl-LDHs and CuZnAl-LDHs. The CuNiAL-LDH showed high yield for methanol production i.e. 0.210 mmol/g h, which was high efficient. In addition, the influence of the different M2+ on the structures and stability of the CuMAl-LDHs was also investigated by analyzing the geometric parameters, electronic arrangement, charge populations, hydrogen-bonding, and binding energies by density functional theory (DFT) analysis. The theoretical calculation results show that the chemical stability of LDH materials followed the order of CuMgAl-LDHs>CuZnAl-LDHs>CuNiAl-LDHs, which is just opposite with the photocatalytic activity and band gaps of three materials.

  6. Organo-layered double hydroxides composite thin films deposited by laser techniques

    Science.gov (United States)

    Birjega, R.; Vlad, A.; Matei, A.; Dumitru, M.; Stokker-Cheregi, F.; Dinescu, M.; Zavoianu, R.; Raditoiu, V.; Corobea, M. C.

    2016-06-01

    We used laser techniques to create hydrophobic thin films of layered double hydroxides (LDHs) and organo-modified LDHs. A LDH based on Zn-Al with Zn2+/Al3+ ratio of 2.5 was used as host material, while dodecyl sulfate (DS), which is an organic surfactant, acted as guest material. Pulsed laser deposition (PLD) and matrix assisted pulsed laser evaporation (MAPLE) were employed for the growth of the films. The organic anions were intercalated in co-precipitation step. The powders were subsequently used either as materials for MAPLE, or they were pressed and used as targets for PLD. The surface topography of the thin films was investigated by atomic force microscopy (AFM), the crystallographic structure of the powders and films was checked by X-ray diffraction. FTIR spectroscopy was used to evidence DS interlayer intercalation, both for powders and the derived films. Contact angle measurements were performed in order to establish the wettability properties of the as-prepared thin films, in view of functionalization applications as hydrophobic surfaces, owing to the effect of DS intercalation.

  7. Synthesis and reversible hydration behavior of the thiosulfate intercalated layered double hydroxide of Zn and Al

    Energy Technology Data Exchange (ETDEWEB)

    Radha, S. [Department of Chemistry, Central College, Bangalore University, Bangalore-560 001 (India); Milius, Wolfgang [Department of Inorganic Chemistry I, University of Bayreuth, Bayreuth (Germany); Breu, Josef, E-mail: josef.breu@uni-bayreuth.de [Department of Inorganic Chemistry I, University of Bayreuth, Bayreuth (Germany); Kamath, P. Vishnu, E-mail: vishnukamath8@hotmail.com [Department of Chemistry, Central College, Bangalore University, Bangalore-560 001 (India)

    2013-08-15

    The thiosulfate-intercalated layered double hydroxide of Zn and Al undergoes reversible hydration with a variation in the relative humidity of the ambient. The hydrated and dehydrated phases, which represent the end members of the hydration cycle, both adopt the structure of the 3R{sub 1} polytype. In the intermediate range of relative humidity values (40–60%), the hydrated and dehydrated phases coexist. The end members of the hydration cycle adopt the structure of the same polytype, and vary only in their basal spacings. This points to the possibility that all the intermediate phases have a kinetic origin. - Graphical abstract: Basal spacing evolution of the thiosulfate ion intercalated [Zn–Al] LDH during one complete hydration–dehydration cycle as a function of relative humidity. Display Omitted - Highlights: • Thiosulfate intercalated [Zn–Al] LDHs were synthesized by co-precipitation. • The LDH exhibits reversible hydration with variation in humidity. • Both the end members of the hydration cycle adopt the same polytype structure. • The interstratified intermediates observed are kinetic in origin.

  8. Synthesis and characterization of organic intercalated layered double hydroxides and their application in bitumen modification

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Song [State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China); Yu, Jianying, E-mail: jyyu@whut.edu.cn [State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China); Sun, Yubin [Center for Materials Research and Analysis, Wuhan University of Technology, Wuhan 430070 (China); Wu, Shaopeng [State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070 (China)

    2015-02-15

    Organic layered double hydroxides (LDHs) intercalated by sodium dodecylbenzenesulfonate (SDBS) were prepared by anion-exchange method and applied to modify bitumen aiming at improving ageing resistance of bitumen. The organic LDHs (SDBS–LDHs) were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and Ultraviolet and visible (UV–vis) spectrophotometry. The effect of SDBS–LDHs and LDHs on physical and anti-ageing properties of bitumen was evaluated by means of conventional and rheological test. The results of XRD, FTIR and SEM show that SDBS is successfully intercalated into interlayer of LDHs, and the UV–vis reflectance and absorbance curves illustrate that intercalation of SDBS enhances the UV shielding effect of LDHs. The addition of SDBS–LDHs or LDHs has little influence on physical properties of bitumen because SDBS–LDHs and LDHs are physically mixed in bitumen. Compared with pristine bitumen after TFOT and UV irradiation ageing, the introduction of SDBS–LDHs and LDHs significantly improves thermal- and photo-oxidative ageing resistance of bitumen. Notably, bitumen with SDBS–LDHs exhibits better anti-ageing performance than that with LDHs, implying more effective modification of SDBS-LDHs which is due to the enhanced UV protective ability and compatibility with bitumen of SDBS–LDHs. - Highlights: • XRD, FTIR and SEM were used to confirm the successful intercalation. • SDBS–LDHs show superior UV protective ability. • SDBS–LDHs improved the anti-ageing properties of bitumen.

  9. New sulfur adsorbents derived from layered double hydroxides. Part 1. Synthesis and COS adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, Dennis E.; Morgan, Tonya; Patterson, Patricia M.; Tackett, S. Adam; Morris, Erin; Crocker, Mark [Center for Applied Energy Research, University of Kentucky, 2540 Research Park Drive, Lexington, KY 40511-8479 (United States)

    2008-08-08

    Mixed oxides, prepared via the thermal decomposition of layered double hydroxides (LDHs), were screened gravimetrically for their ability to adsorb carbonyl sulfide (COS). Based on promising results obtained for Ni/Mg/Al, Ni/Mg/Fe and Co/Mg/Al mixed oxides, a study was undertaken to optimize the composition of these materials for COS adsorption. To investigate the effect of the M(II):M(III) ratio, LDHs of the type [M{sub z}Mg{sub y}Al{sub x}(OH){sub 2}](CO{sub 3}){sub x/2}.0.5H{sub 2}O (where M = Ni or Co, and x + y + z 1) were prepared at values of x corresponding to 0.33 and 0.20. Simultaneously, the elemental ratio of transition metal to magnesium (z/y) was varied. Mixed oxides obtained from the resulting LDHs were tested in fixed bed mode with a feed of 100 ppm COS in N{sub 2} to determine breakthrough capacity. In general Ni/Mg/Al mixed oxides showed the best performance, a composition with Ni/Mg/Al = 0.32/0.48/0.20 showing the best adsorption capacity. Treatment of the spent adsorbent under an atmosphere of 5% H{sub 2} in N{sub 2} at 450 C was found to provide an effective means of restoring the adsorption capacity over two cycles of adsorption and regeneration, although after three such cycles, adsorption capacity decreased. (author)

  10. Efficient removal of nitrobenzene by Fenton-like process with Co-Fe layered double hydroxide

    Science.gov (United States)

    Bai, Jianfei; Liu, Yong; Yin, Xiaohong; Duan, Hongtao; Ma, Junhua

    2017-09-01

    Co-Fe layered double hydroxide (Co-Fe LDH) prepared by the co-precipitation method was proposed as the Fenton-like catalyst for nitrobenzene removal. The properties of prepared catalysts were characterized by BET, SEM and XRD analyses. The initial pH, hydrogen peroxide concentration, catalyst dosage and the nitrobenzene concentration on the removal of nitrobenzene have been studied. The best removal efficiency (100%) was obtained at pH = 2.7, [H2O2]0 = 500 mg/L, catalyst dosage = 1 g/L for the initial concentration of 50 mg/L nitrobenzene. Co-Fe LDH retained the catalytic activity after five cycles. The mechanism of nitrobenzene oxidation was radical mediated process, confirmed by the addition of T-butanol (·OH scavenger). The iron leaching was only 12.47 mg/L even at pH 2.7. Moreover, the intermediates were detected by LC/MS and a possible pathway for nitrobenzene removal in the Co-Fe LDH and H2O2 system was proposed.

  11. Polymer coated CaAl-layered double hydroxide nanomaterials for potential calcium supplement.

    Science.gov (United States)

    Kim, Tae-Hyun; Lee, Jeong-A; Choi, Soo-Jin; Oh, Jae-Min

    2014-12-05

    We have successfully prepared layered double hydroxide (LDH) nanomaterials containing calcium and aluminum ions in the framework (CaAl-LDH). The surface of CaAl-LDH was coated with enteric polymer, Eudragit®L 100 in order to protect nanomaterials from fast dissolution under gastric condition of pH 1.2. The X-ray diffraction patterns, Fourier transform infrared spectroscopy, scanning electron and transmission electron microscopy revealed that the pristine LDH was well prepared having hydrocalumite structure, and that the polymer effectively coated the surface of LDH without disturbing structure. From thermal analysis, it was determined that only a small amount (less than 1%) of polymer was coated on the LDH surface. Metal dissolution from LDH nanomaterials was significantly reduced upon Eudragit®L 100 coating at pH 1.2, 6.8 and 7.4, which simulates gastric, enteric and plasma conditions, respectively, and the dissolution effect was the most suppressed at pH 1.2. The LDH nanomaterials did not exhibit any significant cytotoxicity up to 1000 μg/mL and intracellular calcium concentration significantly increased in LDH-treated human intestinal cells. Pharmacokinetic study demonstrated absorption efficiency of Eudragit®L 100 coated LDH following oral administration to rats. Moreover, the LDH nanomaterials did not cause acute toxic effect in vivo. All the results suggest the great potential of CaAl-LDH nanomaterials as a calcium supplement.

  12. Structure and thermal evolution of Mg-Al layered double hydroxide containing interlayer organic glyphosate anions

    Energy Technology Data Exchange (ETDEWEB)

    Li Feng; Zhang Lihong; Evans, David G.; Forano, Claude; Duan Xue

    2004-12-15

    Layered double hydroxide (LDH) with the Mg{sup 2+}/Al{sup 3+} molar ratio of 2.0 containing interlayer organic pesticide glyphosate anions (MgAl-Gly-LDH) has been synthesized by the use of anion exchange and coprecipitation routes. Intercalation experiments with glyphosate (Gly) reveal a correlation between the temperatures for thermal treatments and the types of reaction it undergoes with Gly. The grafting of the Gly anion onto hydroxylated sheets of LDH by moderate thermal treatments (hydrothermal treatments and calcinations) was confirmed by a combination of several techniques, including powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry analysis (TGA-DTG), and {sup 31}P nuclear magnetic resonance (NMR). The thermal decomposition of MgAl-Gly-LDH results in the removal of loosely held interlayer water, grafting reaction between the interlayer anions and hydroxyl groups on the lattice of LDH, dehydroxylation of the lattice and decomposition of the interlayer species in succession, thus leading to a variety of crystallographic transitions.

  13. From layered double hydroxide to spinel nanostructures: facile synthesis and characterization of nanoplatelets and nanorods.

    Science.gov (United States)

    Sun, Genban; Sun, Lingna; Wen, He; Jia, Zhiqian; Huang, Kunlin; Hu, Changwen

    2006-07-13

    Mg-Al spinel (MgAl2O4) nanorods and nanoplatelets transformed from Mg-Al layered double hydroxide (Mg-Al-LDHs) were synthesized via a combined hydrothermal method and calcination route using Al(NO3).9H2O and Mg(NO3)2.6H2O as raw materials. The nanorods and nanoplatelets were characterized by means of physical techniques, including powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microcopy (HRTEM), selected-area electron diffraction (SAED), Fourier transform infrared spectra (FT-IR), thermogravimetric (TG), and nitrogen adsorption-desorption isotherms. XRD patterns reveal that the Mg-Al-LDHs nanostructures were obtained under a hydrothermal reaction temperature of 200 degrees C and Mg-Al spinel nanostructures were fabricated via calcination of the Mg-Al-LDHs nanostructures at 750 degrees C. It can be seen from TEM that the sizes of the Mg-Al-LDHs nanoplatelets were about 20-40 nm and the diameters of the MgAl2O4 nanorods were ca. 6 nm. The HRTEM images indicate that the crystal lattice spaces of the MgAl2O4 nanorods and nanoplatelets are 0.282 and 0.287 nm, respectively.

  14. Chelator-Free Labeling of Layered Double Hydroxide Nanoparticles for in Vivo PET Imaging.

    Science.gov (United States)

    Shi, Sixiang; Fliss, Brianne C; Gu, Zi; Zhu, Yian; Hong, Hao; Valdovinos, Hector F; Hernandez, Reinier; Goel, Shreya; Luo, Haiming; Chen, Feng; Barnhart, Todd E; Nickles, Robert J; Xu, Zhi Ping; Cai, Weibo

    2015-11-20

    Layered double hydroxide (LDH) nanomaterial has emerged as a novel delivery agent for biomedical applications due to its unique structure and properties. However, in vivo positron emission tomography (PET) imaging with LDH nanoparticles has not been achieved. The aim of this study is to explore chelator-free labeling of LDH nanoparticles with radioisotopes for in vivo PET imaging. Bivalent cation (64)Cu(2+) and trivalent cation (44)Sc(3+) were found to readily label LDH nanoparticles with excellent labeling efficiency and stability, whereas tetravalent cation (89)Zr(4+) could not label LDH since it does not fit into the LDH crystal structure. PET imaging shows that prominent tumor uptake was achieved in 4T1 breast cancer with (64)Cu-LDH-BSA via passive targeting alone (7.7 ± 0.1%ID/g at 16 h post-injection; n = 3). These results support that LDH is a versatile platform that can be labeled with various bivalent and trivalent radiometals without comprising the native properties, highly desirable for PET image-guided drug delivery.

  15. Novel biohybrids of layered double hydroxide and lactate dehydrogenase enzyme: Synthesis, characterization and catalytic activity studies

    Science.gov (United States)

    Djebbi, Mohamed Amine; Braiek, Mohamed; Hidouri, Slah; Namour, Philippe; Jaffrezic-Renault, Nicole; Ben Haj Amara, Abdesslem

    2016-02-01

    The present work introduces new biohybrid materials involving layered double hydroxides (LDH) and biomolecule such as enzyme to produce bioinorganic system. Lactate dehydrogenase (Lac Deh) has been chosen as a model enzyme, being immobilized onto MgAl and ZnAl LDH materials via direct ion-exchange (adsorption) and co-precipitation methods. The immobilization efficiency was largely dependent upon the immobilization methods. A comparative study shows that the co-precipitation method favors the immobilization of great and tunable amount of enzyme. The structural behavior, chemical bonding composition and morphology of the resulting biohybrids were determined by X-ray diffraction (XRD) study, Fourier transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM), respectively. The free and immobilized enzyme activity and kinetic parameters were also reported using UV-Visible spectroscopy. However, the modified LDH materials showed a decrease in crystallinity as compared to the unmodified LDH. The change in activity of the immobilized lactate dehydrogenase was considered to be due, to the reduced accessibility of substrate molecules to the active sites of the enzyme and the partial conformational change of the Lac Deh molecules as a result of the immobilization way. Finally, it was proven that there is a correlation between structure/microstructure and enzyme activity dependent on the immobilization process.

  16. A pH-responsive layered double hydroxide (LDH)-phthalocyanine nanohybrid for efficient photodynamic therapy.

    Science.gov (United States)

    Li, Xing-Shu; Ke, Mei-Rong; Huang, Wei; Ye, Chun-Hong; Huang, Jian-Dong

    2015-02-16

    A pH-responsive nanohybrid (LDH-ZnPcPS4 ), in which a highly hydrophilic zinc(II) phthalocyanine tetra-α-substituted with 4-sulfonatophenoxy groups (ZnPcPS4 ) is incorporated with a cationic layered double hydroxide (LDH) based on electrostatic interaction, has been specially designed and prepared through a facile co-precipitation approach. ZnPcPS4 is an excellent singlet-oxygen generator with strong absorption at the near-infrared region (692 nm) in cellular culture media, whereas the photoactivities of ZnPcPS4 were remarkably inhibited after incorporation with the LDH. The nanohybrid is essentially stable in aqueous media at pH 7.4; nevertheless, in slightly acidic media of pH 6.5 or 5.0, ZnPcPS4 can be efficiently released from the LDH matrix, thus leading to restoration of the photoactivities. The nanohybrid shows a high photocytotoxicity against HepG2 cells as a result of much more efficient cellular uptake and preferential accumulation in lysosomes, whereby the acidic environment leads to the release of ZnPcPS4 . The IC50 value of LDH-ZnPcPS4 is as low as 0.053 μM, which is 24-fold lower than that of ZnPcPS4 . This work provides a facile approach for the fabrication of photosensitizers with high photocytotoxicity, potential tumor selectivity, and rapid clearance character.

  17. Self-Assembly of Single-Layer CoAl-Layered Double Hydroxide Nanosheets on 3D Graphene Network Used as Highly Efficient Electrocatalyst for Oxygen Evolution Reaction.

    Science.gov (United States)

    Ping, Jianfeng; Wang, Yixian; Lu, Qipeng; Chen, Bo; Chen, Junze; Huang, Ying; Ma, Qinglang; Tan, Chaoliang; Yang, Jian; Cao, Xiehong; Wang, Zhijuan; Wu, Jian; Ying, Yibin; Zhang, Hua

    2016-09-01

    A non-noble metal based 3D porous electrocatalyst is prepared by self-assembly of the liquid-exfoliated single-layer CoAl-layered double hydroxide nanosheets (CoAl-NSs) onto 3D graphene network, which exhibits higher catalytic activity and better stability for electrochemical oxygen evolution reaction compared to the commercial IrO2 nanoparticle-based 3D porous electrocatalyst.

  18. Methotrexatum intercalated layered double hydroxides: Statistical design, mechanism explore and bioassay study

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiao-Feng [Department of Gastroenterology, Weihai municipal hospital, Weihai 264200 (China); Liu, Su-Qing [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China); Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China)

    2015-04-01

    A series of methotrexatum intercalated layered double hydroxide (MTX/LDH for short) hybrids have been synthesized by a mechanochemical–hydrothermal method, the statistical experiments are planned and conducted to find out the critical factor influencing the physicochemical properties. Four variables, i.e., addition of NaOH solution, grinding duration, hydrothermal temperature and time, are chosen to play as the examined factors in the orthogonal design. Furthermore, three respective levels, i.e., high, medium and low levels, are conducted in the design. The resulting hybrids are then characterized by X-ray diffraction (XRD) patterns, transmission electron microscope (TEM) graphs and Zeta potentials. XRD diffractions indicate that MTX anions have been successfully intercalated into LDH interlayers and the amount of NaOH solution can change the gallery height greatly. The information from TEM graphs and Zeta potentials state that the increase of alkali solution gives rise to regular morphology and the increase of Zeta potentials. As a result of the statistical analysis, addition of alkali solution is the major factor affecting the morphology and drug-loading capacity. At last, the mechanism of particle growth is explored emphatically, and the anticancer efficacy of some MTX/LDH hybrids is estimated by MTT assay on A549 cells as well. - Graphical abstract: Schematic illustration of synthesis and properties of MTX intercalated LDH hybrids. - Highlights: • Increasing NaOH solution gives rise to high drug-loading capacity. • Increasing the alkali solution leads to high layer charge and regular morphology. • The monodispersity has critical effect on the tumor suppression efficiency.

  19. Layered double hydroxide catalyst for the conversion of crude vegetable oils to a sustainable biofuel

    Science.gov (United States)

    Mollaeian, Keyvan

    Over the last two decades, the U.S. has developed the production of biodiesel, a mixture of fatty acid methyl esters, using chiefly vegetable oils as feedstocks. However, there is much concern about the availability of high-quality vegetable oils for longterm biodiesel production. Problems have also risen due to the production of glycerol, an unwanted byproduct, as well as the need for process wash water. Therefore, this study was initiated to produce not only fatty acid methyl esters (FAMEs) but also fatty acid glycerol carbonates (FAGCs) by replacing methanol with dimethyl carbonate (DMC). The process would have no unnecessary byproducts and would be a simplified process compared to traditional biodiesel. In addition, this altering of the methylating agent could convert triglycerides, free fatty acids, and phospholipids to a sustainable biofuel. In this project, Mg-Al Layered Double Hydroxide (LDH) was optimized by calcination in different temperature varied from 250°C to 450°C. The gallery between layers was increased by intercalating sodium dodecylsulfate (SDS). During catalyst preparation, the pH was controlled ~10. In our experiment, triazabicyclodecene (TBD) was attached with trimethoxysilane (3GPS) as a coupling agent, and N-cetyl-N,N,N-trimethylammonium bromide (CTAB) was added to remove SDS from the catalyst. The catalyst was characterized by XRD, FTIR, and Raman spectroscopy. The effect of the heterogeneous catalyst on the conversion of canola oil, corn oil, and free fatty acids was investigated. To analyze the conversion of lipid oils to biofuel an in situ Raman spectroscopic method was developed. Catalyst synthesis methods and a proposed mechanism for converting triglycerides and free fatty acids to biofuel will be presented.

  20. Synthesis of protocatechuic acid–zinc/aluminium–layered double hydroxide nanocomposite as an anticancer nanodelivery system

    Energy Technology Data Exchange (ETDEWEB)

    Barahuie, Farahnaz [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Hussein, Mohd Zobir, E-mail: mzobir@upm.edu.my [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Gani, Shafinaz Abd [Department of Biochemistry, Faculty of Biotechnology and Biomolecular Sciences, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Fakurazi, Sharida [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Department of Human Anatomy, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Zainal, Zulkarnain [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia)

    2015-01-15

    Protocatechuic acid, an active anticancer agent, has been intercalated into Zn/Al–layered double hydroxide at Zn/Al=2) using two different preparation methods, co-precipitation and ion-exchange, which are labelled as PZAE and PZAC, respectively. The release of protocatechuate from the nanocomposites occurred in a controlled manner and was fitted satisfactorily to pseudo-second order kinetics. The basal spacing of the resulting nanocomposites PZAE and PZAC was 10.2 and 11.0 Å, respectively, indicating successful intercalation of protocatechuate anions into the interlayer galleries of Zn/Al–NO{sub 3}–LDH in a monolayer arrangement with angles of 24 and 33° from the z-axis in PZAE and PZAC, respectively. The formation of nanocomposites was further confirmed by a Fourier transform infrared study. Thermogravimetric and differential thermogravimetric analyses indicated that the thermal stability of the intercalated protocatechuic acid was significantly enhanced compared to its free protocatechuic acid, and the drug content in the nanocomposites was estimated to be approximately 32.6% in PZAE and 29.2% in PZAC. Both PZAE and PZAC nanocomposites inhibit the growth of human cervical, liver and colorectal cancer cell lines and exhibit no toxic effects towards normal fibroblast 3T3 cell after 72 h of treatment. - Graphical abstract: Protocatechuate anions were arranged in monolayer mode with the angle of 24° for PZAE and 33° for PZAC from Z axis to maximize interaction between carboxylate groups and brucite-like layers. - Highlights: • Two methods gave nanocomposites with slightly different physico-chemical properties. • PZAE and PZAC have the potential to be used as a controlled release formulation. • The thermal stability of PA is markedly enhanced upon the intercalation process. • Higher cancer cell growth inhibition for PZAE and PZAC nanocomposites than for PA.

  1. Use of layered double hydroxides and their derivatives as adsorbents for inorganic and organic pollutants

    Science.gov (United States)

    You, Youwen

    Contamination of surface and groundwaters by hazardous inorganic and organic pollutants has become an increasing threat to the safety of drinking waters. Cleanup of contaminated surface and groundwaters has, therefore, become a major focus of environmental research. Primary objectives of this dissertation study were to examine the adsorption properties of layered double hydroxides (LDHs) and their derivatives for inorganic and organic contaminants and to identify potential technologies that utilize LDHs and their derivatives for environment remediation. Studies examined the adsorption characteristics of anionic selenium, arsenic and dicamba (3,6 dichloro-2-methoxy benzoic acid) on original LDHs and calcined-LDHs. Adsorption of selenium and arsenic on LDHs was a function of pH. Competing anions in solution strongly affected adsorption of all three contaminants, with divalent anions decreasing adsorption more intensely than monovalent anions. Adsorbed selenium, arsenic and dicamba could be released from LDHs in anion solutions. Adsorption isotherms for selenium and arsenic retention could be fitted to a simple Langmuir equation. Calcination processes significantly increased adsorption capacities of LDHs. Because of adsorption-desorpion characteristics, LDHs could be recycled. X-ray diffraction patterns revealed an increase of d-spacing coupling with adsorption of contaminants, verifying the intercalation of contaminants into layer structure of LDHs. Long chain anionic surfactants intercalated into LDHs modified their surface properties, resulting in organo-LDHs with hydrophobic surface properties. Various organo-LDHs were developed by incorporating different surfactants into LDHs via different synthesis methods. Surfactant intercalation properties were examined and the geometrical arrangements of the intercalated surfactants were characterized. Results revealed that surfactant molecules could adopt various configurations within the LDH interlayer space. Intercalation

  2. Efficient defluoridation of water using reusable nanocrystalline layered double hydroxides impregnated polystyrene anion exchanger.

    Science.gov (United States)

    Cai, Jianguo; Zhang, Yanyang; Pan, Bingcai; Zhang, Weiming; Lv, Lu; Zhang, Quanxing

    2016-10-01

    Water decontamination from fluoride is still a challenging task of global concern. Recently, Al-based layered double hydroxides (LDHs) have been extensively studied for specific fluoride adsorption from water. Unfortunately, they cannot be readily applied in scaled-up application due to their ultrafine particles as well as the regeneration issues caused by their poor stability at alkaline pHs. Here, we developed a novel (LDH)-based hybrid adsorbent, i.e., LALDH-201, by impregnating nanocrystalline Li/Al LDHs (LADLH) inside a commercial polystyrene anion exchanger D201. TEM image and XRD spectra of the resultant nanocomposite confirmed that the LDHs particles were nanosized inside the pores of D201 of highly crystalline nature and well-ordered layer structure. After impregnation, the chemical and mechanical stability of LALDH were significantly improved against pH variation, facilitating its application at a wide pH range (3.5-12). Fluoride adsorption onto LALDH-201 was compared to D201 and activated alumina, evidencing the preferable removal fluoride of LALDH-201. Fluoride adsorption onto LALDH-201 followed pseudo-second-order model, with the maximum capacity (62.5 mg/g from the Sips model) much higher than the other two adsorbents. Fixed-bed adsorption run indicated the qualified treatable volume of the fluoride contaminated groundwater (4.1 mg/L initially) with LALDH-201 was about 11 times as much as with the anion exchanger D201 when the breakthrough point was set as 1.5 mg/L. The capacity of LALDH-201 could be effectively refreshed for continuous column operation without observable loss by using the mixed solution of 0.01 M NaOH + 1 M NaCl. The above results suggested that the hybrid adsorbent LALDH-201 is very promising for water defluoridation in scaled-up application.

  3. [Role of layered double hydroxide (LDH) in the protection of herring testis DNA from heavy metals].

    Science.gov (United States)

    Tang, Yi-Ni; Wu, Ping-Xiao; Zhu, Neng-Wu

    2012-10-01

    The role of layered double hydroxide (LDH) in the protection of herring testis DNA from heavy metals Cd2+ and Pb2+ was studied by X-ray diffraction ( XRD) spectra, Fourier transform infrared (FTIR) spectra, Scanning Electron Microscopy (SEM), Cyclic Voltammetry and Ultraviolet Spectrometry. Size expansion of the basal spacing (003) from 0. 76 nm in LDH to 2. 30 nm was observed in the resulting DNA-LDH nanohybrids and it gave peaks corresponding to C=O (1 534 cm(-1) and 1488 cm(-1)) in skeleton and bases, C-O stretching vibration (1228 cm(-1)), and P-O symmetrical stretching vibration (1096 cm(-1)) in functional groups of DNA, indicating that DNA were intercalated into the LDH by the ion exchange. However, the displacement of NO3(-) was not fully complete (partial intercalation of DNA). The DNA outside LDH interlayers was absorbed on the surface of LDH. The cyclic voltammetric curves showed that DNA in the composites exhibited a very similar peaks, which corresponded to the two reduction current peaks (E(P) = - 1.2 mV and E(P) = -2.4 mV) of free DNA. Also there was no cathode sag emerging in cyclic voltammetric curves, suggesting that both Cd2+ and Pb2+ cannot insert into the groove of DNA to associate with base pairs or other groups when DNA was bound on LDH. The results showed that, on the one hand, both Cd2+ and Pb2+ were absorbed on the external surface of LDH for immobilization, on the other hand, the layer of LDH provided ideal space for DNA by the action of protecting DNA molecules from Cd2+ and Pb2+.

  4. Control of crystallite and particle size in the synthesis of layered double hydroxides: Macromolecular insights and a complementary modeling tool.

    Science.gov (United States)

    Galvão, Tiago L P; Neves, Cristina S; Caetano, Ana P F; Maia, Frederico; Mata, Diogo; Malheiro, Eliana; Ferreira, Maria J; Bastos, Alexandre C; Salak, Andrei N; Gomes, José R B; Tedim, João; Ferreira, Mário G S

    2016-04-15

    Zinc-aluminum layered double hydroxides with nitrate intercalated (Zn(n)Al-NO3, n=Zn/Al) is an intermediate material for the intercalation of different functional molecules used in a wide range of industrial applications. The synthesis of Zn(2)Al-NO3 was investigated considering the time and temperature of hydrothermal treatment. By examining the crystallite size in two different directions, hydrodynamic particle size, morphology, crystal structure and chemical species in solution, it was possible to understand the crystallization and dissolution processes involved in the mechanisms of crystallite and particle growth. In addition, hydrogeochemical modeling rendered insights on the speciation of different metal cations in solution. Therefore, this tool can be a promising solution to model and optimize the synthesis of layered double hydroxide-based materials for industrial applications.

  5. Molecular modeling of the structure and dynamics of the interlayer species of ZnAlCl layered double hydroxide.

    Science.gov (United States)

    Pisson, J; Morel, J P; Morel-Desrosiers, N; Taviot-Guého, C; Malfreyt, P

    2008-07-03

    Molecular dynamics simulations of the ZnAl layered double hydroxide containing interlayer chloride anions have been performed in the NpT and Np(zz)T statistical ensembles for metal Zn/Al ratios of 2 and 3. We have monitored the interlayer spacing as a function of the number of intercalated water molecules for each statistical ensemble. We have studied how these profiles are affected by the method of calculation of the charges of the hydroxide layer atoms. Diffusion coefficients of the interlayer water molecules have been calculated for different Zn/Al ratios. The calculation of the chemical potential of the interlayer water molecules has been carried out for three amounts of interlayer water molecules. The calculation showed a qualitative agreement with the bulk water chemical potential within a range of interlayer water molecule contents.

  6. Evolution of rheological properties of the nanofluids composed of laponite particles and Mg–Fe layered double hydroxide nanosheets

    Energy Technology Data Exchange (ETDEWEB)

    Hur, Tae-Bong [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Univ. of Pittsburgh, PA (United States); Phuoc, Tran X. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Chyu, Minking K. [Univ. of Pittsburgh, PA (United States); Romanov, Vyacheslav [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)

    2011-05-01

    The thixotropic clay suspensions composed of laponite particles and Mg-Fe layered double hydroxide nanosheets were examined. By adding a very small amount of the layered double hydroxide nanosheets overall theological properties of the host laponite suspension have been changed. Though the particle concentration of the mixture suspension is only about 1 wt%, the mixture quickly becomes a gel in a day by the electrostatic attraction between nano-materials. When a constant shear rate is applied to the mixture gel suspension, at short time, stress increases linearly with elastic deformation of the mixture. Beyond the maximum of stress, while the solid-like gel structure is being broken down with time of shearing, the stress increases again by reflecting shear enhanced association of solid phase. This is likely that the mixture suspension shows partially the behavior of memory effect.

  7. Magnetic cellulose ionomer/layered double hydroxide: An efficient anion exchange platform with enhanced diclofenac adsorption property.

    Science.gov (United States)

    Hossein Beyki, Mostafa; Mohammadirad, Mosleh; Shemirani, Farzaneh; Saboury, Ali Akbar

    2017-02-10

    Polymeric ionomers with anion exchange capability are considered to be classes of environmentally friendly compounds as combination of them with anionic layered hydroxides constitute emerging advance materials. Biosorption by polymeric ionomer - layered double hydroxide (LDH) hybrid material exhibits an attractive green, low cost and low toxic - clean way. As a result, a novel anion exchange platform has been developed by the reaction of CaAl - LDH with Fe(2+), cellulose solution, epichlorohydrin and pyridine. Magnetite cellulose - LDH (MCL) and the ionomer were used for efficient biosorption of diclofenac sodium (DF). Results showed that ionomer has more efficiency for DF adsorption relative to MCL. Magnetite ionomer showed fast equilibrium time (2min) with maximum uptake of 268mgg(-1). Isotherm and Kinetic models were also studied. Regeneration of the sorbent was performed with a mixture of methanol -NaOH (2.0molL(-1)) solution.

  8. Studies of the Catalytic Activity and Deactivation of Calcined Layered Double Hydroxides in the Reaction of Ethanol with Propylene Oxide

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The reaction of ethanol with propylene oxide over calcined layered double hydroxides(CLDH) was investigated. The results show that CLDH has a good activity and a good selectivity, but the activity and the selectivity of CLDH decrease when CLDH reforms LDH- the so called "memory effect". The influence of the "memory effect" on the CLDH returning to LDH was studied by the hydration reaction. It is shown that the "memory effect" is not complete, and the decreases of the Mg/Al molar ratio of LDH and the crystallite size due to the increase of the hydration reaction time result in the drop of the activity and the selectivity.Keyworcds Ethanol, Propylene oxide, Calcined layered double hydroxide, "Memory effect", Hydration

  9. Visions of Reconstruction: Layers of Moving Images

    Directory of Open Access Journals (Sweden)

    Floris Jan Willem Paalman

    2015-12-01

    Full Text Available After WWII, films accompanied the reconstruction of Europe’s destroyed cities. Many contained historical footage. How was this material used, to articulate visions of reconstruction, what happened to the material later on, and how do the films relate to municipal film archives? This question is approached in terms of collective cognitive functions, applied to a media archaeological case study of Rotterdam. In focus are two audiovisual landmarks, from 1950 and 1966, and their historical footage, all with different temporal horizons. This study attempts to position the city film archive in media history.

  10. Synthesis, structure refinement and chromate sorption characteristics of an Al-rich bayerite-based layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Britto, Sylvia, E-mail: sylviabritto11@gmail.com; Kamath, P. Vishnu

    2014-07-01

    “Imbibition” of Zn{sup 2+} ions into the cation vacancies of bayerite–Al(OH){sub 3} and NO{sub 3}{sup −} ions into the interlayer gallery yields an Al-rich layered double hydroxide with Al/Zn ratio ∼3. NO{sub 3}{sup −} ions are intercalated with their molecular planes inclined at an angle to the plane of the metal hydroxide slab and bonded to it by hydrogen bonds. Rietveld refinement of the structure shows that the monoclinic symmetry of the precursor bayerite is preserved in the product, showing that the imbibition is topochemical in nature. The nitrate ion is labile and is quantitatively replaced by CrO{sub 4}{sup 2−} ions from solution. The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm, thus showing that the hydroxide is a candidate material for green chemistry applications for the removal of CrO{sub 4}{sup 2−} ions from waste water. Rietveld refinement of the structure of the hydroxide after CrO{sub 4}{sup 2−} inclusion reveals that the CrO{sub 4}{sup 2−} ion is intercalated with one of its 2-fold axes parallel to the b-crystallographic axis of the crystal, also the principal 2 axis of the monoclinic cell. - Graphical abstract: The structure of the [Zn–Al4-nitrate] LDH viewed along the a-axis. - Highlights: • Synthesis of Al-rich layered double hydroxide with Al/Zn ratio ∼3. • Rietveld refinement indicates that the imbibition of Zn into Al(OH){sub 3} is topochemical in nature. • The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm.

  11. Study on the supramolecular structure of sorbic acid intercalated Zn-Al layered double hydroxides and its thermal decomposition

    Institute of Scientific and Technical Information of China (English)

    MENG Jinhong; ZHANG Hui; David G. Evans; DUAN Xue

    2005-01-01

    A novel organic-inorganic composite, sorbic acid intercalated zinc aluminum layered double hydroxides (SA-ZnAl-LDHs) has been successfully assembled by a simple direct coprecipitation method. A holistic approach including normal XRD, FT-IR, and UV-Vis measurements and simultaneous TG/DTA/MS and in situ HT-XRD techniques was employed to explore the supramolecular intercalation structure and the thermal decomposition properties of as-synthesized SA-ZnAl-LDHs material.

  12. Novel nanocomposite hydrogels consisting of layered double hydroxide with ultrahigh tensibility and hierarchical porous structure at low inorganic content.

    Science.gov (United States)

    Hu, Ziqiao; Chen, Guangming

    2014-09-10

    A novel type of polymer nanocomposite (NC) hydrogel with extraordinary mechanical properties at low inorganic content is prepared and investigated. The NC hydrogels consist of isethionate-loaded layered double hydroxide/polyacrylamide (LDH-Ise/PAM) - with LDH-Ise being used because of its swelling properties - and no conventional organic crosslinker. The NC hydrogels exhibit an unusual hierarchical porous structure at the micro- and nanometer scales, and their elongation at break can exceed 4000%.

  13. Toxicity and Metabolism of Layered Double Hydroxide Intercalated with Levodopa in a Parkinson’s Disease Model

    Directory of Open Access Journals (Sweden)

    Aminu Umar Kura

    2014-04-01

    Full Text Available Layered hydroxide nanoparticles are generally biocompatible, and less toxic than most inorganic nanoparticles, making them an acceptable alternative drug delivery system. Due to growing concern over animal welfare and the expense of in vivo experiments both the public and the government are interested to find alternatives to animal testing. The toxicity potential of zinc aluminum layered hydroxide (ZAL nanocomposite containing anti-Parkinsonian agent may be determined using a PC 12 cell model. ZAL nanocomposite demonstrated a decreased cytotoxic effect when compared to levodopa on PC12 cells with more than 80% cell viability at 100 µg/mL compared to less than 20% cell viability in a direct levodopa exposure. Neither levodopa-loaded nanocomposite nor the un-intercalated nanocomposite disturbed the cytoskeletal structure of the neurogenic cells at their IC50 concentration. Levodopa metabolite (HVA released from the nanocomposite demonstrated the slow sustained and controlled release character of layered hydroxide nanoparticles unlike the burst uptake and release system shown with pure levodopa treatment.

  14. Comparative X-ray diffraction and infrared spectroscopy study of Zn-Al layered double hydroxides: Vanadate vs nitrate

    Science.gov (United States)

    Salak, Andrei N.; Tedim, João; Kuznetsova, Alena I.; Ribeiro, José L.; Vieira, Luís G.; Zheludkevich, Mikhail L.; Ferreira, Mário G. S.

    2012-03-01

    Zn-Al layered double hydroxides (LDH) are promising as nanocontainers of corrosion inhibitors in self-healing corrosion protection coatings. Zn(2)Al-vanadate (Zn/Al = 2:1) is prepared by anion exchange from the parent composition Zn(2)Al-nitrate at pH ˜ 8. Crystal structure and vibrational spectra of both LDHs have been studied in comparison. Their interlayer distances are rather larger than those corresponding to the most compact arrangement of the intercalated anions. Nevertheless, no sign of a turbostratic disorder has been detected in these LDH. Based on the analysis of the spectroscopic data in combination with the XRD results, it has been shown that vanadate anion, which substitutes nitrate at the anion exchange, is pyrovanadate, VO74-. The observed disorder in the hydroxide layers in Zn(2)Al-V2O7 is likely to result from strong interactions between V5+ and Zn2+/Al3. Although Zn(2)Al-NO3 is less disordered than Zn(2)Al-V2O7, it exhibits no long-range order in arrangement of cations in the hydroxide layers.

  15. Removal of boron from oilfield wastewater via adsorption with synthetic layered double hydroxides.

    Science.gov (United States)

    Delazare, Thais; Ferreira, Letícia P; Ribeiro, Nielson F P; Souza, Mariana M V M; Campos, Juacyara C; Yokoyama, Lídia

    2014-01-01

    Hydrotalcite is a layered double hydroxide (LDH) consisting of brucite-like sheets of metal ions (Mg-Al). In this work, hydrotalcites were synthesized, and boron removal from oilfield wastewater was evaluated. LDHs were synthesized using the co-precipitation method. The calcined products (CLDHs) were obtained by heating at 500°C and characterized using X-ray diffraction, X-ray fluorescence, thermogravimetric analysis and the specific surface area (BET). The affinity of LDHs for borate ions was evaluated for calcined and uncalcined LDHs as a function of contact time, initial pH of the oilfield wastewater (pH ∼ 9) and the LDH surface area. The tests were conducted at room temperature (approximately 25ºC). The results indicated that 10 min were needed to reach a state of equilibrium during boron removal for calcined LDHs due to the high surface area (202.3 m(2) g(-1)) regardless of the initial pH of the oilfield wastewater, which resulted from the high buffering capacity of the LDHs. The adsorption capacity increased as the adsorbents levels increased for the range studied. After treatment of the oilfield wastewater containing 30 mg L(-1) of boron with Mg-Al-CO3-LDHs, the final concentration of boron was within the discharge limit set by current Brazilian environmental legislation, which is 5 mg L(-1). Pseudo-first-order and pseudo-second-order kinetic models were tested, and the latter was found to fit the experimental data better. Isotherms for boron adsorption by CLDHs were well described using the Langmuir and Freundlich equations.

  16. Atomistic simulation of nanoporous layered double hydroxide materials and their properties. II. Adsorption and diffusion

    Science.gov (United States)

    Kim, Nayong; Harale, Aadesh; Tsotsis, Theodore T.; Sahimi, Muhammad

    2007-12-01

    Nanoporous layered double hydroxide (LDH) materials have wide applications, ranging from being good adsorbents for gases (particularly CO2) and liquid ions to membranes and catalysts. They also have applications in medicine, environmental remediation, and electrochemistry. Their general chemical composition is [M1-xIIMxIII(OH-)2]x+[Xn/mm -•nH2O], where M represents a metallic cation (of valence II or III), and Xn/mm - is an m-valence inorganic, or heteropolyacid, or organic anion. We study diffusion and adsorption of CO2 in a particular LDH with MII=Mg, MIII=Al, and x ≃0.71, using an atomistic model developed based on energy minimization and molecular dynamics simulations, together with a modified form of the consistent-valence force field. The adsorption isotherms and self-diffusivity of CO2 in the material are computed over a range of temperature, using molecular simulations. The computed diffusivities are within one order of magnitude of the measured ones at lower temperatures, while agreeing well with the data at high temperatures. The measured and computed adsorption isotherms agree at low loadings, but differ by about 25% at high loadings. Possible reasons for the differences between the computed properties and the experimental data are discussed, and a model for improving the accuracy of the computed properties is suggested. Also studied are the material's hydration and swelling properties. As water molecules are added to the pore space, the LDH material swells to some extent, with the hydration energy exhibiting interesting variations with the number of the water molecules added. The implications of the results are discussed.

  17. Arsenate removal by layered double hydroxides embedded into spherical polymer beads: Batch and column studies.

    Science.gov (United States)

    Nhat Ha, Ho Nguyen; Kim Phuong, Nguyen Thi; Boi An, Tran; Mai Tho, Nguyen Thi; Ngoc Thang, Tran; Quang Minh, Bui; Van Du, Cao

    2016-01-01

    In this study, the performance of poly(layered double hydroxides) [poly(LDHs)] beads as an adsorbent for arsenate removal from aqueous solution was investigated. The poly(LDHs) beads were prepared by immobilizing LDHs into spherical alginate/polyvinyl alcohol (PVA)-glutaraldehyde beads (spherical polymer beads). Batch adsorption studies were conducted to assess the effect of contact time, solution pH, initial arsenate concentrations and co-existing anions on arsenate removal performance. The potential reuse of these poly(LDHs) beads was also investigated. Approximately 79.1 to 91.2% of arsenic was removed from an arsenate solution (50 mg As L(-1)) by poly(LDHs). The adsorption data were well described by the pseudo-second-order kinetics model and the Langmuir isotherm model, and the adsorption capacities of these poly(LDHs) beads at pH 8 were from 1.64 to 1.73 mg As g(-1), as calculated from the Langmuir adsorption isotherm. The adsorption ability of the poly(LDHs) beads decreased by approximately 5-6% after 5 adsorption-desorption cycles. Phosphates markedly decreased arsenate removal. The effect of co-existing anions on the adsorption capacity declined in the following order: HPO4 (2-) > HCO3 (-) > SO4 (2-) > Cl(-). A fixed-bed column study was conducted with real-life arsenic-containing water. The breakthrough time was found to be from 7 to 10 h. Under optimized conditions, the poly(LDHs) removed more than 82% of total arsenic. The results obtained in this study will be useful for further extending the adsorbents to the field scale or for designing pilot plants in future studies. From the viewpoint of environmental friendliness, the poly(LDHs) beads are a potential cost-effective adsorbent for arsenate removal in water treatment.

  18. Layered double hydroxide-oxidized carbon nanotube hybrids as highly efficient flame retardant nanofillers for polypropylene

    Science.gov (United States)

    Gao, Yanshan; Zhang, Yu; Williams, Gareth R.; O’Hare, Dermot; Wang, Qiang

    2016-01-01

    Aqueous miscible organic layered double hydroxides (AMO-LDHs) can act as organophilic inorganic flame retardant nanofillers for unmodified non-polar polymers. In this contribution, AMO [Mg3Al(OH)8](CO3)0.5·yH2O LDH–oxidized carbon nanotube (AMO-LDH–OCNT) hybrids are shown to perform better than the equivalent pure AMO-LDH. A synergistic effect between the AMO-LDH and OCNT was observed; this endows the hybrid material with enhanced flame retardancy, thermal stability, and mechanical properties. The thermal stability of polypropylene (PP) was significantly enhanced by adding AMO-LDH–OCNT hybrids. For PP mixed with AMO-LDH–OCNT hybrids to produce a composite with 10 wt% LDH and 2 wt% OCNT, the 50% weight loss temperature was increased by 43 °C. Further, a system with 10 wt% of AMO-LDH and 1 wt% OCNT showed a peak heat release rate (PHRR) reduction of 40%, greater than the PHRR reduction with PP/20 wt% AMO-LDH (31%). The degree of dispersion (mixability) between AMO-LDH and OCNT has a significant effect on the flame retardant performance of the hybrids. In addition, the incorporation of AMO-LDH–OCNT hybrids led to better mechanical properties, such as higher tensile strength (27.5 MPa) and elongation at break (17.9%), than those composites containing only AMO-LDH (25.6 MPa and 7.5%, respectively). PMID:27752096

  19. Layered Double Hydroxides with Hydrotalcite-type Structure Containing Fe3+, Al3+ and Mg2+

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Layered double hydroxides(LDHs) with hydrotalcite-type structure containing Fe3+, Al3+ and Mg2+ were prepared by means of a coprecipitation method. The products were characterized by element analysis, X-ray powder diffraction and transmission electron microscopy. It was found that even if the molar ratio of n(Fe+Al)/n(Fe+Al+Mg)>0.33, yet a pure hydrotalcite-like compound(HTlc) phase was gained when n(Fe)/n(Al+Mg+Fe)≤0.30 and n(Al)/n(Al+Mg+Fe)≤0.30; the Al(OH)3 phase appeared in the products when n(Al)/n(Al+Mg+Fe)>0.30; and an amorphous phase emerged when n(Fe)/n(Al+Mg+Fe)>0.33. These results show that there is no concentration superposition effect between Fe3+ and Al3+ on the crystalline state of the produced samples. In our previous work, the concentration superposition effect between Zn2+ and Mg2+ in the synthesis of Zn-Mg-Al-LDHs was found. For the prepared Fe-Al-Mg-LDHs samples, the value of lattice parameter a is between 0.30-0.32 nm; and the value of lattice parameter c is between 2.30-2.47 nm, the basal spacing is in the range of 0.76-0.83 nm. When the ratio of n(Fe)/n(Al) is a constant, the values of a and c increase with the increase of the Mg2+ content of the produced samples. The mean particle size and the mean crystal grain were determined by virtue of a particle-size instrument, XRD-Scherrer formula and TEM method, respectively.

  20. Epigallocatechin Gallate/Layered Double Hydroxide Nanohybrids: Preparation, Characterization, and In Vitro Anti-Tumor Study.

    Directory of Open Access Journals (Sweden)

    Seyedeh Sara Shafiei

    Full Text Available In recent years, nanotechnology in merging with biotechnology has been employed in the area of cancer management to overcome the challenges of chemopreventive strategies in order to gain promising results. Since most biological processes occur in nano scale, nanoparticles can act as carriers of certain drugs or agents to deliver it to specific cells or targets. In this study, we intercalated Epigallocatechin-3-Gallate (EGCG, the most abundant polyphenol in green tea, into Ca/Al-NO3 Layered double hydroxide (LDH nanoparticles, and evaluated its efficacy compared to EGCG alone on PC3 cell line. The EGCG loaded LDH nanohybrids were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy (TEM and nanosizer analyses. The anticancer activity of the EGCG-loaded LDH was investigated in prostate cancer cell line (PC3 while the release behavior of EGCG from LDH was observed at pH 7.45 and 4.25. Besides enhancing of apoptotic activity of EGCG, the results showed that intercalation of EGCG into LDH can improve the anti- tumor activity of EGCG over 5-fold dose advantages in in-vitro system. Subsequently, the in-vitro release data showed that EGCG-loaded LDH had longer release duration compared to physical mixture, and the mechanism of diffusion through the particle was rate-limiting step. Acidic attack was responsible for faster release of EGCG molecules from LDH at pH of 4.25 compared to pH of 7.4. The results showed that Ca/Al-LDH nanoparticles could be considered as an effective inorganic host matrix for the delivery of EGCG to PC3 cells with controlled release properties.

  1. Layered double hydroxide-oxidized carbon nanotube hybrids as highly efficient flame retardant nanofillers for polypropylene

    Science.gov (United States)

    Gao, Yanshan; Zhang, Yu; Williams, Gareth R.; O'Hare, Dermot; Wang, Qiang

    2016-10-01

    Aqueous miscible organic layered double hydroxides (AMO-LDHs) can act as organophilic inorganic flame retardant nanofillers for unmodified non-polar polymers. In this contribution, AMO [Mg3Al(OH)8](CO3)0.5·yH2O LDH-oxidized carbon nanotube (AMO-LDH-OCNT) hybrids are shown to perform better than the equivalent pure AMO-LDH. A synergistic effect between the AMO-LDH and OCNT was observed; this endows the hybrid material with enhanced flame retardancy, thermal stability, and mechanical properties. The thermal stability of polypropylene (PP) was significantly enhanced by adding AMO-LDH-OCNT hybrids. For PP mixed with AMO-LDH-OCNT hybrids to produce a composite with 10 wt% LDH and 2 wt% OCNT, the 50% weight loss temperature was increased by 43 °C. Further, a system with 10 wt% of AMO-LDH and 1 wt% OCNT showed a peak heat release rate (PHRR) reduction of 40%, greater than the PHRR reduction with PP/20 wt% AMO-LDH (31%). The degree of dispersion (mixability) between AMO-LDH and OCNT has a significant effect on the flame retardant performance of the hybrids. In addition, the incorporation of AMO-LDH-OCNT hybrids led to better mechanical properties, such as higher tensile strength (27.5 MPa) and elongation at break (17.9%), than those composites containing only AMO-LDH (25.6 MPa and 7.5%, respectively).

  2. Rapid exchange between atmospheric CO2 and carbonate anion intercalated within magnesium rich layered double hydroxide.

    Science.gov (United States)

    Sahoo, Pathik; Ishihara, Shinsuke; Yamada, Kazuhiko; Deguchi, Kenzo; Ohki, Shinobu; Tansho, Masataka; Shimizu, Tadashi; Eisaku, Nii; Sasai, Ryo; Labuta, Jan; Ishikawa, Daisuke; Hill, Jonathan P; Ariga, Katsuhiko; Bastakoti, Bishnu Prasad; Yamauchi, Yusuke; Iyi, Nobuo

    2014-10-22

    The carbon cycle, by which carbon atoms circulate between atmosphere, oceans, lithosphere, and the biosphere of Earth, is a current hot research topic. The carbon cycle occurring in the lithosphere (e.g., sedimentary carbonates) is based on weathering and metamorphic events so that its processes are considered to occur on the geological time scale (i.e., over millions of years). In contrast, we have recently reported that carbonate anions intercalated within a hydrotalcite (Mg0.75Al0.25(OH)2(CO3)0.125·yH2O), a class of a layered double hydroxide (LDH), are dynamically exchanging on time scale of hours with atmospheric CO2 under ambient conditions. (Ishihara et al., J. Am. Chem. Soc. 2013, 135, 18040-18043). The use of (13)C-labeling enabled monitoring by infrared spectroscopy of the dynamic exchange between the initially intercalated (13)C-labeled carbonate anions and carbonate anions derived from atmospheric CO2. In this article, we report the significant influence of Mg/Al ratio of LDH on the carbonate anion exchange dynamics. Of three LDHs of various Mg/Al ratios of 2, 3, or 4, magnesium-rich LDH (i.e., Mg/Al ratio = 4) underwent extremely rapid exchange of carbonate anions, and most of the initially intercalated carbonate anions were replaced with carbonate anions derived from atmospheric CO2 within 30 min. Detailed investigations by using infrared spectroscopy, scanning electron microscopy, powder X-ray diffraction, elemental analysis, adsorption, thermogravimetric analysis, and solid-state NMR revealed that magnesium rich LDH has chemical and structural features that promote the exchange of carbonate anions. Our results indicate that the unique interactions between LDH and CO2 can be optimized simply by varying the chemical composition of LDH, implying that LDH is a promising material for CO2 storage and/or separation.

  3. Nanohybrid based on antibiotic encapsulated layered double hydroxide as a drug delivery system.

    Science.gov (United States)

    Khan, Sher Bahadar; Alamry, Khalid A; Alyahyawi, Nedaa A; Asiri, Abdullah M; Arshad, Muhammad Nadeem; Marwani, Hadi M

    2015-02-01

    Nanohybrid of cefuroxime (CFO) with layered double hydroxide (LDH) has been prepared, and the rate of dissolution and bioavailability of CFO using nanohybrid as a drug delivery system has been broadly studied. The intercalation process was confirmed by X-ray diffraction, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The CFO contents were found to be 19.0 wt% in the nanohybrid. The release mechanism of CFO was investigated with respect to anion and pH of the dissolution media such as gastric, intestinal and blood simulated media. The effect of pH was evaluated on the release of CFO from nanohybrid, and the dissolution of CFO from the nanohybrid was found to be a slow process at pH 4.0, 6.8, and 7.4. Further the addition of Cl ion and PAM in release media did not affect the release rate of drug at pH 4.0 and 6.8, while at pH 7.4, Cl ion and PAM have significant role on the drug release. At pH 1.2, the release study shows that LDH dissolved in the acidic medium and CFO released in its molecular form. The release behavior suggests two mechanisms that are responsible for the release of CFO from nanohybrid: weathering (dependent on the pH) and ion exchange (highly dependent on the anions). Surface reactions mediated by solid weathering ruled the release in gastric fluid, whereas anion exchange determined CFO release in lysosomal, intestinal, and blood medium. In order to evaluate the drug release mechanism, the released data were fitted by mathematical models describing various kinetic.

  4. Insights into the synthesis of layered double hydroxide (LDH) nanoparticles: Part 2. Formation mechanisms of LDH.

    Science.gov (United States)

    Sun, Xiaodi; Dey, Sandwip K

    2015-11-15

    This study demonstrates the effect of (co)intercalated anion compositions on nanostructure evolution to understand the formation mechanisms of layered double hydroxide (LDH) nanoparticles following coprecipitation and hydrothermal treatments (HT). Initially, the room temperature coprecipitation resulted in amorphous primary nanoparticles that agglomerated at the edges due to low surface charge densities. The reversibility of such agglomeration was determined by the crystalline quality upon HT and consequent surface charge density, which in turn were strongly influenced by the composition of the intercalated anions. Upon crystallization, the agglomerated Zn2Al(OH)6(NO3)0.3(CO3)0.35⋅xH2O primary nanoparticles re-dispersed, but the Zn2Al(OH)6(NO3)⋅xH2O nanoparticles with much lower stability and higher disorder (especially at the edges) exhibited irreversible agglomeration, and transformed into secondary nanoparticles via aggregational growth. Additionally, the stability studies on Zn2Al(OH)6(NO3)y(CO3)0.5(1-y)⋅xH2O nanoparticles (y=0-1) showed that the size difference between the cointercalated anions caused phase separation when 0.9⩾y⩾0.6, leading to bimodal size distributions. Moreover, the coarsening rates were controlled through the cointercalated anion compositions. By gradually varying the ratio of cointercalated NO3(-) to CO3(2-), monodispersed Zn2Al(OH)6(NO3)y(CO3)0.5(1-y)⋅xH2O (0.5⩾y⩾0) nanoparticles with systematic variation in the particle size of ∼200-400nm were obtained after HT at 85°C for 12h.

  5. Reconstruction of microstructure in catalyst layer of PEM fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Rong, F.; Huang, C.; Liu, Z.S.; Song, D.T.; Wang, Q.P. [National Research Council of Canada, Vancouver, BC (Canada). Inst. for Fuel Cell Innovation

    2007-07-01

    Different microstructures of catalyst layer (CL) have been experimentally studied to improve the performance of the proton membrane exchange (PEM) fuel cell. These experiments have revealed the microstructure in catalyst layers can be considered as one kind of random media and its changes will have significant influence on the performance of PEM fuel cell. This paper presented the results of a study that applied the filtering method and stochastic optimization to reconstruct the microstructure based on the statistical information of catalyst layers. The filtering method changes the Gauss distributed signals to three-phase microstructure reconstruction while the stochastic optimization method, refines the microstructure reconstruction to fit the statistical features of experimental images. Based on the physical properties as well as the mass ratio, the statistical feature extraction based on image process of catalyst layer and the reconstruction procedure was proposed. The paper discussed evaluation of phase statistical information, initial reconstruction based on filtering method, stochastic optimization for reconstruction, as well as a summary of the study. It was concluded that the results of the filtering method as the initial pattern of stochastic optimization could make the error (between the final result and the experimental target) less than that of the random initial value and saved the computational time simultaneously. 13 refs., 6 figs.

  6. Structural features of intercalated CaFe-layered double hydroxides studied by X-ray diffractometry, infrared spectroscopy and computations

    Science.gov (United States)

    Ferencz, Zs.; Ádok-Sipiczki, M.; Hannus, I.; Sipos, P.; Pálinkó, I.

    2015-06-01

    The intercalation of various N-containing carboxylic acid anions into CaFe-layered double hydroxides was performed by the dehydration-rehydration method. Particular attention was paid to the effect of solvent mixture used during preparation. It was found that various solvent mixtures resulted in different interlayer distances and, thus, different arrangements of the anions between the layers. The dimensions of the intercalated anions and detailed analysis of the infrared spectra gave clues for the reasonable prediction of the spatial arrangements of the anions in the interlamellar space.

  7. Preparation, characterization and thermodynamic properties of Zr-containing Cl-bearing layered double hydroxides (LDHs)

    Energy Technology Data Exchange (ETDEWEB)

    Rozov, Konstantin; Curtius, Hilde; Bosbach, Dirk [Forschungszentrum Juelich GmbH (Germany). Inst. of Energy and Climate Research (IEK-6) Nuclear Waste Management and Reactor Safety

    2015-07-01

    Zr-containing layered double hydroxides (LDHs) with variable xZr{sub solid} = Zr/(Zr + Al) mole fractions were synthesized by a co-precipitation method at ambient conditions. The chemical compositions of samples and corresponding aqueous solutions after syntheses were analyzed by ICP-OES, EDX (Mg, Al, Zr) and ion chromatography (Cl{sup -}). Results of PXRD technique demonstrated that solids with 0 ≤ x Zr{sub solid} ≤ 0.5 show only X-ray reflexes typical for pure LDH compositions, while products of syntheses with xZr{sub solid} > 0.5 display additional patterns attributed to brucite. ICP-OES and EDX techniques shown that in pure Zr-containing LDHs the Mg/(Al + Zr) ratio is reducing with increase of xZr{sub solid} and the stoichiometry of brucite-like layers corresponds to [Mg{sub 3-2x}Al{sub 1-x}Zr{sub x}]. This fact may indicate that the incorporation of 1 Zr-containing specie results in the removal of 1 Al- and 2 Mg-containing species from the pure Mg-Al-composition. Such mechanism may be confirmed by the observation that measured a{sub 0} = b{sub 0} distances are generally consistent with theoretical estimates obtained from [Mg{sub 3-2x}Al{sub 1-x}Zr{sub x}]-stoichiometry. The presence of predominant Mg{sup 2+}, Al(OH){sub 4}{sup -} and Zr(OH){sub 5}{sup -} complexes in aqueous solutions after syntheses was established in thermodynamic calculations by applying GEMS-Selektor v.3. code and, therefore, the reaction: Mg{sub 3}Al{sub 1}(OH){sub 8}Cl{sub 1} + Zr(OH){sub 5}{sup -} = Mg{sub 1}Zr{sub 1}(OH){sub 5}Cl{sub 1} + Al(OH){sub 4}{sup -} + 2Mg{sup 2+} + 4OH{sup -} can describe a mechanism of Zr-substitution. Estimates of the molar Gibbs free energies of Zr-containing LDHs with 0 ≤ = xZr{sub solid} ≤ 0.5 show that the incorporation of Zr into the LDH increasing significantly their aqueous solubility. Thus, it is not possible to neglect that Zr can be partly localized as Zr(OH){sub 5}{sup -}-ligands in the interlayer space of the LDH structure.

  8. Synthesis and characterization of metal (Core) - layered double hydroxide (Shell) nanostructures

    Science.gov (United States)

    Noh, Woo C.

    Layered double hydroxides (LDH) which belong to a class of inorganic ceramic layered materials have been studied since the mid-19th century for a variety of applications including catalysis, anion exchange, adsorbents and antacid, but more recently as a potential drug and gene delivery platform. Drug delivery platforms based on nano-sized geometries are nanovectors which promise a revolutionary impact on the therapy and imaging of various types of cancers and diseases. To date, various polymeric platforms have been the focus of intense research, but the development of inorganic, bio-hybrid nanoparticles for therapeutics and molecular imaging are at a stage of infancy. The hybridization of LDH with bioactive agents or the fabrication of metal (Core)---LDH (Shell) nanostructures could have many beneficial effects including multimodality, active targetability, and efficacy. For example, Core---Shell nanostructures may be designed to have a high scattering optical cross-section for imaging, but may also be tailored to strongly absorb near infrared (NIR) light for hyperthermic ablation. The central theme of this thesis was to demonstrate proof-of-concept of spherical silver and gold metal (Core)---LDH (Shell) nanostructures that have uniform size distribution and are agglomeration free. The effects of processing parameters on the characteristics of LDH as well as LDH-coated spherical metal (Ag, Au) nanoparticles have been evaluated using X-ray Diffraction, Dynamic Light Scattering, Scanning Electron Microscopy, Transmission Electron Microscopy, Rutherford Backscattering Spectrometry, and Inductively Coupled Plasma Emission Spectrometry to arrive at appropriate process windows. The core---shell nanostructures were also characterized for their optical properties in the ultra---violet---visible region, and the data were compared with simulated data, computed by using a quasi static model from Mie scattering theory. Moreover, in order to achieve a strong plasmon resonance

  9. Ion exchange and intercalation properties of layered double hydroxides towards halide anions.

    Science.gov (United States)

    Costantino, Umberto; Vivani, Riccardo; Bastianini, Maria; Costantino, Ferdinando; Nocchetti, Morena

    2014-08-14

    A layered double hydroxide (LDH) obtained by the urea method, having an empirical formula [Zn(0.61)Al(0.39)(OH)2](CO3)(0.195)·0.50H2O, has been converted into the corresponding chloride form [Zn(0.61)Al(0.39)(OH)2]Cl(0.39)·0.47H2O by making the solid come into contact with a suitable HCl solution. The intercalation of the other halide anions (X(-) = F(-), Br(-), I(-)) via the Cl(-)/X(-) anion exchange has been attained and the respective anion exchange isotherms have been obtained with the batch method. The analysis of the isotherms indicates that the selectivity of LDH towards the halides decreases with the increase of the X(-) ionic radius, the selectivity order being F(-) > Cl(-)≥ Br(-) > I(-). The CO3(2-)/Cl(-) isotherm has also been reported to highlight the extraordinary selectivity of LDH towards carbonate anions. Samples taken from the isotherms at different exchange degrees were analyzed by X-ray diffraction, thermogravimetry and thermodiffractometry to obtain information about the ion exchange mechanism. The Cl(-)/Br(-) and the reverse Br(-)/Cl(-) exchanges occur with the formation of solid solutions, very likely because of the similar ionic radius of the exchanging anions. In contrast, in the Cl(-)/F(-) and Cl(-)/I(-) exchange, the co-existence of the Cl(-) and F(-) (or I(-)) phases in the same sample was detected, indicating the occurrence of a first order phase transition, in which the starting phase is transformed into the final phase, as the process goes on. The variation of the interlayer distances of ZnAl-X intercalation compounds with the hydration degree has been interpreted with a structural model based on the nesting of the guest species into the trigonal pockets of the brucite-like layer surface. Rietveld refinements of the phases with the maximum F(-), Br(-) and I(-) content were also performed and compared with the above model, giving indications of the arrangement and order/disorder of the halide anions in the interlayer region.

  10. Analysing the archaeological context: Reconstructing stratigraphic layers

    Science.gov (United States)

    Schubert, Lutz; Predoi, Ana; Jeffery, Keith

    2017-07-01

    The stratigraphic layout of an excavation determines how finds can be interpreted regarding their timeline and relationships with each other. Older excavation reports do not fully record this layout however and reconstructing the relationships is often subject to conjecture. In this paper we present a first approach for reasoning over and visualizing the stratigraphy given only profile information. We will demonstrate how this can be used for spatial analysis, but also for reasoning over different processes contributing to the found layout, including potential influences that left no visible traces.

  11. Study of the structure and luminescent properties of terbium complex intercalated Zn/Al layered double hydroxide

    Science.gov (United States)

    Gao, Xiaorui; Xie, Juan; Yin, Yaobing; Hao, Yongjing; Lian, Yiwei

    2016-01-01

    Terbium complex of ethylenediaminetetraacetate ([Tb(EDTA)]-) intercalated Zn/Al layered double hydroxide (LDH), as an inorganic-organic green-emitting phosphor, was synthesized through an ion exchange method. X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) spectra exhibit a successful intercalation of [Tb(EDTA)]- anions between the hydroxide sheets of the LDH. The basal spacing of 14.5 Å indicate a vertical arrangement of [Tb(EDTA)]- anions with the maximal dimension in the gallery is adopted. The luminescent properties of this material were studied by excitation and emission spectra. The results show that the strongest emission peak of Tb3+ ion occurs at 544 nm. This material may supply a candidate of green light emitting phosphor.

  12. Synthesis of mesoporous silica@Co-Al layered double hydroxide spheres: layer-by-layer method and their effects on the flame retardancy of epoxy resins.

    Science.gov (United States)

    Jiang, Shu-Dong; Bai, Zhi-Man; Tang, Gang; Song, Lei; Stec, Anna A; Hull, T Richard; Hu, Yuan; Hu, Wei-Zhao

    2014-08-27

    Hierarchical mesoporous silica@Co-Al layered double hydroxide (m-SiO2@Co-Al LDH) spheres were prepared through a layer-by-layer assembly process, in order to integrate their excellent physical and chemical functionalities. TEM results depicted that, due to the electrostatic potential difference between m-SiO2 and Co-Al LDH, the synthetic m-SiO2@Co-Al LDH hybrids exhibited that m-SiO2 spheres were packaged by the Co-Al LDH nanosheets. Subsequently, the m-SiO2@Co-Al LDH spheres were incorporated into epoxy resin (EP) to prepare specimens for investigation of their flame-retardant performance. Cone results indicated that m-SiO2@Co-Al LDH incorporated obviously improved fire retardant of EP. A plausible mechanism of fire retardant was hypothesized based on the analyses of thermal conductivity, char residues, and pyrolysis fragments. Labyrinth effect of m-SiO2 and formation of graphitized carbon char catalyzed by Co-Al LDH play pivotal roles in the flame retardance enhancement.

  13. Layered Double Hydroxide Assemblies with Controllable Drug Loading Capacity and Release Behavior as well as Stabilized Layer-by-Layer Polymer Multilayers.

    Science.gov (United States)

    Lv, Fengzhu; Xu, Linan; Zhang, Yihe; Meng, Zilin

    2015-09-02

    A stable drug release system with magnetic targeting is essential in a drug delivery system. In the present work, layered double hydroxide assemblies stabilized by layer-by-layer polymer multilayers were prepared by alternative deposition of poly(allylamine hydrochloride) and poly(acrylic acid) species on composite particles of Fe3O4 and ZnAl-LDH and then covalent cross-linkage of the polymer multilayers by photosensitive cross-linker. The successful fabrication was recorded by Zeta potential and Fourier transform infrared spectrum measurements. The formed assemblies were stable in high pH solutions (pH > 7). The drug loading capacity and release behavior of the assemblies could be controlled by treatment with appropriate acidic solution, and were confirmed by loading and release of a simulated drug, methylene blue. The formed assemblies possessed enough saturated magnetic strength and were sensitive to external magnetic field which was essential for targeting drug delivery. The formed assemblies were multifunctional assemblies with great potential as drug delivery system.

  14. Layer-by-layer assembled multilayer films of exfoliated layered double hydroxide and carboxymethyl-β-cyclodextrin for selective capacitive sensing of acephatemet.

    Science.gov (United States)

    Gong, Jingming; Han, Xinmei; Zhu, Xiaolei; Guan, Zhangqiong

    2014-11-15

    Novel organic-inorganic hybrid ultrathin films were fabricated by alternate assembly of cationic exfoliated Mg-Al-layered double hydroxide (LDH) nanosheets and carboxymethyl-β-cyclodextrin (CMCD) as a polyanion onto a glassy carbon electrode (GCE) via a layer-by-layer (LBL) approach. The multilayer films were then characterized by means of X-ray powder diffraction (XRD), infrared spectroscopy (IR), and scanning electron microscopy (SEM). These films were found to possess a long range stacking order in the normal direction of the substrate with a continuous and uniform morphology. Its electrochemical performance was systematically investigated. Our results demonstrate that such a newly designed (LDH/CMCD)n multilayer film, combining the individual properties of CMCD (a high supramolecule recognition and enrichment capability) together with LDH nanosheets (a rigid inorganic matrix), can be applied to a sensitive, simple, and label-free capacitive detection of acephatemet (AM). Molecular docking calculations further disclose that the selective sensing behavior toward AM may be attributed to the specific binding ability of CMCD to AM. Under the optimized conditions, the capacitive change of AM was proportional to its concentration ranging from 0.001 to 0.10 μg mL(-1) and 0.1 to 0.8 μg mL(-1) with a detection limit 0.6 ng mL(-1) (S/N=3). Toward the goal for practical applications, this simple probe was further evaluated by monitoring AM in real samples.

  15. Co-intercalation of Acid Red 337 and a UV absorbent into layered double hydroxides: enhancement of photostability.

    Science.gov (United States)

    Li, Dianqing; Qian, Leilei; Feng, Yongjun; Feng, Junting; Tang, Pinggui; Yang, Lan

    2014-12-10

    Organic-inorganic hybrid pigments with enhanced thermo- and photostability have been prepared by co-intercalating C.I. Acid Red 337 (AR337) and a UV absorbent (BP-4) into the interlayer of ZnAl layered double hydroxides through a coprecipitation method. The obtained compounds were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermogravimetric-differential thermal analysis, UV-visible spectroscopy, and the International Commission on Illumination (CIE) 1976 L*a*b* color scales. The results show the successful co-intercalation of AR337 and BP-4 into the interlayer region of layered double hydroxides (LDHs) and reveal the presence of host-guest interactions between LDH host layers and guest anions of AR337 and BP-4 and guest-guest interactions between AR337 and BP-4. The intercalation can improve the thermostability of AR337 due to the protection of LDH layers. Moreover, the co-intercalation of AR337 and BP-4 not only markedly enhances the photostability of AR337 but also significantly influences the color of the hybrid pigment.

  16. Signalling pathways involved in the activation of dendritic cells by layered double hydroxide nanoparticles.

    Science.gov (United States)

    Li, Ang; Qin, Lili; Zhu, Di; Zhu, Rongrong; Sun, Jing; Wang, Shilong

    2010-02-01

    Layered double hydroxide (LDH) nanoparticles are attractive as potential drug vectors for the targeting not only of tissues, but also of intracellular organelles, and particularly the acidic endolysosomes created after cell endocytosis. The purpose of this study was to investigate the ability of LDH nanoparticles designed as vectors to activate dendritic cells (DCs), as measured by various cellular functions. The study also explored the possible signaling pathway through which the LDH nanoparticles exerted their effects on the cellular functions of DCs. First, LDH nanoparticles with different ratios of Mg(OH)(2) to Al(OH)(3) (1:1, 2:1 and 3:1, called R1, R2 and R3 respectively) were optimized and had a hydrodynamic diameter of 57 nm with a zeta potential of +35 mV. Then, the efficient endocytosis of the optimized LDH nanoparticles by bone marrow-derived dendritic cells (MDDCs) was monitored by fluorescence-activated cell sorting. The effect of R1, R2 and R3 on the expression of the pro- and anti-inflammatory cytokines (TNF-alpha, IL-6, and IL-12) and the co-stimulatory molecules (CD40, CD80, CD86, and MHC class II) in MDDCs was examined. The exposure of R1 caused a dose-dependent increase in the expression of TNF-alpha, IL-12, CD86 and CD40, while R2 and R3 did not up-regulate these cytokines and co-stimulatory molecules. Migration assays showed that R1 could increase the migration capacity of DCs to CCL21 and up-regulate the expression of CCR7. Furthermore, we found that R1 significantly increased the NF-kappaB expression in the nucleus (in a dose-dependent manner) and promoted the degradation of total IkappaBalpha levels, indicating that the NF-kappaB signaling pathway might involve in an R1-induced DC activation. Our results suggested that LDH nanoparticles, in the future, may function as a useful vector for ex vivo engineering to promote vaccine delivery in immune cells.

  17. Hybrid Materials Based on Magnetic Layered Double Hydroxides: A Molecular Perspective.

    Science.gov (United States)

    Abellán, Gonzalo; Martí-Gastaldo, Carlos; Ribera, Antonio; Coronado, Eugenio

    2015-06-16

    Design of functional hybrids lies at the very core of synthetic chemistry as it has enabled the development of an unlimited number of solids displaying unprecedented or even improved properties built upon the association at the molecular level of quite disparate components by chemical design. Multifunctional hybrids are a particularly appealing case among hybrid organic/inorganic materials. Here, chemical knowledge is used to deploy molecular components bearing different functionalities within a single solid so that these properties can coexist or event interact leading to unprecedented phenomena. From a molecular perspective, this can be done either by controlled assembly of organic/inorganic molecular tectons into an extended architecture of hybrid nature or by intercalation of organic moieties within the empty channels or interlamellar space offered by inorganic solids with three-dimensional (MOFs, zeolites, and mesoporous hosts) or layered structures (phosphates, silicates, metal dichalcogenides, or anionic clays). This Account specifically illustrates the use of layered double hydroxides (LDHs) in the preparation of magnetic hybrids, in line with the development of soft inorganic chemistry processes (also called "Chimie Douce"), which has significantly contributed to boost the preparation hybrid materials based on solid-state hosts and subsequent development of applications. Several features sustain the importance of LDHs in this context. Their magnetism can be manipulated at a molecular level by adequate choice of constituting metals and interlayer separation for tuning the nature and extent of magnetic interactions across and between planes. They display unparalleled versatility in accommodating a broad range of anionic species in their interlamellar space that encompasses not only simple anions but chemical systems of increasing dimensionality and functionalities. Their swelling characteristics allow for their exfoliation in organic solvents with high

  18. Layered double hydroxides as the next generation inorganic anion exchangers: Synthetic methods versus applicability.

    Science.gov (United States)

    Chubar, Natalia; Gilmour, Robert; Gerda, Vasyl; Mičušík, Matej; Omastova, Maria; Heister, Katja; Man, Pascal; Fraissard, Jacques; Zaitsev, Vladimir

    2017-07-01

    This work is the first report that critically reviews the properties of layered double hydroxides (LDHs) on the level of speciation in the context of water treatment application and dynamic adsorption conditions, as well as the first report to associate these properties with the synthetic methods used for LDH preparation. Increasingly stronger maximum allowable concentrations (MAC) of various contaminants in drinking water and liquid foodstuffs require regular upgrades of purification technologies, which might also be useful in the extraction of valuable substances for reuse in accordance with modern sustainability strategies. Adsorption is the main separation technology that allows the selective extraction of target substances from multicomponent solutions. Inorganic anion exchangers arrived in the water business relatively recently to achieve the newly approved standards for arsenic levels in drinking water. LDHs (or hydrotalcites, HTs) are theoretically the best anion exchangers due to their potential to host anions in their interlayer space, which increases their anion removal capacity considerably. This potential of the interlayer space to host additional amounts of target aqueous anions makes the LDHs superior to bulk anion exchanger. The other unique advantage of these layered materials is the flexibility of the chemical composition of the metal oxide-based layers and the interlayer anions. However, until now, this group of "classical" anion exchangers has not found its industrial application in adsorption and catalysis at the industrial scale. To accelerate application of LDHs in water treatment on the industrial scale, the authors critically reviewed recent scientific and technological knowledge on the properties and adsorptive removal of LDHs from water on the fundamental science level. This also includes review of the research tools useful to reveal the adsorption mechanism and the material properties beyond the nanoscale. Further, these properties are

  19. Ag-loaded MgSrFe-layered double hydroxide/chitosan composite scaffold with enhanced osteogenic and antibacterial property for bone engineering tissue.

    Science.gov (United States)

    Cao, Dandan; Xu, Zhengliang; Chen, Yixuan; Ke, Qinfei; Zhang, Changqing; Guo, Yaping

    2017-04-17

    Bone tissue engineering scaffolds for the reconstruction of large bone defects should simultaneously promote osteogenic differentiation and avoid postoperative infection. Herein, we develop, for the first time, Ag-loaded MgSrFe-layered double hydroxide/chitosan (Ag-MgSrFe/CS) composite scaffold. This scaffold exhibits three-dimensional interconnected macroporous structure with a pore size of 100-300 μm. The layered double hydroxide nanoplates in the Ag-MgSrFe/CS show lateral sizes of 200-400 nm and thicknesses of ∼50 nm, and the Ag nanoparticles with particle sizes of ∼20 nm are uniformly dispersed on the scaffold surfaces. Human bone marrow-derived mesenchymal stem cells (hBMSCs) present good adhesion, spreading, and proliferation on the Ag-MgSrFe/CS composite scaffold, suggesting that the Ag and Sr elements in the composite scaffold have no toxicity to hBMSCs. When compared with MgFe/CS composite scaffold, the Ag-MgSrFe/CS composite scaffold has better osteogenic property. The released Sr(2+) ions from the composite scaffold enhance the alkaline phosphatase activity of hBMSCs, promote the extracellular matrix mineralization, and increase the expression levels of osteogenic-related RUNX2 and BMP-2. Moreover, the Ag-MgSrFe/CS composite scaffold possesses good antibacterial property because the Ag nanoparticles in the composite scaffold effectively prevent biofilm formation against S. aureus. Hence, the Ag-MgSrFe/CS composite scaffold with excellent osteoinductivity and antibacterial property has a great potential for bone tissue engineering. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2017. © 2017 Wiley Periodicals, Inc.

  20. Tribological performance of Mg/Al/Ce layered double hydroxides nanoparticles and intercalated products as lubricant additives

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shuo; Qin, Haojing; Zuo, Ranfang; Bai, Zhimin, E-mail: zhimibai@cugb.edu.cn

    2015-10-30

    Highlights: • Mg/Al/Ce layered double hydroxides (LDHs) were synthesized by coprecipitation. • Mg/Al/Ce LDHs were intercalated with succinic acid and lauric acid respectively. • LDHs intercalated with lauric acid had the best friction properties among products. • Sliding of layers, good dispersity and a protective film decided the performance. - Abstract: Mg/Al/Ce ternary layered double hydroxides (LDHs) were synthesized via coprecipitation and intercalated by succinic acid and lauric acid through ion exchange method respectively. The LDHs products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared (FT-IR). Tribological properties of LDHs as lubricant additives were evaluated by four-ball friction and air compressor test. The results indicated that Mg/Al/Ce LDHs were prepared successfully with Ce/Al molar ratio of 0.05 and crystallization temperature of 140 °C. The interlayer spacing of LDHs precursor was expanded by succinic acid and lauric acid to 8.838 and 17.519 Å respectively. All the three LDHs products can reduce friction and wear of engine lubricating oil in the tests. LDHs intercalated with lauric acid showed best tribological performance among them which was attributed to sliding each other between laminates, good dispersibility in oil medium and a protective tribofilm formed on the worn surface.

  1. Phosphate-intercalated Ca-Fe-layered double hydroxides: Crystal structure, bonding character, and release kinetics of phosphate

    Science.gov (United States)

    Woo, Myong A.; Woo Kim, Tae; Paek, Mi-Jeong; Ha, Hyung-Wook; Choy, Jin-Ho; Hwang, Seong-Ju

    2011-01-01

    The nitrate-form of Ca-Fe-layered double hydroxide (Ca-Fe-LDH) was synthesized via co-precipitation method, and its phosphate-intercalates were prepared by ion-exchange reaction. According to X-ray diffraction analysis, the Ca-Fe-LDH-NO 3- compound and its H 2PO 4--intercalate showed hexagonal layered structures, whereas the ion-exchange reaction with HPO 42- caused a frustration of the layer ordering of LDH. Fe K-edge X-ray absorption spectroscopy clearly demonstrated that the Ca-Fe-LDH lattice with trivalent iron ions was well-maintained after the ion-exchange with HPO 42- and H 2PO 4-. Under acidic conditions, phosphate ions were slowly released from the Ca-Fe-LDH lattice and the simultaneous release of hydroxide caused the neutralization of acidic media. Fitting analysis based on kinetic models indicated a heterogeneous diffusion process of phosphates and a distinct dependence of release rate on the charge of phosphates. This study strongly suggested that Ca-Fe-LDH is applicable as bifunctional vector for slow release of phosphate fertilizer and for the neutralization of acid soil.

  2. Layered double hydroxides as electrode materials for Ni based batteries and as novel inorganic/organic hybrid materials

    Energy Technology Data Exchange (ETDEWEB)

    Caravaggio, G.

    2002-07-01

    This study examined the electrochemical properties of layered double hydroxides (LDH) in half-cells to determine if they can be used in nickel-cadmium (Ni-Cd) and nickel-metal hydride (NiMH) batteries. The LDHs were prepared by coprecipitation and were characterized by X-ray diffraction analysis. The nickel-aluminium LDHs were found to be the most stable during potassium hydroxide electrolyte discharge because the aluminium acted in a two fold manner. The high charge to radius ratio increased the electrostatic interaction between the anions and the metal layers. The acidity of the hydroxyl groups was due to the high exchange of electrons. The powders had lower discharge capacity compared to commercial electrode materials because of their low density. The nickel-vanadium LDHs exchanged only up to 1.2 electrons and were stable only up to a maximum of 14 days in electrolytic solutions of the cells. Zinc-aluminium LDHs were also synthesized and intercalated with phenyl phosphonic acid or 1,4-phenylene bis phosphonic acid to create microporous materials. X-ray diffraction, infra-red spectroscopy and nuclear magnetic resonance was used to characterize the compounds and determine crystallographic spacing. Grafting of both phosphonates to the metal layers had occurred and both materials showed little or no microporosity.

  3. How the Method of Synthesis Governs the Local and Global Structure of Zinc Aluminum Layered Double Hydroxides

    DEFF Research Database (Denmark)

    Puschparaj, Suraj S. C.; Forano, Claude; Prevot, Vanessa

    2015-01-01

    Seven zinc aluminum layered double hydroxides (ZnAl LDHs), [Zn1-xAlx (OH)2Ax,nH2O] A = NO3-, Cl- or CO32-, prepared by the urea and co-precipitation synthesis methods were investigated to determine how synthesis parameters (pH, metal ion concentration and post synthesis treatment) affect the local...... (atomic) and long (global) range structure of the LDH product. Sample composition, purity, crystal defects and other structural aspects of the LDH products were obtained from powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), Micro-Raman, elemental analysis, and solid state 1H, 27Al...

  4. Line broadening in the PXRD patterns of layered hydroxides: The relative effects of crystallite size and structural disorder

    Indian Academy of Sciences (India)

    Grace S Thomas; P Vishnu Kamath

    2006-01-01

    Layered hydroxides crystallize in a hexagonal structure and incorporate a number of different types of structural disorders as an exigency of anisotropic bonding. Structural disorder contributes to the non-uniform broadening of lines in the powder X-ray diffraction pattern. Common among the disorders are stacking faults, which broaden the ℎ0ℓ/0ℓ reflections. Interstratification selectively broadens the 00ℓ reflections and turbostratic disorder broadens the 0ℓ reflections. The line broadening caused by structural disorder has to be discounted before estimates of particle size are made by applying the Scherrer formula.

  5. Palladium on Layered Double Hydroxide: A Heterogeneous System for the Enol Phosphate Carbon-Oxygen Bond Activation in Aqueous Media

    Directory of Open Access Journals (Sweden)

    Jaqueline D. Senra

    2017-01-01

    Full Text Available In this work, a new catalytic approach for the C-O activation of enol phosphates based on a palladium supported on layered double hydroxide was developed. In this case, two different ketene aminal phosphates were used as models to study the synthesis of α-phenyl enecarbamates N-Boc/CBz under the Suzuki-Miyaura conditions. The use of an ortho-bromoaniline as precursor allowed the synthesis of the 2-phenyl indole through an arylation/Heck cyclization. Catalyst reusability enabled the synthesis of the heterocycle in moderate yields for four consecutive runs.

  6. Dysprosium-containing layered double hydroxides nanoparticles intercalated with biologically active species as an approach for theranostic systems

    KAUST Repository

    Arratia-Quijada, Jenny

    2015-10-23

    A layered double hydroxide structure including dysprosium cations was prepared by co-precipitation. The nanoparticles showed a linear relationship with the reciprocal relaxation spin-lattice (T1) time of water protons which is reflected as contrast in aqueous suspensions analyzed by magnetic resonance imaging. The interlayer space of dysprosium containing LDH was successfully intercalated with folate, ibuprofen and gallate ions, which are key molecules for recognition of some cancer cells and treatment of diseases. The paramagnetic property of the dysprosium-containing LDH detected in this work beside the ability to transport drugs open up the opportunity to design theranostic materials in a single crystal phase with nanometric dimensions.

  7. A new nanostructured material based on fluorophosphate incorporated into a zinc–aluminium layered double hydroxide by ion exchange

    Indian Academy of Sciences (India)

    EL HASSAN ELKHATTABI; MOHAMED LAKRAIMI; MOHA BERRAHO; AHMED LEGROURI; RADOUAN HAMMAL; LAYLA EL GAINI

    2017-08-01

    Layered double hydroxides (LDHs), also called anionic clays, consist of cationic brucite-like layers and exchangeable interlayer anions. These hydrotalcite-like compounds, with Zn and Al in the layers and chloride in the interlayer space, were prepared following the coprecipitation method at constant pH. The effect of pH, aging time and anion concentration on the intercalation of fluorophosphate (PO$_3$F$_2$−, FP) in the [Zn–Al] LDH was investigated. The best crystalline material, with high exchange extent, was obtained by carrying out the exchange at 25◦C in a 0.03 M FP solution at pH 7 with at least 42 h of aging time. A mechanism for the FP intercalation was confirmed by X-ray diffraction, infrared spectroscopy and thermogravimetry (TG) analyses (TG and DTG curves).

  8. Structural and electronic analysis of Li/Al layered double hydroxides and their adsorption for CO2

    Science.gov (United States)

    Hou, Xin-Juan; Li, Huiquan; He, Peng; Sun, Zhenhua; Li, Shaopeng

    2017-09-01

    The most stable structures and electronic properties of different Li/Al layered double hydroxides models (i.e., Li/Al-X, X = F-, Cl-, Br-, OH-, NO3-, CO32-, SO42-) and their hydrates, the adsorption of CO2 on Li/Al-X (X = Cl-, NO3-, CO32-) were ascertained by means of density functional theory. Results revealed that the planes of NO3- and CO32- are parallel with the layers in dehydrated state, although the plane of NO3- becomes vertical with the layers upon the introduction of water molecules. Electronic density analysis suggested that SO42- and CO32- significantly strengthens the reducibility of the Li/Al layered double hydroxides. The distribution of the frontier orbitals indicated the high reactivity of the anions and hydroxyl groups of the layers. The orders of the predicted stability are F- > Cl- > Br- > NO3- for the monovalent anions and SO42- > CO32- for the divalent anions. The calculated adsorption energies of CO2 in Li/Al-X (X = Cl-, NO3-, CO3-) supported the experimental observation that Li/Al-CO3 exhibits higher CO2 capture capacity than Li/Al-NO3 and Li/Al-Cl. Non-covalent interaction analysis indicated that the interactions among mineral surfaces, anions, water and CO2 are dominated by H-bonds, electrostatic interactions, and van der Waals forces. In addition, radial distribution functions were applied to provide insight for the interaction of water or CO2 with carbonate ion and hydroxyl layers.

  9. One-step synthesis of layered yttrium hydroxides in immiscible liquid–liquid systems: Intercalation of sterically-bulky hydrophobic organic anions and doping of europium ions

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Mebae; Fujihara, Shinobu, E-mail: shinobu@applc.keio.ac.jp

    2014-02-15

    Inorganic–organic layered rare-earth compounds were synthesized on the basis of a biphasic liquid–liquid system in one pot. Layered yttrium hydroxides (LYHs) were chosen as a host material for the intercalation of hydrophobic organic guest anions such as benzoate, sebacate, or laurate. In a typical synthesis, an organic phase dissolving carboxylic acid was placed in contact with an equal amount of an aqueous phase dissolving yttrium nitrate n-hydrate and urea. At elevated temperatures up to 80 °C, urea was hydrolyzed to release hydroxyl anions which were used to form yttrium hydroxide layers. LYHs were then precipitated with the intercalation of carboxylate anions delivered from the organic phase under the distribution law. The structure and the morphology of the LYHs could be modulated by the intercalated anions. Doped with Eu{sup 3+} ions, the LYHs exhibited red photoluminescence which was enhanced by the intercalated anions due to the antenna effect. - Graphical abstract: The Eu{sup 3+}-doped layered yttrium hydroxide exhibits intense red photoluminescence after intercalation of benzoate ions. Display Omitted - Highlights: • Immiscible biphasic liquid systems were introduced to synthesize layered yttrium hydroxides. • The temperature of the biphasic systems does not exceed 80 °C in one step of the synthesis. • Hydrophobic organic anions were intercalated between the hydroxide layers in one pot. • Structure and morphology of the hydroxides were modulated by changing the kind of organic anions. • Eu{sup 3+}-doping led to red luminescence from the hydroxides in association with the intercalated organic anions.

  10. Bifunctional sensor of pentachlorophenol and copper ions based on nanostructured hybrid films of humic acid and exfoliated layered double hydroxide via a facile layer-by-layer assembly.

    Science.gov (United States)

    Yuan, Shuang; Peng, Dinghua; Hu, Xianluo; Gong, Jingming

    2013-06-27

    A new, highly sensitive bifunctional electrochemical sensor for the simultaneous determination of pentachlorophenol (PCP) and copper ions (Cu(2+)) has been developed, where organic-inorganic hybrid ultrathin films were fabricated by alternate assembly of humic acid (HA) and exfoliated Mg-Al-layered double hydroxide (LDH) nanosheets onto ITO substrates via a layer-by-layer (LBL) approach. The multilayer films were then characterized by means of UV-vis spectrometry, scanning electron microscopy (SEM), and atomic force microscope (AFM). These films were found to have a relatively smooth surface with almost equal amounts of HA incorporated in each cycle. Its electrochemical performance was systematically investigated. Our results demonstrate that such a newly designed (LDH/HA)n multilayer films, combining the individual properties of HA (dual recognition ability for organic herbicides and metal ions) together with LDH nanosheets (a rigid inorganic matrix), can be applied to the simultaneous analysis of PCP and Cu(II) without interference from each other. The LBL assembled nanoarchitectures were further investigated by X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR), which provides insight for bifunctional sensing behavior. Under the optimized conditions, the detection limit was found to be as low as 0.4 nM PCP, well below the guideline value of PCP in drinking water (3.7 nM) set by the United States Environmental Protection Agency (U.S. EPA), and 2.0 nM Cu(2+), much below the guideline value (2.0 mg L(-1), ~31.2 nM) from the World Health Organization (WHO), respectively. Toward the goal for practical applications, this simple and cost-effective probe was further evaluated by monitoring PCP and Cu(II) in water samples.

  11. Applications vs properties of Mg-Al Layered Double Hydroxides provided by their syntheses methods: alkoxide and alkoxide-free sol-gel syntheses and hydrothermal precipitation

    NARCIS (Netherlands)

    Chubar, N.; Gerda, V.; Megantari, O.; Mičušík, M.; Omastova, M.; Heister, K.; Man, P.; Fraissard, J.

    2013-01-01

    A tremendous number of studies have examined layered double hydroxides (LDH) for their technological applications in the ion exchange removal of toxic ions, recovery of valuable substances, catalysis, CO2 capture, as a layered host for storage/delivery of biologically active molecules, additives to

  12. Applications vs properties of Mg-Al Layered Double Hydroxides provided by their syntheses methods: alkoxide and alkoxide-free sol-gel syntheses and hydrothermal precipitation

    NARCIS (Netherlands)

    Chubar, N.; Gerda, V.; Megantari, O.; Mičušík, M.; Omastova, M.; Heister, K.; Man, P.; Fraissard, J.

    2013-01-01

    A tremendous number of studies have examined layered double hydroxides (LDH) for their technological applications in the ion exchange removal of toxic ions, recovery of valuable substances, catalysis, CO2 capture, as a layered host for storage/delivery of biologically active molecules, additives to

  13. Development of a Highly Biocompatible Antituberculosis Nanodelivery Formulation Based on Para-Aminosalicylic Acid—Zinc Layered Hydroxide Nanocomposites

    Directory of Open Access Journals (Sweden)

    Bullo Saifullah

    2014-01-01

    Full Text Available Tuberculosis is a lethal epidemic, difficult to control disease, claiming thousands of lives every year. We have developed a nanodelivery formulation based on para-aminosalicylic acid (PAS and zinc layered hydroxide using zinc nitrate salt as a precursor. The developed formulation has a fourfold higher efficacy of PAS against mycobacterium tuberculosis with a minimum inhibitory concentration (MIC found to be at 1.40 μg/mL compared to the free drug PAS with a MIC of 5.0 μg/mL. The newly developed formulation was also found active against Gram-positive bacteria, Gram-negative bacteria, and Candida albicans. The formulation was also found to be biocompatible with human normal lung cells MRC-5 and mouse fibroblast cells-3T3. The in vitro release of PAS from the formulation was found to be sustained in a human body simulated phosphate buffer saline (PBS solution at pH values of 7.4 and 4.8. Most importantly the nanocomposite prepared using zinc nitrate salt was advantageous in terms of yield and free from toxic zinc oxide contamination and had higher biocompatibility compared to one prepared using a zinc oxide precursor. In summary, these promising in vitro results are highly encouraging for the continued investigation of para-aminosalicylic acid and zinc layered hydroxide nanocomposites in vivo and eventual preclinical studies.

  14. Synthesis and Physico-Chemical Properties of Zinc Layered Hydroxide-4-Chloro-2-Methylphenoxy Acetic Acid (ZMCPA) Nanocomposite

    Science.gov (United States)

    Salleh, N. M.; Mohsin, SM N.; Sarijo, S. H.; Ghazali, S. A. I. S. M.

    2017-05-01

    Hybrid nanocomposite zinc layered hydroxide-4-chloro-2-methylphenoxyacetic acid (ZMCPA) was successfully synthesized via direct reaction of 4-chloro-2-methylphenoxy acetic acid (MCPA) with zinc oxide (ZnO) under an aqueous environment. The pure phase and well-ordered ZMCPA was obtained when ZMCPA was synthesized at 0.3 M MCPA. The resulting nanocomposite, ZMCPA was characterized by powder X-ray diffraction (PXRD), fourier transform infrared(FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), thermogravimetric and differential thermogravimetric analyses (TGA/DTG) and CHNS Analyzer. Basal spacing showed that the gallery height of zinc layered hydroxide (ZLH) expanded from 11.Å to 24.1 Å, indicating that the MCPA anions were successfully intercalated into the interlayer space of ZLH. The FTIR spectrum of the ZMCPA shows it resembles the spectra of ZnO and MCPA that confirms the intercalation of MCPA between the ZLH sheets. FESEM shows the ZnO precursor has granular structure and transformed into a flake-like structure when the nanohybrid is formed. Percentage loading of MCPA interleaved in the nanohybrid is 50.2%.

  15. Exchange of interlayer terephthalate anions from a Mg Al layered double hydroxide: formation of intermediate interstratified phases

    Science.gov (United States)

    Kaneyoshi, Masami; Jones, William

    1998-10-01

    The exchange of interlayer terephthalate (TA) anions from a Mg-Al layered double hydroxide (LDH) by carbonate, sulfate, chloride and nitrate anions is reported. It is shown that TA is readily exchanged by CO 32- and SO 42- but only partly by Cl - and NO 3-. We demonstrate that during the exchange process interstratified phases are observed. Such interstratification has previously been reported only for directly synthesised materials. The origin of the interstratification is believed to be associated with two preferred orientations of TA anions within the layers, i.e. vertical or horizontal to the clay sheets. Two models for the possible exchange mechanism which is operating in these systems are proposed.

  16. Intercalation assembly of optical hybrid materials based on layered terbium hydroxide hosts and organic sensitizer anions guests

    Institute of Scientific and Technical Information of China (English)

    Liang-Liang Liu; Qin Wang; Dan Xia; Ting-Ting Shen; Ming-Hui Yu; Wei-Sheng Liu; Yu Tang

    2013-01-01

    Optical hybrid materials based on inorganic hosts and organic sensitizer guests hold promise for a virtually unlimited number of applications.In particular,the interaction and the combination of the properties of a defined inorganic matrix and a specific sensitizer could lead to synergistic effects in luminescence enhancing and tuning.The current article focuses on the intercalation assembly of optical hybrid materials based on the layered terbium hydroxide (LTbH) hosts and organic divalent carboxylic sensitizer anion guests by a hydrothermal process.The studies on the interactions between hosts and guests indicate that the type and arrangement of organic guests in the layer spacing of the LTbH hosts can make a difference in the luminescence of the hybrid inorganic-organic materials.

  17. Structure, flame retarding and smoke suppressing properties of Zn-Mg-Al-CO3 layered double hydroxides

    Institute of Scientific and Technical Information of China (English)

    SHI Ling; LI Dianqing; LI Sufeng; WANG Jianrong; Evans D. G.; DUAN Xue

    2005-01-01

    Zn-Mg-Al-CO3 layered double hydroxides (LDHs) have been synthesized by a new method involving separate nucleation and aging steps. The Zn-Mg-Al-CO3 LDHs were characterized by XRD, FT-IR, ICP and TG-DTA. The limiting oxygen index and smoke density of composites of the LDHs with EVA-28 were determined. Incorporation of Zn2+ in the layers of the LDHs was found promoting material charring and smoke suppression. The mechanism of flame retardation and smoke suppression is discussed. The results show that Zn-Mg-Al-CO3 LDHs have better flame retarding and smoke suppressing effects than Mg-Al-CO3 LDHs.

  18. In vitro controlled release of vitamin C from Ca/Al layered double hydroxide drug delivery system.

    Science.gov (United States)

    Gao, Xiaorui; Chen, Le; Xie, Juan; Yin, Yaobing; Chang, Tao; Duan, Yancong; Jiang, Nan

    2014-06-01

    A new drug delivery system for vitamin C (VC), Ca/Al layered double hydroxide (LDH), is demonstrated in this work. VC anions were intercalated successfully in the Ca/Al LDH gallery by a coprecipitation method. The interlayer space of 9.8Å suggests that VC anions are vertical to the LDH layers in the form of interdigitated bilayer. The loading of VC in LDH is 36.4wt.%. The thermal stability of VC is significantly enhanced after intercalation. In vitro VC release results show that the release time of VC in a phosphate buffer at pH7.4 was significantly extended, and the maximal percentage of VC released is 80% of the total. The Avrami-Erofe'ev equation most satisfactorily explains the release kinetics of VC, which is that the release of VC is mainly dominated by the ion-exchange reaction.

  19. Mg-Cu-Al layered double hydroxides based catalysts for the reduction of nitrates in aqueous solutions

    Directory of Open Access Journals (Sweden)

    Vulić Tatjana J.

    2010-01-01

    Full Text Available The secondary waste and bacterial contamination in physico-chemical and biological separation processes used today for nitrate removal from ground water make novel catalytic technologies that convert nitrates to unharmful gaseous nitrogen, very attractive for scientific research. The Mg-Cu-Al layered double hydroxide (LDH based catalysts with different Mg/Al ratio were investigated in water denitrification reaction in the presence of hydrogen and with solely copper as an active phase. Since LDHs have ion exchange properties and their derived mixed oxides possess memory effect (restoration of layered structure after thermal decomposition, their adsorption capacity for nitrates was also measured in the same model system. All studied samples showed nitrate removal from 23% to 62% following the decrease in Al content, as well as the substantial adsorption capacity ranging from 18% to 38%. These results underlie the necessity to take into account the effects of the adsorption in all future investigations.

  20. Structure of oxides prepared by decomposition of layered double Mg–Al and Ni–Al hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Cherepanova, Svetlana V. [Boreskov Institute of Catalysis Siberian branch of Russian Academy of Sciences, pr. Lavrentieva 5, Novosibirsk 630090 (Russian Federation); Novosibirsk State University, Novosibirsk (Russian Federation); Leont’eva, Natalya N., E-mail: n_n_leonteva@list.ru [Institute of hydrocarbons processing Siberian branch of Russian Academy of Sciences, Neftezavodskaya, 54, Omsk 644040 (Russian Federation); Arbuzov, Aleksey B.; Drozdov, Vladimir A. [Institute of hydrocarbons processing Siberian branch of Russian Academy of Sciences, Neftezavodskaya, 54, Omsk 644040 (Russian Federation); Belskaya, Olga B. [Institute of hydrocarbons processing Siberian branch of Russian Academy of Sciences, Neftezavodskaya, 54, Omsk 644040 (Russian Federation); Omsk State Technical University, Omsk (Russian Federation); Antonicheva, Nina V. [Institute of hydrocarbons processing Siberian branch of Russian Academy of Sciences, Neftezavodskaya, 54, Omsk 644040 (Russian Federation)

    2015-05-15

    Abstracts: Thermal decomposition of Mg–Al and Ni–Al layered double hydroxides LDH at temperatures lower than 800 °C leads to the formation of oxides with different structures. Mg–Al oxide has a very defective structure and consists of octahedral layers as in periclase MgO and mixed octahedral–tetrahedral layers as in spinel MgAl{sub 2}O{sub 4}. Mixed Ni–Al oxide has a sandwich-like structure, consisting of a core with Al-doped NiO-like structure and some surface layers with spinel NiAl{sub 2}O{sub 4} structure epitaxial connected with the core. Suggested models were verified by simulation of X-ray diffraction patterns using DIFFaX code, as well as HRTEM, IR-, UV-spectroscopies, and XPS. - Graphical abstract: In the Mg–Al layered double hydroxide Al{sup 3+} ions migrate into interlayers during decomposition. The Mg–Al oxide represents sequence of octahedral and octahedral–tetrahedral spinel layers with vacancies. The Ni–Al oxide has a sandwich-like structure with NiO-like core and surface spinel layers as a result of migration of Al{sup 3+} ions on the surface. The models explain the presence and absence of “memory effect” for the Mg–Al and Ni–Al oxides, respectively. - Highlights: • We study products of Mg(Ni)–Al LDH decomposition by calcination at 500(400)–800 °C. • In Mg–Al/Ni–Al LDH Al ions migrate into interlayers/on the surface during decomposition. • Mg–Al oxide represents sequence of periclase- and spinel-like layers with vacancies. • Ni–Al oxide has a sandwich-like structure with NiO-like core and surface spinel layers. • The models explain the presence/absence of “memory effect” for Mg–Al/Ni–Al oxides.

  1. Variable charge and electrical double layer of mineral-water interfaces: silver halides versus metal (hydr)oxides.

    Science.gov (United States)

    Hiemstra, Tjisse

    2012-11-01

    Classically, silver (Ag) halides have been used to understand thermodynamic principles of the charging process and the corresponding development of the electrical double layer (EDL). A mechanistic approach to the processes on the molecular level has not yet been carried out using advanced surface complexation modeling (SCM) as applied to metal (hydr)oxide interfaces. Ag halides and metal (hydr)oxides behave quite differently in some respect. The location of charge in the interface of Ag halides is not a priori obvious. For AgI(s), SCM indicates the separation of interfacial charge in which the smaller silver ions are apparently farther away from the surface than iodide. This charge separation can be understood from the surface structure of the relevant crystal faces. Charge separation with positive charge above the surface is due to monodentate surface complex formation of Ag(+) ions binding to I sites located at the surface. Negative surface charge is due to the desorption of Ag(+) ions out of the lattice. These processes can be described with the charge distribution (CD) model. The MO/DFT optimized geometry of the complex is used to estimate the value of the CD. SCM reveals the EDL structure of AgI(s), having two Stern layers in series. The inner Stern layer has a very low capacitance (C(1) = 0.15 ± 0.01 F/m(2)) in comparison to that of metal (hydr)oxides, and this can be attributed to the strong orientation of the (primary) water molecules on the local electrostatic field of the Ag(+) and I(-) ions of the surface (relative dielectric constant ε(r) ≈ 6). Depending on the extent of water ordering, mineral surfaces may in principle develop a second Stern layer. The corresponding capacitance (C(2)) will depend on the degree of water ordering that may decrease in the series AgI (C(2) = 0.57 F/m(2)), goethite (C(2) = 0.74 F/m(2)), and rutile (C(2) = ∞), as discussed. The charging principles of AgI minerals iodargyrite and miersite may also be applied to minerals

  2. Corrosion resistance of Zn-Al layered double hydroxide/poly(lactic acid) composite coating on magnesium alloy AZ31

    Science.gov (United States)

    Zeng, Rong-Chang; Li, Xiao-Ting; Liu, Zhen-Guo; Zhang, Fen; Li, Shuo-Qi; Cui, Hong-Zhi

    2015-12-01

    A Zn-Al layered double hydroxide (ZnAl-LDH) coating consisted of uniform hexagonal nano-plates was firstly synthesized by co-precipitation and hydrothermal treatment on the AZ31 alloy, and then a poly(lactic acid) (PLA) coating was sealed on the top layer of the ZnAl-LDH coating using vacuum freeze-drying. The characteristics of the ZnAl-LDH/PLA composite coatings were investigated by means of XRD, SEM, FTIR and EDS. The corrosion resistance of the coatings was assessed by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The results showed that the ZnAl-LDH coating contained a compact inner layer and a porous outer layer, and the PLA coating with a strong adhesion to the porous outer layer can prolong the service life of the ZnAl-LDH coating. The excellent corrosion resistance of this composite coating can be attributable to its barrier function, ion-exchange and self-healing ability.

  3. Synthesis Method and Its Influence Factors of Layered Double Hydroxides%水滑石类材料的合成方法及其影响因素

    Institute of Scientific and Technical Information of China (English)

    朱洪涛; 段宇; 付荔

    2011-01-01

    水滑石类材料是层状阴离子型黏土,具有层间阴离子交换、比表面积大、"记忆功能"等特点。水滑石材料的合成方法主要有共沉淀法、水热合成法、离子交换法、煅烧复原法等。其中即时合成法是合成水滑石材料并同时实现废水处理的一种新思路。原料物质的量比、pH值、反应温度与时间等因素对水滑石类材料的纯度与结晶度具有较大影响。%Layered double hydroxides are layered anion type, with layers of clay between anion exchange, and specific surface area,big, "memory"features. Synthetic Layered double hydroxides include total precipitation,hydrothermal synthesis, ion exchange chromatography, calcining recovery method, etc. Instant synthesis is synthetic Layered double hydroxides and deal with the waste water of a new way of thinking. The mole ratio of raw material, pH value,, reaction temperature and time of some factors such as Layered double hydroxides, the purity of crystallinity and has more influence.

  4. Influence of carbonate intercalation in the surface-charging behavior of Zn-Cr layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, R., E-mail: rrojas@mail.fcq.unc.edu.ar [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Barriga, C. [Departamento de Quimica Inorganica e Ingenieria Quimica, Edificio Marie Curie, Campus de Rabanales, Universidad de Cordoba, 14071 Cordoba (Spain); De Pauli, C.P. [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Avena, M.J. [Departamento de Quimica, Universidad Nacional del Sur, Avenida Alem 1253, 8000 Bahia Blanca (Argentina)

    2010-01-15

    The influence of interlayer composition in the surface charge and reactivity of layered double hydroxides (LDHs) has been explored. With this purpose, a chloride-intercalated Zn-Cr-LDH has been synthesized by the constant pH coprecipitation method and afterwards exchanged with carbonate to obtain solids with different Cl{sup -}/CO{sub 3}{sup 2-} ratios. The solids structure has been characterized by elemental chemical analysis, powder X-ray diffraction and infrared spectroscopy, while its surface-charging behavior and reactivity have been studied by acid-base potentiometric titrations and electrophoretic mobility determinations. The chloride-intercalated sample shows an increasing hydroxyl adsorption with increasing pH and decreasing support electrolyte concentration and the particles present positive electrophoretic mobility in the measured pH range. As carbonate content increases in the samples, the total OH{sup -} uptake diminishes and the samples show an isoelectric point at pH around 10. When the gallery is totally occupied by carbonate anions, the OH uptake vs. pH curves registered at different electrolyte concentrations merge at around pH 10. A LDH-water interface model has been used to give an interpretation to the experimental data. The model indicates that as carbonate content increases, the sample behavior becomes similar to that of a metal (hydr)oxide and that surface (bi)carbonate anions undergo acid-base reactions.

  5. Kinetics of intercalation of fluorescent probes in magnesium-aluminium layered double hydroxide within a multiscale reaction-diffusion framework

    Science.gov (United States)

    Saliba, Daniel; Al-Ghoul, Mazen

    2016-11-01

    We report the synthesis of magnesium-aluminium layered double hydroxide (LDH) using a reaction-diffusion framework (RDF) that exploits the multiscale coupling of molecular diffusion with chemical reactions, nucleation and growth of crystals. In an RDF, the hydroxide anions are allowed to diffuse into an organic gel matrix containing the salt mixture needed for the precipitation of the LDH. The chemical structure and composition of the synthesized magnesium-aluminium LDHs are determined using powder X-ray diffraction (PXRD), thermo-gravimetric analysis, differential scanning calorimetry, solid-state nuclear magnetic resonance (SSNMR), Fourier transform infrared and energy dispersive X-ray spectroscopy. This novel technique also allows the investigation of the mechanism of intercalation of some fluorescent probes, such as the neutral three-dimensional rhodamine B (RhB) and the negatively charged two-dimensional 8-hydroxypyrene-1,3,6-trisulfonic acid (HPTS), using in situ steady-state fluorescence spectroscopy. The incorporation of these organic dyes inside the interlayer region of the LDH is confirmed via fluorescence microscopy, solid-state lifetime, SSNMR and PXRD. The activation energies of intercalation of the corresponding molecules (RhB and HPTS) are computed and exhibit dependence on the geometry of the involved probe (two or three dimensions), the charge of the fluorescent molecule (anionic, cationic or neutral) and the cationic ratio of the corresponding LDH. This article is part of the themed issue 'Multiscale modelling at the physics-chemistry-biology interface'.

  6. A novel and easy chemical-clock synthesis of nanocrystalline iron-cobalt bearing layered double hydroxides.

    Science.gov (United States)

    Hadi, Jebril; Grangeon, Sylvain; Warmont, Fabienne; Seron, Alain; Greneche, Jean-Marc

    2014-11-15

    A novel synthesis of cobalt-iron layered double hydroxide (LDH) with interlayer chlorides was investigated. The method consists in mixing concentrated solutions of hexaamminecobalt(III) trichloride with ferrous chloride at room temperature and in anoxic conditions. Four initial Fe/Co atomic ratios have been tried out (0.12, 0.6, 1.2 and 1.8). Neither heating nor addition of alkali was employed for adjusting the pH and precipitating the metal hydroxides. Still, each mixture led to the spontaneous precipitation of a LDH-rich solid having a crystal-chemistry that depended on the initial solution Fe/Co. These LDHs phases were carefully characterized by mean of X-ray diffraction, (57)Fe Mössbauer spectrometry, transmission electron microscopy and chemical analysis (total dissolution and phenanthroline method). Solution Eh and pH were also monitored during the synthesis. Increasing initial Fe/Co ratio impacted the dynamic of the observed stepwise reaction and the composition of the resulting product. Once the two solutions are mixed, a spontaneous and abrupt color change occurs after an induction time which depends on the starting Fe/Co ratio. This makes the overall process acting as a chemical clock. This spontaneous generation of CoFe-LDH arises from the interplay between redox chemistries of iron and cobalt-ammonium complexes.

  7. Magnesium-containing layered double hydroxides as orthopaedic implant coating materials--An in vitro and in vivo study.

    Science.gov (United States)

    Weizbauer, Andreas; Kieke, Marc; Rahim, Muhammad Imran; Angrisani, Gian Luigi; Willbold, Elmar; Diekmann, Julia; Flörkemeier, Thilo; Windhagen, Henning; Müller, Peter Paul; Behrens, Peter; Budde, Stefan

    2016-04-01

    The total hip arthroplasty is one of the most common artificial joint replacement procedures. Several different surface coatings have been shown to improve implant fixation by facilitating bone ingrowth and consequently enhancing the longevity of uncemented orthopaedic hip prostheses. In the present study, two different layered double hydroxides (LDHs), Mg-Fe- and Mg-Al-LDH, were investigated as potential magnesium (Mg)-containing coating materials for orthopaedic applications in comparison to Mg hydroxide (Mg(OH)2). In vitro direct cell compatibility tests were carried out using the murine fibroblast cell line NIH 3T3 and the mouse osteosarcoma cell line MG 63. The host response of bone tissue was evaluated in in vivo experiments with nine rabbits. Two cylindrical pellets (3 × 3 mm) were implanted into each femoral condyle of the left hind leg. The samples were analyzed histologically and with μ-computed tomography (μ-CT) 6 weeks after surgery. An in vitro cytotoxicity test determined that more cells grew on the LDH pellets than on the Mg(OH)2-pellets. The pH value and the Mg(2+) content of the cell culture media were increased after incubation of the cells on the degradable samples. The in vivo tests demonstrated the formation of fibrous capsules around Mg(OH)2 and Mg-Fe-LDH. In contrast, the host response of the Mg-Al-LDH samples indicated that this Mg-containing biomaterial is a potential candidate for implant coating.

  8. Layered Double Hydroxides as Effective Adsorbents for U(VI and Toxic Heavy Metals Removal from Aqueous Media

    Directory of Open Access Journals (Sweden)

    G. N. Pshinko

    2013-01-01

    Full Text Available Capacities of different synthesized Zn,Al-hydrotalcite-like adsorbents, including the initial carbonate [Zn4Al2(OH12]·CO3·8H2O and its forms intercalated with chelating agents (ethylenediaminetetraacetic acid (EDTA, diethylenetriaminepentaacetic acid (DTPA, and hexamethylenediaminetetraacetic acid (HMDTA and heat-treated form Zn4Al2O7, to adsorb uranium(VI and ions of toxic heavy metals have been compared. Metal sorption capacities of hydrotalcite-like adsorbents have been shown to correlate with the stability of their complexes with the mentioned chelating agents in a solution. The synthesized layered double hydroxides (LDHs containing chelating agents in the interlayer space are rather efficient for sorption purification of aqueous media free from U(VI irrespective of its forms of natural abundance (including water-soluble bi- and tricarbonate forms and from heavy metal ions. [Zn4Al2(OH12]·EDTA·nH2O is recommended for practical application as one of the most efficient and inexpensive synthetic adsorbents designed for recovery of both cationic and particularly important anionic forms of U(VI and other heavy metals from aqueous media. Carbonate forms of LDHs turned out to be most efficient for recovery of Cu(II from aqueous media with pH0≥7 owing to precipitation of Cu(II basic carbonates and Cu(II hydroxides. Chromate ions are efficiently adsorbed from water only by calcinated forms of LDHs.

  9. Hexagonal ZnO porous plates prepared from microwave synthesized layered zinc hydroxide sulphate via thermal decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Machovsky, Michal, E-mail: machovsky@ft.utb.cz [Centre of Polymer Systems, University Institute, Tomas Bata University in Zlin, Nad Ovcirnou 3685, 760 01 Zlin (Czech Republic); Polymer Centre, Faculty of Technology, Tomas Bata University in Zlin, Nam. T.G. Masaryka 275, 762 72 Zlin (Czech Republic); Kuritka, Ivo, E-mail: ivo@kuritka.net [Centre of Polymer Systems, University Institute, Tomas Bata University in Zlin, Nad Ovcirnou 3685, 760 01 Zlin (Czech Republic); Polymer Centre, Faculty of Technology, Tomas Bata University in Zlin, Nam. T.G. Masaryka 275, 762 72 Zlin (Czech Republic); Sedlak, Jakub, E-mail: j1sedlak@ft.utb.cz [Centre of Polymer Systems, University Institute, Tomas Bata University in Zlin, Nad Ovcirnou 3685, 760 01 Zlin (Czech Republic); Polymer Centre, Faculty of Technology, Tomas Bata University in Zlin, Nam. T.G. Masaryka 275, 762 72 Zlin (Czech Republic); Pastorek, Miroslav, E-mail: pastorek@ft.utb.cz [Centre of Polymer Systems, University Institute, Tomas Bata University in Zlin, Nad Ovcirnou 3685, 760 01 Zlin (Czech Republic); Department of Polymer Engineering, Faculty of Technology, Tomas Bata University in Zlin, Nam. T.G. Masaryka 275, 762 72 Zlin (Czech Republic)

    2013-10-15

    Graphical abstract: - Highlights: • Zinc hydroxy sulphate was synthesized in 3 min via microwave hydrothermal route. • Zinc hydroxy sulphate was converted into mesh like porous ZnO by calcining at 900°. • The process of transformation is topotactic. - Abstract: Layered zinc hydroxide sulphate (ZHS) was prepared by microwave-assisted hydrothermal precipitation of zinc sulphate monohydrate with hexamethylenetetramine. Under ambient conditions, the structure of ZHS determined by X-ray diffraction (XRD) was found to be a mixture of zinc hydroxide sulphate pentahydrate Zn{sub 4}SO{sub 4}(OH){sub 6}·5H{sub 2}O and tetrahydrate Zn{sub 4}SO{sub 4}(OH){sub 6}·4H{sub 2}O. Fourier transform infrared (FTIR) spectroscopy was used for characterization of the prepared materials. Based on the interpretation of ZHS's thermal decomposition profile obtained by thermogravimetric analysis, ZnO of high purity was prepared by calcination at 900 °C for 2 h. The structure of the resulting ZnO was confirmed by the XRD. The morphology examination by scanning electron microscopy revealed a porous mesh-like ZnO structure developed from the ZHS precursor at the expense of mass removal due to the release of water and sulphate during the calcination.

  10. Chemical Force Spectroscopy Evidence Supporting the Layer-by-Layer Model of Organic Matter Binding to Iron (oxy)Hydroxide Mineral Surfaces

    KAUST Repository

    Chassé, Alexander W.

    2015-08-18

    © 2015 American Chemical Society. The adsorption of dissolved organic matter (DOM) to metal (oxy)hydroxide mineral surfaces is a critical step for C sequestration in soils. Although equilibrium studies have described some of the factors controlling this process, the molecular-scale description of the adsorption process has been more limited. Chemical force spectroscopy revealed differing adhesion strengths of DOM extracted from three soils and a reference peat soil material to an iron (oxy)hydroxide mineral surface. The DOM was characterized using ultrahigh-resolution negative ion mode electrospray ionization Fourier Transform ion cyclotron resonance mass spectrometry. The results indicate that carboxyl-rich aromatic and N-containing aliphatic molecules of DOM are correlated with high adhesion forces. Increasing molecular mass was shown to decrease the adhesion force between the mineral surface and the DOM. Kendrick mass defect analysis suggests that mechanisms involving two carboxyl groups result in the most stable bond to the mineral surface. We conceptualize these results using a layer-by-layer "onion" model of organic matter stabilization on soil mineral surfaces.

  11. Novel layered pesticide slow/controlled release materials--supramolecular structure and slow release property of glyphosate intercalated layered double hydroxides

    Institute of Scientific and Technical Information of China (English)

    MENG Jinhong; ZHANG Hui; David G. Evans; DUAN Xue

    2005-01-01

    Two different interlayer structured glyphosate (GLY) intercalated MgAl layered double hydroxides, as novel pesticide slow/controlled release materials, have been synthesized by co-precipitation method under various reaction pH values. The slow/controlled release properties have been tested in Na2CO3 aqueous solution. The release mechanism has been interpreted on the basis of the ion-exchange between the guest GLY anions in the lamellar host and in the release media, and the diffusion process of GLY anions in the interstice and interlayer of GLY intercalates, i.e. diffusion through the particles, is the rate-limiting step of GLY release process. The GLY intercalate assembled at lower pH, possessing higher interlayer gallery height and vertical monolayered arrangement of guest anions in the interlayer with larger packing density, exhibits better slow release property than that assembled at higher pH. The results reveal that the layered double hydroxides have potential application in the pesticide slow/controlled release area.

  12. Chemical Force Spectroscopy Evidence Supporting the Layer-by-Layer Model of Organic Matter Binding to Iron (oxy)Hydroxide Mineral Surfaces.

    Science.gov (United States)

    Chassé, Alexander W; Ohno, Tsutomu; Higgins, Steven R; Amirbahman, Aria; Yildirim, Nadir; Parr, Thomas B

    2015-08-18

    The adsorption of dissolved organic matter (DOM) to metal (oxy)hydroxide mineral surfaces is a critical step for C sequestration in soils. Although equilibrium studies have described some of the factors controlling this process, the molecular-scale description of the adsorption process has been more limited. Chemical force spectroscopy revealed differing adhesion strengths of DOM extracted from three soils and a reference peat soil material to an iron (oxy)hydroxide mineral surface. The DOM was characterized using ultrahigh-resolution negative ion mode electrospray ionization Fourier Transform ion cyclotron resonance mass spectrometry. The results indicate that carboxyl-rich aromatic and N-containing aliphatic molecules of DOM are correlated with high adhesion forces. Increasing molecular mass was shown to decrease the adhesion force between the mineral surface and the DOM. Kendrick mass defect analysis suggests that mechanisms involving two carboxyl groups result in the most stable bond to the mineral surface. We conceptualize these results using a layer-by-layer "onion" model of organic matter stabilization on soil mineral surfaces.

  13. Highly biocompatible behaviour and slow degradation of a LDH (layered double hydroxide)-coating on implants in the middle ear of rabbits.

    Science.gov (United States)

    Duda, Franziska; Kieke, Marc; Waltz, Florian; Schweinefuß, Maria E; Badar, Muhammad; Müller, Peter Paul; Esser, Karl-Heinz; Lenarz, Thomas; Behrens, Peter; Prenzler, Nils Kristian

    2015-01-01

    Chronic inflammation can irreversibly damage components of the ossicular chain which may lead to sound conduction deafness. The replacement of impaired ossicles with prostheses does not reduce the risk of bacterial infections which may lead to loss of function of the implant and consequently to additional damage of the connected structures such as inner ear, meninges and brain. Therefore, implants that could do both, reconstruct the sound conduction and in addition provide antibacterial protection are of high interest for ear surgery. Layered double hydroxides (LDHs) are promising novel biomaterials that have previously been used as an antibiotic-releasing implant coating to curb bacterial infections in the middle ear. However, animal studies of LDHs are scarce and there exist only few additional data on the biocompatibility and hardly any on the biodegradation of these compounds. In this study, middle ear prostheses were coated with an LDH compound, using suspensions of nanoparticles of an LDH containing Mg and Al as well as carbonate ions. These coatings were characterized and implanted into the middle ear of healthy rabbits for 10 days. Analysis of the explanted prostheses showed only little signs of degradation. A stable health constitution was observed throughout the whole experiment in every animal. The results show that LDH-based implant coatings are biocompatible and dissolve only slowly in the middle ear. They, therefore, appear as promising materials for the construction of controlled drug delivery vehicles.

  14. A magnetic organic inorganic composite: Synthesis and characterization of magnetic 5-aminosalicylic acid intercalated layered double hydroxides

    Science.gov (United States)

    Zhang, Hui; Zou, Kang; Sun, Hui; Duan, Xue

    2005-11-01

    A core-shell structured magnetic layered organic-inorganic material involving 5-aminosalicylic acid (5-ASA) intercalated Zn-Al layered double hydroxides (LDHs) and magnesium ferrite (MgFe 2O 4) is assembled by a coprecipitation method. The powder X-ray diffraction results show the coexistence of the clear but weak diffractions of MgFe 2O 4 and ordered relatively stronger reflections of 5-ASA intercalated LDHs. The TEM image of magnetic 5-ASA intercalated LDHs reveals that the LDHs layer covers the MgFe 2O 4 particles or their aggregates with particle size of 50-80 nm. The vibration sample magnetization (VSM) measurements exhibit the increase in saturation magnetization of magnetic 5-ASA intercalated LDHs samples with increasing amount of magnetic core. The XPS analyses account for a majority of Zn, Al and O atoms on the surface of magnetic particles. It is suggested that the magnetic core MgFe 2O 4 was coated with LDHs layer probably through Zn-O-Mg and Al-O-Mg linkages, and a core-shell structured model is tentatively proposed.

  15. Luminescent ultrathin film of anionic styrylbiphenyl derivative-layered double hydroxide and its reversible sensing for heavy metal ions.

    Science.gov (United States)

    Yan, Dongpeng; Lu, Jun; Wei, Min; Li, Shuangde; Evans, David G; Duan, Xue

    2012-06-28

    Ordered ultrathin films (UTFs) with blue luminescence based on a styrylbiphenyl derivative (BTBS) and Mg-Al-layered double hydroxide (LDH) nanosheets have been constructed employing the layer-by-layer assembly technique. UV-visible absorption and fluorescence spectroscopy showed a stepwise and regular growth of the films upon increasing the number of deposition cycles. XRD, AFM and SEM indicated that the films possess a periodic layered structure with a period of ca. 1.5 nm, and uniform surface morphology. The film thickness can be precisely controlled in the range ca. 15-53 nm. The BTBS-LDH UTFs exhibit improved UV-light resistance capability compared with the pristine BTBS and show well-defined polarized photoemission, with anisotropy of ca. 0.24. The UTFs show a fast, selective and reversible luminescent response to aqueous solutions containing different heavy metal ions, with the most significant luminescent quenching occurring for the Hg(2+) solution, shedding light on the fact that these films can serve as a new type of selective solid luminescent metal-ion sensor.

  16. Growth and characterization of ternary Ni, Mg–Al and Ni–Al layered double hydroxides thin films deposited by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Birjega, R. [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., Magurele, 76900 Bucharest (Romania); Vlad, A., E-mail: angela.vlad@gmail.com [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., Magurele, 76900 Bucharest (Romania); Matei, A.; Ion, V.; Luculescu, C.; Dinescu, M. [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., Magurele, 76900 Bucharest (Romania); Zavoianu, R. [University of Bucharest, Faculty of Chemistry, Department of Chemical Technology and Catalysis, 4-12 Regina Elisabeta Bd., Bucharest (Romania)

    2016-09-01

    Layered double hydroxides (LDHs) are a class of layered materials consisting of positively charged brucite-like layers and exchangeable interlayer anions. Layered double hydroxides containing a transition metal which undergoes a reversible redox reaction in the useful potential range have been proposed as electrode coating materials due to their properties of charge transport and redox catalysts in basic solutions. Ni–Al,(Ni,Mg)–Al and, as reference, non-electronically conductive Mg–Al double hydroxides thin films were obtained via pulsed laser deposition technique. The thin films were deposited on different substrates (Si, glass) by using a Nd:YAG laser (1064 nm) working at a repetition rate of 10 Hz. X-ray diffraction, Atomic Force Microscopy, Energy Dispersive X-ray spectroscopy, Fourier Transform Infra-Red Spectroscopy, Secondary Ions Mass Spectrometry, Impedance Analyzer and ellipsometry were the techniques used for the as deposited thin films investigation. The optical properties of Ni based LDH thin films and the effect of the Ni amount on the structural, morphological and optical response are evidenced. The optical band gap values, covering a domain between 3.84 eV and 4.38 eV, respond to the Ni overall concentration: the higher Ni amount the lower the band gap value. - Highlights: • Ternary Ni, Mg–Al and Ni–Al layered double hydroxides thin films were deposited. • The effect of the nickel is evidenced. • The possibility to tailor the materials accompanied by an optical response is shown.

  17. Catalytic Combustion of Low Concentration Methane over Catalysts Prepared from Co/Mg-Mn Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Hongfeng Liu

    2014-01-01

    Full Text Available A series of Co/Mg-Mn mixed oxides were synthesized through thermal decomposition of layered double hydroxides (LDHs precursors. The resulted catalysts were then subjected for catalytic combustion of methane. Experimental results revealed that the Co4.5Mg1.5Mn2LDO catalyst possessed the best performance with the T90=485°C. After being analyzed via XRD, BET-BJH, SEM, H2-TPR, and XPS techniques, it was observed that the addition of cobalt had significantly improved the redox ability of the catalysts whilst certain amount of magnesium was essential to guarantee the catalytic activity. The presence of Mg was helpful to enhance the oxygen mobility and, meanwhile, improved the dispersion of Co and Mn oxides, preventing the surface area loss after calcination.

  18. Prolate spheroidal hematite particles equatorially belt with drug-carrying layered double hydroxide disks: Ring Nebula-like nanocomposites

    Directory of Open Access Journals (Sweden)

    Nedim Ay Ahmet

    2011-01-01

    Full Text Available Abstract A new nanocomposite architecture is reported which combines prolate spheroidal hematite nanoparticles with drug-carrying layered double hydroxide [LDH] disks in a single structure. Spindle-shaped hematite nanoparticles with average length of 225 nm and width of 75 nm were obtained by thermal decomposition of hydrothermally synthesized hematite. The particles were first coated with Mg-Al-NO3-LDH shell and then subjected to anion exchange with salicylate ions. The resulting bio-nanohybrid displayed a close structural resemblance to that of the Ring Nebula. Scanning electron microscope and transmission electron microscopy images showed that the LDH disks are stacked around the equatorial part of the ellipsoid extending along the main axis. This geometry possesses great structural tunability as the composition of the LDH and the nature of the interlayer region can be tailored and lead to novel applications in areas ranging from functional materials to medicine by encapsulating various guest molecules.

  19. Synthesis and physical properties of new layered double hydroxides based on ionic liquids: Application to a polylactide matrix

    KAUST Repository

    Livi, Sébastien

    2012-12-01

    Ionic liquids based on tetraalkylphosphonium salts combined with different anions (decanoate and dodecylsulfonate) have been used as intercalating agents of layered double hydroxides (LDHs) by ion exchange. The synthesized phosphonium-treated LDHs display a dramatically improved thermal degradation and a significant increase in the interlayer distance as confirmed by thermogravimetric analysis (TGA) and X-ray Diffraction (XRD), respectively. To highlight the effect of thermostable ionic liquids, a very low amount of LDHs has been introduced within a polylactide (PLA) matrix and PLA/LDHs nanocomposites have been processed in melt by twin-screw extrusion. Then, transmission electron microscopy (TEM) analysis has been used to investigate the influence of ILs on the different morphologies of these nanocomposites. Even though the thermal stability of PLA matrix decreased, an excellent stiffness-toughness compromise has been obtained. © 2012 Elsevier Inc.

  20. Electrochemical synthesis of nickel-iron layered double hydroxide: application as a novel modified electrode in electrocatalytic reduction of metronidazole.

    Science.gov (United States)

    Nejati, Kamellia; Asadpour-Zeynali, Karim

    2014-02-01

    A new and simple approach based on the electrochemical method was used for preparation of reproducible nanostructure thin film of Ni/Fe-layered double hydroxides (Ni/Fe-LDH) on the glassy carbon electrode (GCE). The electrochemical behavior of the Ni/Fe-LDH deposited on GCE electrode is studied. Study of the scanning electron microscopy shows the formation of a nanostructure thin film on the glassy carbon electrode. Electrochemical experiments show that Ni/Fe-LDH modified glassy carbon electrode exhibits excellent electrocatalytic reduction activity with Metronidazole. The method was successfully applied for the analysis of Metronidazole in tablets. The results were favorably compared to those obtained by the reported BP method.

  1. Characterization of photocatalytically active coatings based on TiO2/Zn-Al layered double hydroxide on ceramic tiles

    Directory of Open Access Journals (Sweden)

    Vulić Tatjana J.

    2013-01-01

    Full Text Available The self-cleaning function (photocatalytic activity and surface hydrophilicity/hydrophobicity is of great importance for ceramic tiles from both economic and environmental point of view. This research is focused on the preparation of suitable photocatalytic suspensions studying the influence of the photocatalyst powder amount and the molecular mass of polyethylene glycol (PEG on the self-cleaning properties of the suspensions deposited on the ceramic tile surface. Photocatalysts based on Zn-Al double layered hydroxides with TiO2 as active component, were synthesized and used for the preparation of the suspensions. The coated tiles prepared using smaller photocatalyst amount and the highest investigated molecular mass of PEG (PEG 4000 showed the highest photocatalytic activity in the Rhodamine B degradation reaction, as well as the appropriate surface properties. [Projekat Ministarstva nauke Republike Srbije, br. III45008

  2. Synthesis of Nitrogen-Doped Carbon Nanocoils with Adjustable Morphology using Ni–Fe Layered Double Hydroxides as Catalyst Precursors

    Directory of Open Access Journals (Sweden)

    Tomohiro Iwasaki

    2015-01-01

    Full Text Available Nitrogen-doped carbon nanocoils (CNCs with adjusted morphologies were synthesized in a one-step catalytic chemical vapour deposition (CVD process using acetoni‐ trile as the carbon and nitrogen source. The nickel iron oxide/nickel oxide nanocomposites, which were derived from nickel–iron layered double hydroxide (LDH precur‐ sors, were employed as catalysts for the synthesis of CNCs. In this method, precursor-to-catalyst transformation, catalyst activation, formation of CNCs, and nitrogen doping were all performed in situ in a single process. The morphology (coil diameter, coil pitch, and fibre diameter and nitrogen content of the synthesized CNCs was indi‐ vidually adjusted by modulation of the catalyst composi‐ tion and CVD reaction temperature, respectively. The adjustable ranges of the coil diameter, coil pitch, fibre diameter, and nitrogen content were confirmed to be approximately 500±100 nm, 600±100 nm, 100±20 nm, and 1.1±0.3 atom%, respectively.

  3. Eu-doped Mg-Al layered double hydroxide as a responsive fluorescent material and its interaction with glutamic acid.

    Science.gov (United States)

    Chen, Yufeng; Li, Fei; Yu, Gensheng; Wei, Junchao

    2012-10-01

    The paper describes a study on the fluorescence of a Eu-doped Mg-Al layered double hydroxide (Eu-doped LDH) response to glutamic acid (Glu). Various characterizations (UV-Vis transmittance, TG-DTA and IR-spectrum) indicated that there is an interaction between the Eu-doped LDH and Glu. Fluorescent study was found that the red emissions resulted from (5)D(0)-(7)F(J) transition (J=1, 2) of Eu(3+) markedly decreased, while the blue emission at 440 nm contributed to Glu shifted to low energy after the addition of Glu to the Eu-doped LDH. The fluorescent changes may be relevant to the hydrogen-bond interaction between the Eu-doped LDH and Glu, and the mechanism of the interaction between Eu-doped LDH and Glu was discussed.

  4. Gold Nanoparticles Supported on a Layered Double Hydroxide as Efficient Catalysts for the One-Pot Synthesis of Flavones.

    Science.gov (United States)

    Yatabe, Takafumi; Jin, Xiongjie; Yamaguchi, Kazuya; Mizuno, Noritaka

    2015-11-02

    Flavones are a class of natural products with diverse biological activities and have frequently been synthesized by step-by-step procedures using stoichiometric amounts of reagents. Herein, a catalytic one-pot procedure for the synthesis of flavone and its derivatives is developed. In the presence of gold nanoparticles supported on a Mg-Al layered double hydroxide (Au/LDH), various kinds of flavones can be synthesized starting from 2'-hydroxyacetophenones and benzaldehydes (or benzyl alcohols). The present one-pot procedure consists of a sequence of several reactions, and Au/LDH can catalyze all these different types of reactions. The catalysis is shown to be truly heterogeneous, and Au/LDH can be readily recovered and reused.

  5. Development of a biocompatible nanodelivery system for tuberculosis drugs based on isoniazid-Mg/Al layered double hydroxide.

    Science.gov (United States)

    Saifullah, Bullo; Arulselvan, Palanisamy; El Zowalaty, Mohamed Ezzat; Fakurazi, Sharida; Webster, Thomas J; Geilich, Benjamin M; Hussein, Mohd Zobir

    2014-01-01

    The primary challenge in finding a treatment for tuberculosis (TB) is patient non-compliance to treatment due to long treatment duration, high dosing frequency, and adverse effects of anti-TB drugs. This study reports on the development of a nanodelivery system that intercalates the anti-TB drug isoniazid into Mg/Al layered double hydroxides (LDHs). Isoniazid was found to be released in a sustained manner from the novel nanodelivery system in humans in simulated phosphate buffer solutions at pH 4.8 and pH 7.4. The nanodelivery formulation was highly biocompatible compared to free isoniazid against human normal lung and 3T3 mouse fibroblast cells. The formulation was active against Mycobacterium tuberculosis and gram-positive bacteria and gram-negative bacteria. Thus results show significant promise for the further study of these nanocomposites for the treatment of TB.

  6. Insights into the behaviour of biomolecules on the early Earth: The concentration of aspartate by layered double hydroxide minerals

    Science.gov (United States)

    Grégoire, Brian; Erastova, Valentina; Geatches, Dawn L.; Clark, Stewart J.; Greenwell, H. Christopher; Fraser, Donald G.

    2016-03-01

    The role of mineral surfaces in concentrating and facilitating the polymerisation of simple protobiomolecules during the Hadean and Archean has been the subject of much research in order to constrain the conditions that may have led to the origin of life on early Earth. Here we examine the adsorption of the amino acid aspartate on layered double hydroxide minerals, and use a combined computer simulation - experimental spectroscopy approach to gain insight into the resulting structures of the host-aspartate material. We show that the uptake of aspartate occurs in alkaline solution by anion exchange of the dianion form of aspartate, rather than by surface adsorption. Anion exchange only occurs at values of pH where a significant population of aspartate has the amino group deprotonated, and is then highly efficient up to the mineral anion exchange capacity.

  7. Corrosion Resistance of the Superhydrophobic Mg(OH2/Mg-Al Layered Double Hydroxide Coatings on Magnesium Alloys

    Directory of Open Access Journals (Sweden)

    Fen Zhang

    2016-04-01

    Full Text Available Coatings of the Mg(OH2/Mg-Al layered double hydroxide (LDH composite were formed by a combined co-precipitation method and hydrothermal process on the AZ31 alloy substrate in alkaline condition. Subsequently, a superhydrophobic surface was successfully constructed to modify the composite coatings on the AZ31 alloy substrate using stearic acid. The characteristics of the composite coatings were investigated by means of X-ray diffractometer (XRD, Fourier transform infrared spectroscopy (FTIR, X-ray photoelectron spectroscopy (XPS, scanning electronic microscope (SEM and contact angle (CA. The corrosion resistance of the coatings was assessed by potentiodynamic polarization, the electrochemical impedance spectrum (EIS, the test of hydrogen evolution and the immersion test. The results showed that the superhydrophobic coatings considerably improved the corrosion resistant performance of the LDH coatings on the AZ31 alloy substrate.

  8. Recent Advances in Stimuli-Responsive Photofunctional Materials Based on Accommodation of Chromophore into Layered Double Hydroxide Nanogallery

    Directory of Open Access Journals (Sweden)

    Wu Li

    2013-01-01

    Full Text Available The assembly of photofunctional molecules into host matrices has become an important strategy to achieve tunable fluorescence and to develop intelligent materials. The stimuli-responsive photofunctional materials based on chromophores-assembled layered double hydroxides (LDHs have received much attention from both academic and industry fields as a result of their advantages, such as high photo/thermal stability, easy processing, and well reversibility, which can construct new types of smart luminescent nanomaterials (e.g., ultrathin film and nanocomposite for sensor and switch applications. In this paper, external environmental stimuli have mainly involved physical (such as temperature, pressure, light, and electricity and chemical factors (such as pH and metal ion; recent progress on the LDH-based organic-inorganic stimuli-responsive materials has been summarized. Moreover, perspectives on further development of these materials are also discussed.

  9. Prolate spheroidal hematite particles equatorially belt with drug-carrying layered double hydroxide disks: Ring Nebula-like nanocomposites

    Science.gov (United States)

    Nedim Ay, Ahmet; Konuk, Deniz; Zümreoglu-Karan, Birgul

    2011-12-01

    A new nanocomposite architecture is reported which combines prolate spheroidal hematite nanoparticles with drug-carrying layered double hydroxide [LDH] disks in a single structure. Spindle-shaped hematite nanoparticles with average length of 225 nm and width of 75 nm were obtained by thermal decomposition of hydrothermally synthesized hematite. The particles were first coated with Mg-Al-NO3-LDH shell and then subjected to anion exchange with salicylate ions. The resulting bio-nanohybrid displayed a close structural resemblance to that of the Ring Nebula. Scanning electron microscope and transmission electron microscopy images showed that the LDH disks are stacked around the equatorial part of the ellipsoid extending along the main axis. This geometry possesses great structural tunability as the composition of the LDH and the nature of the interlayer region can be tailored and lead to novel applications in areas ranging from functional materials to medicine by encapsulating various guest molecules.

  10. The preparation of layered double hydroxide wrapped carbon nanotubes and their application as a flame retardant for polypropylene

    Science.gov (United States)

    Du, Baoxian; Fang, Zhengping

    2010-08-01

    Carbon nanotubes (CNTs) wrapped with layered double hydroxide (LDH-w-CNTs) were facilely obtained through in situ introduction of CNTs into the hydrothermal reaction system of LDH, with the goal of combining their unique physical and chemical characteristics to meet new advanced applications. Morphological observations indicated that LDH lamellae enwrapped the surface of CNTs and the wrapping degree was dependent on the functionalization of CNTs. ζ-potential measurements showed that the interaction between the positive charge of LDH and the negative charge of CNTs was the main driving force of the wrapping process. Both hybrids led to a reduction in the peak heat release rate (PHRR) of polypropylene, indicating that they could confer better flame retardancy on polypropylene with respect to LDH and CNTs.

  11. Electrochemical oxidation of 4-chloro phenol over a carbon paste electrode modified with Zn Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez F, D.; Palomar P, M.; Licona S, T. de J.; Romero R, M. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Departamento de Materiales, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D. F. (Mexico); Valente, Jaime S., E-mail: mepp@correo.azc.uam.mx [Instituto Mexicano del Petroleo, Eje Central No. 152, 07730 Mexico D. F. (Mexico)

    2014-07-01

    A study is presented on the electrochemical oxidation of 4-chloro phenol (4cp) in aqueous solution using a bare carbon paste electrode, Cpe, and another one that was modified with Zn Al layered double hydroxides (Cpe/Zn Al-LDH). The electro-oxidation was effected at ph values ranging from 3 up to 11. It was found through cyclic voltammetry that this process was irreversible, namely, there were no reduction peaks, and that depending on the nature of the electrode, the anodic current was limited either by adsorption (Cpe) or diffusion (Cpe/Zn Al-LDH). The energy required and the oxidation reaction rate depended on the ph and on the nature of the electrode, such that the greater rates were obtained when the Cpe/Zn Al-LDH electrode and acid ph were used. The Zn Al-LDH was characterized by means of X-ray diffraction. (Author)

  12. Dysprosium-containing layered double hydroxides nanoparticles intercalated with biologically active species as an approach for theranostic systems

    Energy Technology Data Exchange (ETDEWEB)

    Arratia-Quijada, Jenny [Departamento de Ciencias de la Salud, Centro Universitario Tonalá, Universidad de Guadalajara, Av. Nuevo Periférico No. 555, C.P. 48525, Tonalá, Jalisco (Mexico); Sánchez Jiménez, Cecilia [Departamento de Química, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico); Gurinov, Andrey [Research Resources Center for Magnetic Resonance, St. Petersburg State University, Universitetskiy pr. 26, 198504 St. Petersburg (Russian Federation); NMR Core Lab, King Abdullah University of Science and Technology, Thuwal 23955-6900 (Saudi Arabia); Pérez Centeno, Armando; Ceja Andrade, Israel [Departamento de Física, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico); Carbajal Arízaga, Gregorio Guadalupe, E-mail: gregoriocarbajal@yahoo.com.mx [Departamento de Química, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico)

    2016-01-15

    Graphical abstract: - Highlights: • LDH structure including dysprosium was prepared by co-precipitation. • LDH was capable to produce contrast in the T1 mode of MRI. • LDH were intercalated with folate, ibuprofen and gallate ions. - Abstract: A layered double hydroxide structure including dysprosium cations was prepared by co-precipitation. The nanoparticles showed a linear relationship with the reciprocal relaxation spin-lattice (T1) time of water protons which is reflected as contrast in aqueous suspensions analyzed by magnetic resonance imaging. The interlayer space of dysprosium containing LDH was successfully intercalated with folate, ibuprofen and gallate ions, which are key molecules for recognition of some cancer cells and treatment of diseases. The paramagnetic property of the dysprosium-containing LDH detected in this work beside the ability to transport drugs open up the opportunity to design theranostic materials in a single crystal phase with nanometric dimensions.

  13. Surfactant-modified flowerlike layered double hydroxide-coated magnetic nanoparticles for preconcentration of phthalate esters from environmental water samples.

    Science.gov (United States)

    Zhao, Xiaoli; Liu, Shuangliu; Wang, Peifang; Tang, Zhi; Niu, Hongyun; Cai, Yaqi; Wu, Fengchang; Wang, Hao; Meng, Wei; Giesy, John P

    2015-10-02

    A novel type of layered, flowerlike magnetic double hydroxide (MLDH) nanoparticles modified by surfactants has been successfully synthesized and was applied as an effective sorbent for pre-concentration of several phthalate ester pollutants (PAEs) from water prior to quantification. The MLDH was obtained via a simple ultrasound-assisted method by using silica coated Fe3O4 as the core and anisotropic Mg-Al layered double hydroxide (Mg-Al LDH) nanocrystals as the shell to which analytes were absorbed. Orientation and dimensionality hierarchical structure as well as the large expandable interlayer free space and positive charge of the Mg-Al LDH shell make it easier to form anionic surfactant micelles on its surface via self-assembly. Due to its high adsorption area, compared with non-mesoporous nano solid-phase extraction agents, mesoporous channel shell and reduction diffusion path, MLDH exhibited high extraction efficiency of organic target residues. Under optimized conditions, with a total of 30mg of adsorbant added to from samples containing 400mL water from the environment recoveries of DPP, DBP, DCP and DOP were consistent with ranges of 69-101%, 79-101%, 86-102% and 63-100%, respectively. Standard deviations of recoveries ranged from 1 to 7%, respectively and the method was sensitive with limits of detection of 12.3, 18.7, 36.5 and 15.6ngL(-1). To the best of our knowledge, this is the first report of use of surfactant-modified MLDH nanoparticles and its application as adsorbent to pre-concentration of PAEs from environmental water samples prior to instrumental analyses.

  14. Enhanced Hydrogen Generation Properties of MgH2-Based Hydrides by Breaking the Magnesium Hydroxide Passivation Layer

    Directory of Open Access Journals (Sweden)

    Liuzhang Ouyang

    2015-05-01

    Full Text Available Due to its relatively low cost, high hydrogen yield, and environmentally friendly hydrolysis byproducts, magnesium hydride (MgH2 appears to be an attractive candidate for hydrogen generation. However, the hydrolysis reaction of MgH2 is rapidly inhibited by the formation of a magnesium hydroxide passivation layer. To improve the hydrolysis properties of MgH2-based hydrides we investigated three different approaches: ball milling, synthesis of MgH2-based composites, and tuning of the solution composition. We demonstrate that the formation of a composite system, such as the MgH2/LaH3 composite, through ball milling and in situ synthesis, can improve the hydrolysis properties of MgH2 in pure water. Furthermore, the addition of Ni to the MgH2/LaH3 composite resulted in the synthesis of LaH3/MgH2/Ni composites. The LaH3/MgH2/Ni composites exhibited a higher hydrolysis rate—120 mL/(g·min of H2 in the first 5 min—than the MgH2/LaH3 composite— 95 mL/(g·min—without the formation of the magnesium hydroxide passivation layer. Moreover, the yield rate was controlled by manipulation of the particle size via ball milling. The hydrolysis of MgH2 was also improved by optimizing the solution. The MgH2 produced 1711.2 mL/g of H2 in 10 min at 298 K in the 27.1% ammonium chloride solution, and the hydrolytic conversion rate reached the value of 99.5%.

  15. Enhancement of photocatalytic degradation of dimethyl phthalate with nano-TiO{sub 2} immobilized onto hydrophobic layered double hydroxides: A mechanism study

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Zhujian [College of Environmental Science and Engineering, South China University of Technology, Guangzhou 510006 (China); The Key Lab of Pollution Control and Ecosystem Restoration in Industry Clusters, Ministry of Education, Guangzhou 510006 (China); Wu, Pingxiao, E-mail: pppxwu@scut.edu.cn [College of Environmental Science and Engineering, South China University of Technology, Guangzhou 510006 (China); The Key Lab of Pollution Control and Ecosystem Restoration in Industry Clusters, Ministry of Education, Guangzhou 510006 (China); The Key Laboratory of Environmental Protection and Eco-Remediation of Guangdong Regular Higher Education Institutions (China); Lu, Yonghong; Wang, Xiaorong; Zhu, Nengwu [College of Environmental Science and Engineering, South China University of Technology, Guangzhou 510006 (China); The Key Lab of Pollution Control and Ecosystem Restoration in Industry Clusters, Ministry of Education, Guangzhou 510006 (China); Dang, Zhi [College of Environmental Science and Engineering, South China University of Technology, Guangzhou 510006 (China); The Key Lab of Pollution Control and Ecosystem Restoration in Industry Clusters, Ministry of Education, Guangzhou 510006 (China); The Key Laboratory of Environmental Protection and Eco-Remediation of Guangdong Regular Higher Education Institutions (China)

    2013-02-15

    Highlights: ► The reconstructed organic LDHs are consisted of the interconnecting nano-flakes. ► It is confirmed that organic LDHs/TiO{sub 2} composites are combined together by chemical bonds. ► The organic LDHs with flaky structure effectively enrich DPM onto the composite. ► The abundant external hydroxyl groups of organic LDHs promote the production of ·OH. ► TiO{sub 2} immobilized onto organic LDHs greatly enhances the photodegradation of DMP. -- Abstract: The organic layered double hydroxides (LHDs)/TiO{sub 2} composites with various mass ratios were prepared by the reconstruction of mixed metal oxides to photodegrade dimethyl phthalate (DMP). The physicochemical properties of the obtained products were analyzed by X-ray diffraction (XRD) spectra, X-ray photoelectron spectra (XPS), UV–vis diffuse reflectance spectroscope and scanning electron microscope (SEM). The results showed that the TiO{sub 2} particles and the organic LDHs were combined together through chemical bonds, and TiO{sub 2} particles were well distributed on the surface of the interconnecting organic LDHs nano-flakes. According to the experimental results of adsorptive and photodegradation of DMP, the organic LDHs with flaky structure could effectively adsorb the DMP molecules and the adsorption isotherm by the composites modeled well with the Langmuir equation. The enrichment of DMP onto the composites and the external hydroxyl groups of the composites produce a synergistic effect leading to greatly enhance the rate of DMP photocatalytic degradation by the obtained composites.

  16. Removal of Naphthol Green B from Aqueous Solution by Calcined Layered Double Hydroxides:Adsorption Property and Mechanism Studies

    Institute of Scientific and Technical Information of China (English)

    ZHANG Feng; NI Zheming; XIA Shengjie; LIU Xiaoming; WANG Qiaoqiao

    2009-01-01

    The adsorption of naphthol green B(NGB)by Mg/Al-LDO(layered double oxides)with a Mg/Al molar ratio of librium is 193.4 mg and the percentage of absorption is 96.7%,with an adsorbent dose of 1.0 g/L under the following condition:200 mg/L NGB concentration,temperature 298 K,pH 10.0 and an equilibrium time of 80 min.Langmuir and Freundlich adsorption models were used for fitting the isotherms,and the thermodynamic parameters have been calculated,which showed that the adsorption process was spon 'taneous and exothermic in nature.In the light of so called "memory effect",the Mg/Al-LDO was found to recover their original layered structure after adsorption,and part of NGB ions intercalated into the interlayer of LDH(layered double hydroxides),which has been supported by XRD and FTIR.In addition,the competitive anions for adsorption and the regeneration of Mg/AI-LDO have also been investigated.

  17. A combined study based on experiment and molecular dynamics: perylene tetracarboxylate intercalated in a layered double hydroxide matrix.

    Science.gov (United States)

    Yan, Dongpeng; Lu, Jun; Wei, Min; Ma, Jing; Evans, David G; Duan, Xue

    2009-10-28

    This paper describes a combined experimental and theoretical simulation investigation on the photophysical properties, thermolysis, and orientation of 3,4,9,10-perylene tetracarboxylate (PTCB) intercalated Mg-Al-layered double hydroxide (PTCB/Mg-Al-LDH). UV-vis absorption and fluorescence spectroscopy show the existence of PTCB aggregates within the gallery of LDH, indicative of H-type (blue-shifted absorption band) and J-type dimers (red-shifted absorption band). In situ high-temperature X-ray diffraction (HT-XRD), thermogravimetry and differential thermal analysis (TG-DTA) and elemental analysis were used to study the thermal decomposition properties of PTCB/Mg-Al-LDH, and it was found that the decomposition temperature of the intercalated PTCB is lower than its pristine form (460 vs 565 degrees C), indicating that the strong pi-pi interaction among PTCB was weakened by the positively charged LDH host layers. Molecular dynamics (MD) calculations were employed to simulate the molecular arrangement and aggregation behavior of intercalated PTCB in the gallery of Mg-Al-LDH. The simulation results show that the intercalated PTCB anions exhibit a tendency from tilted to vertical orientation with respect to the layers as the interlayer water content increases, furthermore, the H and J-type dimer species are most likely populated under low and high hydration conditions, respectively. Moreover, the distribution of interlayer water molecules are also discussed.

  18. A combined FTIR and infrared emission spectroscopy investigation of layered double hydroxide as an effective electron donor

    Science.gov (United States)

    Zhang, Jia; Wei, Feng; Liang, Ying; Zhou, Jizhi; Xi, Yunfei; Qian, Guangren; Frost, Ray

    2016-02-01

    A novel method has been presented to characterize electron transfer in layered double hydroxides (LDHs) utilizing an investigation combing FTIR and infrared emission spectroscopy. At room temperature, electron could transfer to interlayer Fe3 + through monodentate ligand cyanide, and resulted in a reduction of 40% Fe3 + to Fe2 +. When the environmental temperature increased from 25 to 300 °C, reduction of Fe3 + and Ni2 + increased to 94% and 42%. Furthermore, electron also transferred to interlayer cation through multidentate ligand EDTA. As a result, LDHs has been proven to be an effective electron donor, and FTIR was a feasible tool in characterizing this property by monitoring the valence state of cations. It was also concluded that octahedral units with OH- groups in LDH layer functioned as electron donor centers. Driving force for electron transfer is attributed to the charge density difference between cation layer and probe anion. These results could help to explain the mechanism of various applications of LDHs in catalysis and photocatalysis.

  19. Preparation and characterization of an anti-inflammatory agent based on a zinc-layered hydroxide-salicylate nanohybrid and its effect on viability of Vero-3 cells

    Directory of Open Access Journals (Sweden)

    Ramli M

    2013-01-01

    Full Text Available Munirah Ramli,1,2 Mohd Zobir Hussein,1,3 Khatijah Yusoff41Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, Universiti Putra Malaysia, Serdang, Selangor, 2Department of Industrial Biotechnology, Faculty of Biosciences and Bioengineering, Universiti Teknologi Malaysia, Skudai, Johor, 3Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, Serdang, Selangor, 4Department of Microbiology, Faculty of Biotechnology and Biomolecular Sciences, Universiti Putra Malaysia, Serdang, Selangor, MalaysiaAbstract: A new organic-inorganic nanohybrid based on zinc-layered hydroxide intercalated with an anti-inflammatory agent was synthesized through direct reaction of salicylic acid at various concentrations with commercially available zinc oxide. The basal spacing of the pure phase nanohybrid was 15.73 Å, with the salicylate anions arranged in a monolayer form and an angle of 57 degrees between the zinc-layered hydroxide interlayers. Fourier transform infrared study further confirmed intercalation of salicylate into the interlayers of zinc-layered hydroxide. The loading of salicylate in the nanohybrid was estimated to be around 29.66%, and the nanohybrid exhibited the properties of a mesoporous-type material, with greatly enhanced thermal stability of the salicylate compared with its free counterpart. In vitro cytotoxicity assay revealed that free salicylic acid, pure zinc oxide, and the nanohybrid have a mild effect on viability of African green monkey kidney (Vero-3 cells.Keywords: anti-inflammatory, salicylic acid, zinc-layered hydroxide, zinc oxide, nanohybrid, cytotoxicity

  20. Kinetic analysis of anionic surfactant adsorption from aqueous solution onto activated carbon and layered double hydroxide with the zero length column method

    NARCIS (Netherlands)

    Schouten, Natasja; Ham, Louis G.J. van der; Euverink, Gert-Jan W.; Haan, André B. de

    2009-01-01

    Low cost adsorption technology offers high potential to clean-up laundry rinsing water. From an earlier selection of adsorbents, layered double hydroxide (LDH) and granular activated carbon (GAC) proved to be interesting materials for the removal of anionic surfactant, linear alkyl benzene sulfonate

  1. Nanohybrids of Mg/Al layered double hydroxide and long-chain (C18) unsaturated fatty acid anions: Structure and sorptive properties

    Science.gov (United States)

    Long-chain (C18) unsaturated fatty acid anions, elaidate (ELA), oleate (OLE), linoleate (LINO), and linolenate (LINOLEN), were intercalated into Mg/Al (3:1) layered double hydroxide (LDH) and the resultant organo-LDH nanohybrid materials were characterized and subsequently evaluated as sorbents of s...

  2. A unique growth mechanism of donut-shaped Mg–Al layered double hydroxides crystals revealed by AFM and STEM–EDX

    NARCIS (Netherlands)

    Budhysutanto, W.N.; Van Den Bruele, F.J.; Rossenaar, B.D.; Van Agterveld, D.; Van Enckevort, W.J.P.; Kramer, H.J.M.

    2010-01-01

    Donut-like crystals of Mg–Al layered double hydroxides (LDH) are synthesized using a hydrothermal method with microwave heating. This morphology provides enlargement of the specific surface area of the {h k 0} faces, needed for adsorption application. The growth mechanism for donut-shaped crystals i

  3. Photocatalytic organic transformation by layered double hydroxides: highly efficient and selective oxidation of primary aromatic amines to their imines under ambient aerobic conditions.

    Science.gov (United States)

    Yang, Xiu-Jie; Chen, Bin; Li, Xu-Bing; Zheng, Li-Qiang; Wu, Li-Zhu; Tung, Chen-Ho

    2014-06-25

    We report the first application of layered double hydroxide as a photocatalyst in the transformation of primary aromatic amines to their corresponding imines with high efficiency and selectivity by using oxygen in an air atmosphere as a terminal oxidant under light irradiation.

  4. A novel injectable thermoresponsive and cytocompatible gel of poly(N-isopropylacrylamide) with layered double hydroxides facilitates siRNA delivery into chondrocytes in 3D culture

    NARCIS (Netherlands)

    Yang, Hsiao-yin; van Ee, Renz J; Timmer, Klaas; Craenmehr, Eric G M; Huang, Julie H; Oner, F. Cumhur; Dhert, Wouter J A; Kragten, Angela H M; Willems, Nicole; Grinwis, Guy C M; Tryfonidou, Marianna A; Papen-Botterhuis, Nicole E; Creemers, Laura B

    2015-01-01

    Hybrid hydrogels composed of poly(N-isopropylacrylamide) (pNIPAAM) and layered double hydroxides (LDHs) are presented in this study as novel injectable and thermoresponsive materials for siRNA delivery, which could specifically target several negative regulators of tissue homeostasis in cartilaginou

  5. In situ oligomerization of 2-(thiophen-3-yl)acetate intercalated into Zn{sub 2}Al layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Tronto, Jairo, E-mail: jairotronto@ufv.br [Universidade Federal de Viçosa, Instituto de Ciências Exatas e Tecnológicas, Campus de Rio Parsanaíba, Rodovia BR 354 km 310, Cx. Postal 22, CEP, 38.810-000 Rio Paranaíba, MG (Brazil); Pinto, Frederico G.; Costa, Liovando M. da [Universidade Federal de Viçosa, Instituto de Ciências Exatas e Tecnológicas, Campus de Rio Parsanaíba, Rodovia BR 354 km 310, Cx. Postal 22, CEP, 38.810-000 Rio Paranaíba, MG (Brazil); Leroux, Fabrice; Dubois, Marc [Clermont Université, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, BP 10448, F-63000 Clermont-Ferrand (France); CNRS, UMR 6296, ICCF, BP 80026, F-6317 Clermont-Ferrand (France); Valim, João B. [Universidade de São Paulo, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Departamento de Química, Av. dos Bandeirantes 3900, CEP 14.040-901, Ribeirão Preto, SP (Brazil)

    2015-01-15

    A layered double hydroxide (LDH) with cation composition Zn{sub 2}Al was intercalated with 2-(thiophen-3-yl)acetate (3-TA) monomers. To achieve in situ polymerization and/or oligomerization of the intercalated monomers, soft thermal treatments were carried out, and subsequent hybrid LDH materials were analyzed by means of several characterization techniques using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), {sup 13}C CP–MAS nuclear magnetic resonance (NMR), electron spin resonance (EPR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), inductively coupled plasma optical emission spectroscopy (ICP–OES), and elemental analysis. PXRD analysis suggested that the intercalated monomers formed a bilayer. Thermal treatment of the hybrid LDH assembly above 120 °C provokes partially the breakdown of the layered structure, generating the phase zincite. EPR results indicated that vicinal monomers (oligomerization) were bound to each other after hydrothermal or thermal treatment, leading to a polaron response characteristic of electron conductivity localized on a restricted number of thiophene-based monomer segments. Localized unpaired electrons exist in the material and interact with the {sup 27}Al nuclei of the LDH layers by superhyperfine coupling. These unpaired electrons also interact with the surface of ZnO (O{sup 2−} vacancies), formed during the thermal treatments. - Graphical abstract: We synthesized a layered double hydroxide (LDH) with cation composition Zn{sub 2}Al, intercalated with 2-(thiophen-3-yl)acetate (3-TA) monomers, by coprecipitation at constant pH. We thermally treated the material, to achieve in situ polymerization and/or oligomerization of the intercalated monomers. - Highlights: • A Zn{sub 2}Al–LDH was intercalated with 2-(thiophen-3-yl)acetate monomers. • To achieve in situ oligomerization of the monomers, thermal treatments were made.

  6. Synthesis of layered double hydroxides containing Mg2+, Zn2+, Ca2+ and Al3+ layer cations by co-precipitation methods-A review

    Science.gov (United States)

    Theiss, Frederick L.; Ayoko, Godwin A.; Frost, Ray L.

    2016-10-01

    Co-precipitation is a common method for the preparation of layered double hydroxides (LDHs) and related materials. This review article is aimed at providing newcomers to the field with some examples of the types of co-precipitation reactions that have been reported previously and to briefly investigate some of the properties of the products of these reactions. Due to the sheer volume of literature on the subject, the authors have had to limit this article to the synthesis of Mg/Al, Zn/Al and Ca/Al LDHs by co-precipitation and directly related methods. LDHs have been synthesised from various reagents including metal salts, oxides and hydroxides. Co-precipitation is also useful for the direct synthesis of LDHs with a wide range of interlayer anions and various bases have been successfully employed to prepare LDHs. Examples of other synthesis techniques including the urea method, hydrothermal synthesis and various mechanochemical methods that are undoubtedly related to co-precipitation have also been included in this review. The effect of post synthesis hydrothermal has also been summarised.

  7. A new route to prepare nanocomposites based on polyvinyl chloride and MgAl layered double hydroxide intercalated with laurylether phosphate

    Directory of Open Access Journals (Sweden)

    2009-09-01

    Full Text Available The MgAl layered double hydroxide (LDH with laurylether phosphate was prepared using reconstruction method. Delamilation of the LDH with laurylether phosphate (LDH-PK in tetrahydrofuran was characterized by AFM (atomic force microscopy, indicating that a large part of the LDH was delaminated into single, double and multi layers. The delaminated LDH-PK suspension was then used with polyvinyl chloride (PVC to prepare a series of high-LDH-loading nanocomposites. Both the XRD (X-ray diffraction patterns and TEM (transmission electron microscopy photographs of the as-prepared PVC/LDH nanocomposites indicated that the LDH nanolayers dispersed uniformly in the PVC matrix. With differential scanning calorimetry (DSC the glass transition temperatures of PVC phases in the PVC/LDH nanocomposites were measured and a slightly lower value than that of pristine PVC has been observed. Thermogravimetric analysis results show that the presence of LDH enhanced the dehydrochlorination temperature (Tmax1, reduced the maximum degradation rate (Rmax1 and the 5% weight loss temperature, and promoted the char formation of PVC. However, the thermal degradation temperature (Tmax2 and thermal degradation rate (Rmax2 of the dehydrochlorinated PVC were slightly affected by the presence of LDH. The apparent activation energies were calculated by the method of Flynn-Wall-Ozawa in nitrogen at four different heating rates, showing that the nanofiller increased the apparent activation energies by 10–26 kJ/mol when compared with pristine PVC, probably implying that the LDH nanolayers improve the stability of chlorine atom on the PVC chains.

  8. Formation of crystalline Zn-Al layered double hydroxide precipitates on γ-alumina: the role of mineral dissolution.

    Science.gov (United States)

    Li, Wei; Livi, Kenneth J T; Xu, Wenqian; Siebecker, Matthew G; Wang, Yujun; Phillips, Brian L; Sparks, Donald L

    2012-11-06

    To better understand the sequestration of toxic metals such as nickel (Ni), zinc (Zn), and cobalt (Co) as layered double hydroxide (LDH) phases in soils, we systematically examined the presence of Al and the role of mineral dissolution during Zn sorption/precipitation on γ-Al(2)O(3) (γ-alumina) at pH 7.5 using extended X-ray absorption fine structure spectroscopy (EXAFS), high-resolution transmission electron microscopy (HR-TEM), synchrotron-radiation powder X-ray diffraction (SR-XRD), and (27)Al solid-state NMR. The EXAFS analysis indicates the formation of Zn-Al LDH precipitates at Zn concentration ≥0.4 mM, and both HR-TEM and SR-XRD reveal that these precipitates are crystalline. These precipitates yield a small shoulder at δ(Al-27) = +12.5 ppm in the (27)Al solid-state NMR spectra, consistent with the mixed octahedral Al/Zn chemical environment in typical Zn-Al LDHs. The NMR analysis provides direct evidence for the existence of Al in the precipitates and the migration from the dissolution of γ-alumina substrate. To further address this issue, we compared the Zn sorption mechanism on a series of Al (hydr)oxides with similar chemical composition but differing dissolubility using EXAFS and TEM. These results suggest that, under the same experimental conditions, Zn-Al LDH precipitates formed on γ-alumina and corundum but not on less soluble minerals such as bayerite, boehmite, and gibbsite, which point outs that substrate mineral surface dissolution plays an important role in the formation of Zn-Al LDH precipitates.

  9. Improving the endoscopic endonasal transclival approach: the importance of a precise layer by layer reconstruction.

    Science.gov (United States)

    Iacoangeli, Maurizio; Di Rienzo, Alessandro; di Somma, Lucia Giovanna Maria; Moriconi, Elisa; Alvaro, Lorenzo; Re, Massimo; Salvinelli, Fabrizio; Carassiti, Massimiliano; Scerrati, Massimo

    2014-04-01

    BACKGROUND. The endoscopic endonasal transclival approach (EETCA) is a minimally-invasive technique allowing a direct route to the base of implant of clival lesions with reduced brain and neurovascular manipulation. On the other hand, it is associated with potentially severe complications related to the difficulties in reconstructing large skull base defects with a high risk of postoperative cerebrospinal fluid (CSF) leakage. The aim of this paper is to describe a precise layer by layer reconstruction in the EETCA including the suture of the mucosa as an additional reinforcing layer between cranial and nasal cavity in order to speed up the healing process and reduce the incidence of CSF leak. METHODS. This closure technique was applied to the last six cases of EETCA used for clival meningiomas (2), clival chordomas (2), clival metastasis (1), and craniopharyngioma with clival extension (1). RESULTS. After a mean follow-up of 6 months we had no one case of postoperative CSF leakage or infections. Seriated outpatient endoscopic endonasal controls showed a fast healing process of nasopharyngeal mucosa with less patient discomfort. CONCLUSIONS. Our preliminary experience confirms the importance of a precise reconstruction of all anatomical layers violated during the surgical approach, including the nasopharygeal mucosa.

  10. Layered double hydroxides as fillers in poly(l-lactide nanocomposites, obtained by in situ bulk polymerization

    Directory of Open Access Journals (Sweden)

    Telma Nogueira

    2016-01-01

    Full Text Available Abstract In this study in situ bulk polymerization of L-lactide filled with layered double hydroxides (LDH was investigated. Four different LDHs intercalated with two different organic anions (salicylate and sebacate were synthesized and characterized. After characterization, these synthetic layered compounds were used as fillers in poly(L-lactide (PLLA nanocomposites with two different fillers’s loadings (1 wt% and 2 wt%. PLLA and PLLA nanocomposites were evaluated by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, ultraviolet and visible spectroscopy, thermogravimetric analysis (TGA, dynamical mechanical analysis (DMA, flexural testing and differential scanning calorimetry (DSC. The results demonstrated that, compared to PLLA, the nanocomposite containing 1 wt% of Zn/Al salicylate transmitted less UVA and UVB light, while keeping a similar transparency in the visible region. Thermogravimetric analysis revealed that the nanocomposite with 1 wt% of Zn/Al salicylate exhibited the highest thermal stability. In general the flexural and dynamical mechanical properties were reduced in compassion to neat PLLA. DSC results, demonstrated that, compared to PLLA, all the nanocomposites exhibited lower glass transition temperature and melting temperature values.

  11. A new route for local probing of inner interactions within a layered double hydroxide/benzene derivative hybrid material.

    Science.gov (United States)

    Fleutot, S; Dupin, J C; Baraille, I; Forano, C; Renaudin, G; Leroux, F; Gonbeau, D; Martinez, H

    2009-05-14

    This paper presents the preparation and characterization of hybrid hydrotalcite-type layered double hydroxides (Zn1-xAlx(OH)2HBSx.nH2O, with x=0.33) where HBS is the 4-phenol sulfonate, with a detailed analysis of the grafting process of this organic entity onto the host lattice. As a set of the usual techniques (XRD, TG-DT/MS, FTIR and 27Al MAS NMR) was used to characterize the hybrid materials, this work focuses on a joint study by X-ray photoelectron spectroscopy and some quantum-calculation modeling in order to highlight the nature of the interactions between the organic and the mineral sub-systems. For the as-prepared hybrid material, the main results lead to a quasi-vertical orientation of the organic molecules within the mineral sheets via H-bond stabilization. By heating the hybrid material up to 200 degrees C, the structure shrinks with the condensation of the organics; the different theoretical modeling done gives an energy-stable situation when a direct attachment of the HBS sulfonate group sets up with the mineral layers, in agreement with the recorded XPS experimental data.

  12. Sorption mechanisms of arsenate on Mg-Fe layered double hydroxides: A combination of adsorption modeling and solid state analysis.

    Science.gov (United States)

    Hudcová, Barbora; Veselská, Veronika; Filip, Jan; Číhalová, Sylva; Komárek, Michael

    2017-02-01

    Layered double hydroxides have been proposed as effective sorbents for As(V), but studies investigating adsorption mechanisms usually lack a comprehensive mechanistic/modeling approach. In this work, we propose coupling surface complexation modeling with various spectroscopic techniques. To this end, a series of batch experiments at different pH values were performed. Kinetic data were well fitted by a pseudo-second order kinetic model, and the equilibrium data were fitted by the Freundlich model. Moreover, the pH-dependent As(V) sorption data were satisfactorily fitted by a diffuse layer model, which described the formation of >SOAsO3H(-) monodentate and >(SO)2AsO2(-) bidentate inner-sphere complexes (">S" represents a crystallographically-bound group on the surface). Additionally, XPS analyses confirmed the adsorption mechanisms. The sorption mechanisms were affected by anion exchange, which was responsible for the formation of outer sphere complexes, as identified by XRD and FTIR analyses. Furthermore, a homogenous distribution of As(V) was determined by HR-TEM with elemental mapping. Using low-temperature Mössbauer spectroscopy on isotope (57)Fe, a slight shift of the hyperfine parameters towards higher values following As(V) sorption was measured, indicating a higher degree of structural disorder. In general, mechanistic adsorption modeling coupled with solid state analyses presents a powerful approach for investigating the adsorption mechanism of As(V) on Mg-Fe LDH or other sorbents.

  13. High performance NiFe layered double hydroxide for methyl orange dye and Cr(VI) adsorption.

    Science.gov (United States)

    Lu, Yi; Jiang, Bin; Fang, Liang; Ling, Faling; Gao, Jiemei; Wu, Fang; Zhang, Xihua

    2016-06-01

    The NiFe layered double hydroxides (LDHs) with different mole ratio of Ni/Fe (4:1, 3:1, 7:3 and 1:1) were prepared by a simple coprecipitation method. The adsorption performance were evaluated by the removal of methyl orange (MO) dye and hexavalent chromium(VI) heavy metal ion. It is found that Ni4Fe1-LDH can remove more than 92% of MO in 10 min at the 10 mg/L MO initial concentration, and 97% of Cr(VI) in 1 h at 4 mg/L Cr2O7(2-) initial concentration. The saturated adsorption capacity of Ni4Fe1-LDH is found to be as large as 205.76 mg/g for MO and 26.78 mg/g for Cr(VI). The adsorption behavior of this new adsorbent is fitted well with Langmuir isotherm and the pseudo-second-order kinetic model, indicative of a monolayer and chemical adsorption that synergistically originates from exchangeable anions mechanism and layer charge density. Due to the excellent removal capacity of MO and Cr(VI), the NiFe-LDHs could be a promising adsorbent for wastewater treatment.

  14. Electrochemical sensor for bisphenol A based on ionic liquid functionalized Zn-Al layered double hydroxide modified electrode.

    Science.gov (United States)

    Zhan, Tianrong; Song, Yang; Li, Xianjun; Hou, Wanguo

    2016-07-01

    The plate-like Zn-Al layered double hydroxide modified with 1-aminopropyl-3-methylimidzaolium tetrafluoroborate (named as ILs-LDH) was synthesized by coprecipitation method. Several techniques confirmed the layered structure of ILs-LDH with a disk-like morphology. A novel electrochemical sensor based on ILs-LDH modified glass carbon electrode (GCE) was developed for bisphenol A (BPA) determination. Experimental factors including modified content, pH, scan rate, accumulation time and potential had been carefully optimized. ILs-LDH/GCE performed the excellent electro-oxidation ability toward BPA with the more negative oxidation overpotential and larger peak current than bare GCE or LDH/GCE. Differential pulse voltammetry determination of BPA afforded a wider linear range from 0.02 to 3μM with the detection limit of 4.6nM (S/N=3). The fabricated sensor demonstrated an acceptable reproducibility, good stability and high sensitivity. The proposed method was successfully used to detect BPA in real water samples with satisfactory recovery ranging from 94.9% to 102.0%.

  15. Self-assembling organomodified Co/Al based layered double hydroxides (LDH) via one-step route

    Institute of Scientific and Technical Information of China (English)

    WANG De-yi; A.LEUTERITZ; U.WAGENKNECHT; G.HEINRICH

    2009-01-01

    The preparation of self-assembling organomodified Co/Al-layered double hydroxide (LDH) via one-step route was studied.A common surfactant,sodium dodecylbenzenesulfonate (DBS),was employed as an organic modifier.The behavior and structure of self-assembled intercalated organic Co/Al-LDH were investigated by FTIR,SEM,WAXS,element analysis and TGA.Based upon the WAXS results and calculation by Bragg equation,the interlayer distance (d value) for organic Co/Al-LDH is enlarged from 0.75 nm to 3.10 nm,showing that the self-assembling behavior has been carried out successfully.Considering the observation from SEM,the product shows the morphology of organic Co/Al-LDH of a layered structure.In addition,FTIR,element analysis and TGA analysis show that the modifier is intercalated into the gallery of the Co/Al-LDH.Since organic modification for nanofiller is deemed to be necessary before applying it into polymer,the successful preparation of organomodified Co/Al-LDH will be significantly beneficial to the preparation and investigation of novel polymer/LDH nanocomposite.

  16. Layered double hydroxides as fillers in poly(l-lactide nanocomposites, obtained by in situ bulk polymerization

    Directory of Open Access Journals (Sweden)

    Telma Nogueira

    Full Text Available Abstract In this study in situ bulk polymerization of L-lactide filled with layered double hydroxides (LDH was investigated. Four different LDHs intercalated with two different organic anions (salicylate and sebacate were synthesized and characterized. After characterization, these synthetic layered compounds were used as fillers in poly(L-lactide (PLLA nanocomposites with two different fillers’s loadings (1 wt% and 2 wt%. PLLA and PLLA nanocomposites were evaluated by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, ultraviolet and visible spectroscopy, thermogravimetric analysis (TGA, dynamical mechanical analysis (DMA, flexural testing and differential scanning calorimetry (DSC. The results demonstrated that, compared to PLLA, the nanocomposite containing 1 wt% of Zn/Al salicylate transmitted less UVA and UVB light, while keeping a similar transparency in the visible region. Thermogravimetric analysis revealed that the nanocomposite with 1 wt% of Zn/Al salicylate exhibited the highest thermal stability. In general the flexural and dynamical mechanical properties were reduced in compassion to neat PLLA. DSC results, demonstrated that, compared to PLLA, all the nanocomposites exhibited lower glass transition temperature and melting temperature values.

  17. A single α-cobalt hydroxide/sodium alginate bilayer layer-by-layer assembly for conferring flame retardancy to flexible polyurethane foams

    Energy Technology Data Exchange (ETDEWEB)

    Mu, Xiaowei [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Yuan, Bihe [School of Resources and Environmental Engineering, Wuhan University of Technology, Wuhan 430070 (China); Pan, Ying; Feng, Xiaming; Duan, Lijin [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Zong, Ruowen, E-mail: zongrw@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Hu, Yuan, E-mail: yuanhu@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230026 (China)

    2017-04-15

    A layer-by-layer (LBL) assembly coating composed of α-cobalt hydroxide (α-Co(OH){sub 2}) and sodium alginate (SA) is deposited on flexible polyurethane (FPU) foam to reduce its flammability. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) are employed to prove the LBL assembly process. It is obvious from SEM results that a uniform and rough coating is deposited on FPU foam compared with that of untreated one. The peak intensity of methylene of SA in FITR spectra and typical (003) diffraction peak of α-Co(OH){sub 2} nanosheets at 11.0° in XRD patterns increases gradually with increment of bilayer number. Combustion behavior and toxicity suppression property of samples are characterized by cone calorimeter (under an irradiance of 35 kW m{sup −2}) and Thermogravimetry/Fourier transform infrared spectroscopy. The one and two bilayers (BL) coating on FPU foam can achieve excellent flame retardancy. Compared with untreated sample, the peak heat release rate of the coated FPU foam containing only one BL coating is reduced by 58.7%. The content of gaseous toxic substances during pyrolysis of FPU foam deposited with a single bilayer coating, such as CO and NCO-containing compounds, are reduced by 20.0% and 9.2%, respectively. Besides, the flame retardant mechanism of the coated FPU foam is also revealed. - Highlights: • The α-Co(OH){sub 2} nanosheets are firstly employed in LBL assembly. • A single α-cobalt hydroxide/sodium alginate bilayer LBL assembly for conferring excellent flame retardancy to FPU foam. • The flame retardant mechanism of LBL assembly FPU foam is displayed.

  18. Large pore volume mesoporous copper particles and scaffold microporous carbon material obtained from an inorganic-organic nanohybrid material, copper-succinate-layered hydroxide.

    Science.gov (United States)

    Ghotbi, Mohammad Yeganeh; Bagheri, Narjes; Sadrnezhaad, S K

    2011-10-01

    Copper-succinate-layered hydroxide (CSLH), a new nanohybrid material, was synthesized as an inorganic-organic nanohybrid, in which organic moiety was intercalated between the layers of a single cation layered material, copper hydroxide nitrate. Microporous scaffold carbon material was obtained by thermal decomposition of the nanohybrid at 500 °C under argon atmosphere followed by acid washing process. Furthermore, the heat-treated product of the nanohybrid at 600 °C was ultrafine mesoporous metallic copper particles. The results of this study confirmed the great potential of CSLH to produce the carbon material with large surface area (580 m(2)/g) and high pore volume copper powder (2.04 cm(3)/g).

  19. Studies on the intercalation of naproxen into layered double hydroxide and its thermal decomposition by in situ FT-IR and in situ HT-XRD

    Science.gov (United States)

    Wei, Min; Shi, Shuxian; Wang, Ji; Li, Yong; Duan, Xue

    2004-07-01

    Layered double hydroxides, novel anionic clay, meet the first requirement as inorganic matrices for encapsulating functional drugs or biomolecules with negative charge in aqueous media. In this study, naproxen has been intercalated into Mg-Al layered double hydroxide by the methods of ion exchange. The structure and composition of the intercalated material have been studied by X-ray diffraction (XRD), UV-vis spectroscopy and inductively coupled plasma emission spectroscopy. A schematic model has been proposed. Furthermore, in situ Fourier transform infrared spectroscopy, in situ high-temperature XRD, and thermogravimetry (TG) have been used to characterize the thermal decomposition of the hybrid material. It has been found that the thermal stability of the intercalated naproxen is significantly enhanced compared with the pure form before intercalation, which suggests that this drug-inorganic layered material may have prospective application as the basis of a novel drug delivery system.

  20. Radiation induced topotactic [2 + 2] dimerisation of acrylate derivatives among the layers of a CaFe layered double hydroxide followed by IR spectroscopy

    Science.gov (United States)

    Srankó, D. F.; Canton, S.; Enghdahl, A.; Muráth, Sz.; Kukovecz, Á.; Kónya, Z.; Sipiczki, M.; Sipos, P.; Pálinkó, I.

    2013-07-01

    Various acrylates [E-phenylpropenoate, E-3(4‧-nitrophenyl)propenoate, E-3(2‧,5‧-difluorphenyl)propenoate, E-3(2‧-thienyl)propenoate, E-3(4‧-imidazolyl)propenoate or E-2,3-dimethylpropenoate] were successfully intercalated into Ca(II)Fe(III) layered double hydroxide (CaFe-LDH) verified by a range of instrumental methods. The possible arrangements for the organic anions were suggested on the basis of basal spacing data, layer thickness and the dimensions of the quantum chemically optimised structures of the acrylate ions. Using the acrylate-CaFe-LDHs as reactant-filled nanoreactors, photoinitiated topotactic [2 + 2] cyclisation reactions followed by IR spectroscopy could be performed with many representatives [E-phenylpropenoate-, E-3(4‧-nitrophenyl)propenoate-, E-3(2‧,5‧-difluorphenyl)propenoate- or E-3(2‧-thienyl)propenoate-CaFe-LDHs] resulting in cyclobutane derivatives within the layers of the host material indicating that there were domains where the intercalated anions were in close proximity to each other and in proper arrangement for the reaction to occur.

  1. Facile synthesis of NiAl-layered double hydroxide/graphene hybrid with enhanced electrochemical properties for detection of dopamine

    Science.gov (United States)

    Li, Meixia; Zhu, Jun E.; Zhang, Lili; Chen, Xu; Zhang, Huimin; Zhang, Fazhi; Xu, Sailong; Evans, David G.

    2011-10-01

    Layered double hydroxides (LDHs), also known as hydrotalcite-like anionic clays, have been investigated widely as promising electrochemical active materials. Due to the inherently weak conductivity, the electrochemical properties of LDHs were improved typically by utilization of either functional molecules intercalated between LDH interlayer galleries, or proteins confined between exfoliated LDH nanosheets. Here, we report a facile protocol to prepare NiAl-LDH/graphene (NiAl-LDH/G) nanocomposites using a conventional coprecipitation process under low-temperature conditions and subsequent reduction of the supporting graphene oxide. Electrochemical tests showed that the NiAl-LDH/G modified electrode exhibited highly enhanced electrochemical performance of dopamine electrooxidation in comparison with the pristine NiAl-LDH modified electrode. Results of high-resolution transmission electron microscopy and Raman spectra provide convincing information on the nanostructure and composition underlying the enhancement. Our results of the NiAl-LDH/G modified electrodes with the enhanced electrochemical performance may allow designing a variety of promising hybrid sensors via a simple and feasible approach.Layered double hydroxides (LDHs), also known as hydrotalcite-like anionic clays, have been investigated widely as promising electrochemical active materials. Due to the inherently weak conductivity, the electrochemical properties of LDHs were improved typically by utilization of either functional molecules intercalated between LDH interlayer galleries, or proteins confined between exfoliated LDH nanosheets. Here, we report a facile protocol to prepare NiAl-LDH/graphene (NiAl-LDH/G) nanocomposites using a conventional coprecipitation process under low-temperature conditions and subsequent reduction of the supporting graphene oxide. Electrochemical tests showed that the NiAl-LDH/G modified electrode exhibited highly enhanced electrochemical performance of dopamine

  2. Layered double hydroxides as carriers for quantum dots@silica nanospheres

    Science.gov (United States)

    Stoica, Georgiana; Castelló Serrano, Iván.; Palomares, Emilio

    2013-02-01

    Quantum dot-hydrotalcite layered nanoplatforms were successfully prepared following a one-pot synthesis. The process is very fast and a priori delamination of hydrotalcite is not a prerequisite for the intercalation of quantum dots. The novel materials were extensively characterized by X-ray diffraction, thermogravimetry, infrared spectroscopy, transmission electron microscopy, true color fluorescence microscopy, photoluminescence, and nitrogen adsorption. The quantum dot-hydrotalcite nanomaterials display extremely high stability in mimicking physiological media such as saline serum (pH 5.5) and PBS (pH 7.2). Yet, quantum dot release from the solid structure is noted. In order to prevent the leaking of quantum dots we have developed a novel strategy which consists on using tailor made double layered hydrotalcites as protecting shells for quantum dots embedded into silica nanospheres without changing either the materials or the optical properties.

  3. Synthesis, characterization and magnetic behavior of Mg–Fe–Al mixed oxides based on layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Heredia, Angélica C., E-mail: angelicacheredia@gmail.com [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina); Oliva, Marcos I. [IFEG, Universidad Nacional de Córdoba, Córdoba (Argentina); CONICET (Argentina); Agú, Ulises [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina); CONICET (Argentina); Zandalazini, Carlos I. [CONICET (Argentina); INFIQC, FCQ Universidad Nacional de Córdoba, Córdoba (Argentina); Marchetti, Sergio G. [CINDECA, UNLP, Buenos Aires (Argentina); Herrero, Eduardo R.; Crivello, Mónica E. [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina)

    2013-09-15

    In the present work, Mg–Al–Fe layered double hydroxides were prepared by coprecipitation reaction with hydrothermal treatment. The characterization of precursors and their corresponding calcinated products (mixed oxides) were carried out by X ray diffraction, X-ray photoelectron spectroscopy (XPS), termogravimetric analysis and differential scanning calorimetry, diffuse reflectance UV–vis spectroscopy, specific surface area, Mössbauaer and magnetic properties. The Fe{sup 3+} species were observed in tetrahedrally and octahedrally coordination in brucite layered. The XPS analysis shows that the Fe{sup 3+} ions can be found in two coordination environments (tetrahedral and octahedral) as mixed oxides, and as spinel-structure. Oxides show a decrease in the specific surface areas when the iron loading is increased. The magnetic and Mössbauaer response show that MgAlFe mixed oxides are different behaviours such as different population ratios of ferromagnetic, weak-ferromagnetic, paramagnetic and superparamagnetic phases. The better crystallization of spinel structure with increased temperature, is correlated with the improved magnetic properties. - Highlights: • Mg–Al–Fe were successfully prepared by coprecipitation with hydrothermal treatment. • MgO, α-Fe{sub 2}O{sub 3,} MgFe{sub 2}O{sub 4} were detected by XRD in the calcined samples. • The Fe{sup 3+} is in tetrahedral and octahedral coordination in the brucite layered. • The specific surface area is directly related with the iron content. • The magnetic properties and MgFe{sub 2}O{sub 4} improve with increasing calcination temperature.

  4. Magnetic-field-assisted assembly of layered double hydroxide/metal porphyrin ultrathin films and their application for glucose sensors.

    Science.gov (United States)

    Shao, Mingfei; Xu, Xiangyu; Han, Jingbin; Zhao, Jingwen; Shi, Wenying; Kong, Xianggui; Wei, Min; Evans, David G; Duan, Xue

    2011-07-01

    The ordered ultrathin films (UTFs) based on CoFe-LDH (layered double hydroxide) nanoplatelets and manganese porphyrin (Mn-TPPS) have been fabricated on ITO substrates via a magnetic-field-assisted (MFA) layer-by-layer (LBL) method and were demonstrated as an electrochemical sensor for glucose. The XRD pattern for the film indicates a long-range stacking order in the normal direction of the substrate. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) images of the MFA LDH/Mn-TPPS UTFs reveal a continuous and uniform surface morphology. Cyclic voltammetry, impedance spectroscopy, and chronoamperometry were used to evaluate the electrochemical performance of the film, and the results show that the MFA-0.5 (0.5 T magnetic field) CoFe-LDH/Mn-TPPS-modified electrode displays the strongest redox current peaks and fastest electron transfer process compared with those of MFA-0 (without magnetic-field) and MFA-0.15 (0.15 T magnetic field). Furthermore, the MFA-0.5 CoFe-LDH/Mn-TPPS exhibits remarkable electrocatalytic activity toward the oxidation of glucose with a linear response range (0.1-15 mM; R(2) = 0.999), low detection limit (0.79 μM) and high sensitivity (66.3 μA mM(-1) cm(-2)). In addition, the glucose sensor prepared by the MFA LBL method also shows good selectivity and reproducibility as well as resistance to poisoning in a chloride ion solution. Therefore, the novel strategy in this work creates new opportunities for the fabrication of nonenzyme sensors with prospective applications in practical detection.

  5. Preparation of Tween 80-Zn/Al-Levodopa-Layered Double Hydroxides Nanocomposite for Drug Delivery System

    OpenAIRE

    Aminu Umar Kura; Samer Hasan Hussein-Al-Ali; Mohd Zobir Hussein; Sharida Fakurazi

    2014-01-01

    We incorporated anti-Parkinsonian drug, levodopa (dopa), in Zn/Al-LDH by coprecipitation method to form dopa-LDH nanocomposite. Further coating of Tween-80 on the external surfaces of dopa-LDH nanocomposite was achieved through the oxygen of C=O group of Tween-80 with the layer of dopa-LDH nanocomposite. The final product is called Tween-dopa-LDH nanocomposite. The X-ray diffraction indicates that the Tween-dopa-LDH nanocomposite was formed by aggregation structure. From the TGA data, the Twe...

  6. Magnesium Hydroxide

    Science.gov (United States)

    Magnesium hydroxide is used on a short-term basis to treat constipation.This medication is sometimes prescribed ... Magnesium hydroxide come as a tablet and liquid to take by mouth. It usually is taken as ...

  7. Atomically thin layered NiFe double hydroxides assembled 3D microspheres with promoted electrochemical performances

    Science.gov (United States)

    Li, Xiaomin; Zai, Jiantao; Liu, Yuanyuan; He, Xiaobo; Xiang, Shijie; Ma, Zifeng; Qian, Xuefeng

    2016-09-01

    LDHs in atomic thickness (mono-/bi-layers) usually exhibit novel physicochemical properties, especially in surface-dependent energy storage and catalysis areas. However, the thickness of the commonly reported 2D LDHs is in nanoscale and the bottom-up synthesis of atomically thin LDHs is rarely reported. Herein, high-quality atomically thin layered NiFe-LDHs assembled 3D microspheres were synthesized via a rational designed reaction system, where the formation of atomically thin building blocks was controlled by the synergetic effects of released carbonate anions and butanol. Furthermore, the complexant and solvents played important effects on the process of coprecipitation and the assembling of LDHs. Due to the nature of atomically thin LDHs nanosheets and unique 3D hierarchical structures, the obtained microspheres exhibited excellent electrocatalytic oxygen evolution reaction (OER) activity in alkaline medium with an onset overpotential (0.435 V, which is lower than that of common LDHs) and good durability. The as-prepared 3D NiFe-LDHs microspheres were also firstly used as supercapacitor materials and displayed a high specific capacitance of 1061 F g-1 at the current density of 1 A g-1.

  8. Self-Supported Nickel Iron Layered Double Hydroxide-Nickel Selenide Electrocatalyst for Superior Water Splitting Activity.

    Science.gov (United States)

    Dutta, Soumen; Indra, Arindam; Feng, Yi; Song, Taeseup; Paik, Ungyu

    2017-09-19

    The design of efficient, low-cost, and stable electrocatalyst systems toward energy conversion is highly demanding for their practical use. Large scale electrolytic water splitting is considered as a promising strategy for clean and sustainable energy production. Herein, we report a self-supported NiFe layered double hydroxide (LDH)-NiSe electrocatalyst by stepwise surface-redox-etching of Ni foam (NF) through a hydrothermal process. The as-prepared NiFe LDH-NiSe/NF catalyst exhibits far better performance in alkaline water oxidation, proton reduction, and overall water splitting compared to NiSex/NF or NiFe LDH/NF. Only 240 mV overpotential is required to obtain a water oxidation current density of 100 mA cm(-2), whereas the same for the hydrogen evolution reaction is 276 mV in 1.0 M KOH. The synergistic effect from NiSe and NiFe LDH leads to the evolution of a highly efficient catalyst system for water splitting by achieving 10 mA cm(-2) current density at only 1.53 V in a two-electrode alkaline electrolyzer. In addition, the designed electrode produces stable performance for a long time even at higher current density to demonstrate its robustness and prospective as a real-life energy conversion system.

  9. Tribological performance of Mg/Al/Ce layered double hydroxides nanoparticles and intercalated products as lubricant additives

    Science.gov (United States)

    Li, Shuo; Qin, Haojing; Zuo, Ranfang; Bai, Zhimin

    2015-10-01

    Mg/Al/Ce ternary layered double hydroxides (LDHs) were synthesized via coprecipitation and intercalated by succinic acid and lauric acid through ion exchange method respectively. The LDHs products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared (FT-IR). Tribological properties of LDHs as lubricant additives were evaluated by four-ball friction and air compressor test. The results indicated that Mg/Al/Ce LDHs were prepared successfully with Ce/Al molar ratio of 0.05 and crystallization temperature of 140 °C. The interlayer spacing of LDHs precursor was expanded by succinic acid and lauric acid to 8.838 and 17.519 Å respectively. All the three LDHs products can reduce friction and wear of engine lubricating oil in the tests. LDHs intercalated with lauric acid showed best tribological performance among them which was attributed to sliding each other between laminates, good dispersibility in oil medium and a protective tribofilm formed on the worn surface.

  10. Removal efficiency of fluoride by novel Mg-Cr-Cl layered double hydroxide by batch process from water

    Institute of Scientific and Technical Information of China (English)

    Sandip Mandal; Swagatika Tripathy; Tapswani Padhi; Manoj Kumar Sahu; Raj Kishore Patel

    2013-01-01

    The fluoride ion removal from aqueous solution using synthesized Mg-Cr-Cl layered double hydroxide has been reported.Mg-Cr-Cl was characterized by X-ray powder diffraction,Fourier-transform infrared,thermo-gravimetric analysis,differential thermal analysis,and scanning electron microscope.Adsorption experiments were carried out in batch mode as a function of adsorption dosages,contact time,pH,and initial fluoride concentration to get optimum adsorption capacity.The adsorption kinetic study showed that the adsorption process followed first order kinetics.The fluoride removal was 88.5% and 77.4% at pH 7 with an adsorbent dose of 0.6 g/100 mL solution and initial fluoride concentration of 10 mg/L and 100 mg/L,respectively.The equilibrium was established at 40 min.Adsorption experiment data were fitted well with Langmuir isotherm with Ra =0.9924.Thermodynamic constants were also measured and concluded that the adsorption process was spontaneous and endothermic in nature.The removal percentage decreased slowly with increasing pH.This process is suitable for industrial effluents.The regeneration of the material is not possible.

  11. Tailoring surface properties and structure of layered double hydroxides using silanes with different number of functional groups

    Science.gov (United States)

    Tao, Qi; He, Hongping; Li, Tian; Frost, Ray L.; Zhang, Dan; He, Zisen

    2014-05-01

    Four silanes, trimethylchlorosilane (TMCS), dimethyldiethoxylsilane (DMDES), 3-aminopropyltriethoxysilane (APTES) and tetraethoxysilane (TEOS), were adopted to graft layered double hydroxides (LDH) via an induced hydrolysis silylation method (IHS). Fourier transform infrared spectra (FTIR) and 29Si MAS nuclear magnetic resonance spectra (29Si MAS NMR) indicated that APTES and TEOS can be grafted onto LDH surfaces via condensation with hydroxyl groups of LDH, while TMCS and DMDES could only be adsorbed on the LDH surface with a small quantity. A combination of X-ray diffraction patterns (XRD) and 29Si MAS NMR spectra showed that silanes were exclusively present in the external surface and had little influence on the long range order of LDH. The surfactant intercalation experiment indicated that the adsorbed and/or grafted silane could not fix the interlamellar spacing of the LDH. However, they will form crosslink between the particles and affect the further surfactant intercalation in the silylated samples. The replacement of water by ethanol in the tactoids and/or aggregations and the polysiloxane oligomers formed during silylation procedure can dramatically increase the value of BET surface area (SBET) and total pore volumes (Vp) of the products.

  12. Horseradish peroxidase immobilization on carbon nanodots/CoFe layered double hydroxides: direct electrochemistry and hydrogen peroxide sensing.

    Science.gov (United States)

    Wang, Yinling; Wang, Zhangcui; Rui, Yeping; Li, Maoguo

    2015-02-15

    Carbon nanodots and CoFe layered double hydroxide composites (C-Dots/LDHs) were prepared via simply mixing C-Dots and CoFe-LDHs. The as-prepared composites were used for the immobilization of horseradish peroxidase (HRP) on the glass carbon (GC) electrode. The electrochemical behavior of the HRP/C-Dots/LDHs/GC electrode and its application as a H2O2 biosensor were investigated. The results indicated that HRP immobilized by C-Dots/LDHs retained the activity of enzyme and displayed quasi-reversible redox behavior and fast electron transfer with an electron transfer rate constant ks of 8.46 s(-1). Under optimum experimental conditions, the HRP/C-Dots/LDHs/GC electrode displayed good electrocatalytic reduction activity and excellent analytic performance toward H2O2. The H2O2 biosensor showed a linear range of 0.1-23.1 μM (R(2) = 0.9942) with a calculated detection limit of 0.04 μM (S/N = 3). In addition, the biosensor exhibited high sensitivity, good selectivity, acceptable reproducibility and stability. The superior properties of this biosensor are attributed to the synergistic effect of HRP, C-Dots and CoFe-LDHs, which has been proved by investigating their electrochemical response to H2O2. Thus the C-Dots and LDHs composites provide a promising platform for the immobilization of redox enzymes and construction of sensitive biosensors.

  13. Preparation and antibacterial property of waterborne polyurethane/Zn-Al layered double hydroxides/ZnO nanocomposites.

    Science.gov (United States)

    Zhang, Wei-De; Zheng, Yun-Min; Xu, Yang-Sen; Yu, Yu-Xiang; Shi, Qing-Shan; Liu, Lihong; Peng, Hong; Ouyang, Yousheng

    2013-01-01

    In this work, a novel environmental-friendly waterborne polyurethane/ZnAl-layered double hydroxides/ZnO nanoparticles composite (WPU/ZnAl-LDHs/ZnO) was synthesized via in-situ polymerization. ZnAl-LDHs and ZnAl-LDHs/ZnO were synthesized by refluxing in an oil bath. In order to disperse ZnAl-LDHs/ZnO homogeneously into WPU matrix, ZnAl-LDHs/ZnO was firstly functionalized by isophorone diisocyanate. The incorporated content of ZnAl-LDHs/ZnO in the composite has profound effect on such physical properties as mechanical strength, thermal stability and water swelling. It is demonstrated that appropriate amount of ZnAl-LDHs/ZnO with good dispersion in the WPU matrix significantly improves the physical performance of the composites. Finally, the antibacterial activity of the composite was tested against G(-) Escherichia coli and G(+) Staphylococcus aureus. The results indicate that WPU incorporated with ZnAl-LDHs/ZnO shows strong antibacterial activity upon contact.

  14. Study on fire-retardant nanocrystalline Mg-Al layered double hydroxides synthesized by microwave-crystallization method

    Institute of Scientific and Technical Information of China (English)

    ZHANG Zejiang; XU Chenghua; QIU Fali; MEI Xiujuan; LAN Bin; ZHANG Shuosheng

    2004-01-01

    Nanocrystalline Mg-Al layered double hydroxides with the particle size being 10-40 nm were firstly prepared by the technology of the microwave-crystallization and the variable-speed addition of the alkali. The obtained samples were characterized by TEM and XRD. The roles of the microwave and addition rate of the alkali were also discussed in the present work. The thermal decomposition activation energy of the nano-LDHs was calculated according to their TG, DTG and DSC curves by the Ozawa method. The results showed that the thermal decomposition of the nano-LDHs had four steps. Thereby the decomposition model of the nano-LDHs was supposed according to the analysis of their thermal decomposition. After PS, ABS, HDPE and PVC were filled with the nano-LDHs, their LOI values could be increased up to 28, 27, 26 and 33, respectively. When the fire-retardant coating contained 1.9% of the nano-LDHs that was 0.27 times the dosage of the conventional TiO2, its fire endurance time reached 32.75min that was 7.05 min longer than that of the best coating containing TiO2 according to the model big-panel combustion test method.

  15. Thermodynamical and structural insights of orange II adsorption by Mg RAlNO 3 layered double hydroxides

    Science.gov (United States)

    Mustapha Bouhent, Mohamed; Derriche, Zoubir; Denoyel, Renaud; Prevot, Vanessa; Forano, Claude

    2011-05-01

    [Mg 1- x Al x(OH) 2][(NO 3) x, nH 2O] Layered Double Hydroxide (LDH) sorbents with variable Mg/Al molar ( R=(1- x)/ x) ratios were investigated for adsorption of azo dye, orange II (OII) at various pH and temperature conditions. Mg 2AlNO 3 displays the highest adsorption capacity with 3.611 mmol of OII per gram of Mg 2AlNO 3 at 40 °C. Adsorption isotherms have been fitted using the Langmuir model and free energy of adsorption (Δ G°), enthalpy (Δ H°) and entropy (Δ S°) were calculated. The experimental values for Δ G° in temperature range between 10 and 40 °C were found to be negative indicating that a spontaneous process occurred. Positive calculated enthalpy values, characteristic of an endothermic process were found. Characterization of solids (PXRD, FTIR, UV-vis, TGA/DTA, adsorption isotherm BET analysis, SEM and Zetametry) before and after adsorption showed that adsorption proceeds in two steps. First, adsorption occurs at the LDH surface, followed by intercalation via anion exchange.

  16. Adsorption study of anionic reactive dye from aqueous solution to Mg-Fe-CO3 layered double hydroxide (LDH)

    Science.gov (United States)

    Ahmed, I. M.; Gasser, M. S.

    2012-10-01

    Mg-Fe-Cl Layered double hydroxides (LDHs) have been prepared using a method involving separate nucleation and aging steps with Mg/Fe = 3. The interlayer anions readily replaced by carbonate are characterized by X-ray diffraction (XRD) and FTIR. The effects of different parameters, such as pH, contact time, concentration of dye and temperature on the capacity and adsorption mechanism of Mg-Fe-CO3-LDH in removing an anionic dye (congo red, CR) from aqueous solution were separately investigated. The results show that Mg-Fe-CO3-LDH is particularly efficient in removing CR and the dye removal increases with decreasing pH. The adsorption of CR on Mg-Fe-CO3-LDH reached equilibrium after 15 min where 100 mg/L CR was removed. The equilibrium isotherm indicates that the adsorption of CR onto Mg-Fe-CO3-LDH fits to Langmuir and Freundlich equation as well. The adsorption data obtained from the Langmuir model gave good values of the determination coefficient and the saturated adsorption capacity of Mg-Fe-CO3-LDH for CR was found to be 104.6 mg/g. The regeneration study indicates that the prepared LDH could be used for several cycles. The thermodynamic parameters have been calculated, and the adsorption process was found to be spontaneous, endothermic in nature and follows a pseudo-second-order kinetic model.

  17. A review of the removal of anions and oxyanions of the halogen elements from aqueous solution by layered double hydroxides.

    Science.gov (United States)

    Theiss, Frederick L; Couperthwaite, Sara J; Ayoko, Godwin A; Frost, Ray L

    2014-03-01

    The application of layered double hydroxides (LDHs) and thermally activated LDHs for the removal of various fluorine (F(-),BF4(-)), chlorine (Cl(-),ClO4(-)), bromine (Br(-),BrO3(-)) and iodine (I(-),IO3(-)) species from aqueous solutions has been reviewed in this article. LDHs and thermally activated LDHs were able to significantly reduce the concentration of selected anions in laboratory scale experiments. The M(2+):M(3+) cation ratio of the LDH adsorbent was an important factor which influenced anion uptake. Though LDHs were able to remove some target anion species through anion exchange and surface adsorption thermal activation and reformation generally produced better results. The presence of competing anions including carbonate, phosphate and sulphate had a significant impact on uptake of the target anion as LDHs typically exhibit lower affinity towards monovalent anions compared to anions with multiple charges. The removal of fluoride and perchlorate from aqueous solution by a continuous flow system utilising fixed bed columns packed with LDH adsorbents has also been investigated. The adsorption capacity of the columns at breakpoint was heavily dependent on the flow rate and lower than result reported for the corresponding batch methods. There is still considerable scope for future research on numerous topics summarised in this article.

  18. Catalytic synthesis of nitrogen-doped multi-walled carbon nanotubes using layered double hydroxides as catalyst precursors

    Indian Academy of Sciences (India)

    Yong Cao; Yun Zhao; Qingxia Li; Qingze Jiao

    2009-03-01

    The nitrogen (N)-doped carbon (CN) nanotubes were synthesized by pyrolysis of ethylenediamine with Ni1.07Mg1.01AlO3.58, Ni1.99Mg0.29AlO3.78, and Ni2.31Mg0.08AlO3.89 mixed oxides as catalysts at 650°C. Those mixed oxides were obtained by calcination of corresponding layered double hydroxide precursors (LDHs). Structure and composition of LDHs and mixed oxides were characterized by X-ray diffraction (XRD) and Inductively coupled plasma spectrum. X-ray photoelectron spectroscopy and transmission electron microscope were used to characterize the N content, proportion of pyridine-like N structure and morphology of CN nanotubes. The results showed that the tubes grown with Ni2.31Mg0.08AlO3.89 as catalysts had more obvious bamboo-like structure, larger diameter than those grown with Ni1.07Mg1.01AlO3.58 and Ni1.99Mg0.29AlO3.78. The N content and proportion of graphitic-like N structures increased with the content of Ni2+ increasing in LDH precursors. The morphology, N content and pyridine-like N structures for CN nanotubes can be controlled to a certain extent by varying the content of Ni2+ in LDH precursors.

  19. Insitu grown superhydrophobic Zn–Al layered double hydroxides films on magnesium alloy to improve corrosion properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Meng; Pang, Xiaolu; Wei, Liang; Gao, Kewei, E-mail: kwgao@yahoo.com

    2015-05-15

    Highlights: • Hierarchical superhydrophobic Zn–Al LDHs film has been fabricated on a magnesium alloy substrate. • The superhydrophobic surface has good long-term stability under atmospheric environment. • The superhydrophobic surface can provide a stable corrosion protection for the Mg alloys. - Abstract: A hierarchical superhydrophobic zinc–aluminum layered double hydroxides (Zn–Al LDHs) film has been fabricated on a magnesium alloy substrate via a facile hydrothermal crystallization method following chemical modification. The characteristics of the films were investigated by X-ray diffraction (XRD), scanning electronic microscope (SEM), and energy dispersive spectroscopy (EDS). XRD patterns and SEM images showed that the micro/nanoscale hierarchical LDHs film surfaces composed of ZnO nanorods and Zn–Al LDHs nanowalls structures. The static contact angle (CA) for the prepared surfaces was observed at around 165.6°. The corrosion resistance of the superhydrophobic films was estimated by electrochemical impedance spectroscopy (EIS) and potentiondynamic polarization measurement. EIS and polarization measurements revealed that the superhydrophobic Zn–Al LDHs coated magnesium alloy had better corrosion resistance in neutral 3.5 wt.% NaCl solution.

  20. The alternative use of layered double hydroxides as extraction medium coupled with microcomplexation for determination of phosphate in water samples

    Science.gov (United States)

    Gissawong, Netsirin; Sansuk, Sira; Srijaranai, Supalax

    2017-02-01

    A simple, rapid, in situ, and green extraction combined with a microcomplexation has been developed for the spectrophotometric determination of phosphate in water samples. Through their formation, layered double hydroxides (LDHs) were employed as the extraction medium, instantly commenced by a rapid addition of a mixed solution of Mg2 + and Al3 + ions into alkaline phosphate solution. After the extraction, LDH precipitate containing phosphate was dissolved by sulfuric acid and the released phosphate was subsequently detected via its complexation with molybdate in the presence of antimonyl and ascorbic acid. Under optimum conditions, the linearity in the range of 5-200 μg L- 1, with the correlation coefficient (r2) of 0.9969, and the enrichment factor (EF) of 14 were obtained. The limit of detection (LOD) of 5 μg L- 1 and good precision, with the relative standard deviations (RSDs) less than 8.16%, were achieved. The proposed method was successfully applied to determine phosphate in water samples and the relative recoveries of 72.97-115.32% were obtained.

  1. Enhanced removal performance by the core-shell zeolites/MgFe-layered double hydroxides (LDHs) for municipal wastewater treatment.

    Science.gov (United States)

    Guo, Lu; Zhang, Xiangling; Chen, Qiaozhen; Ruan, Congying; Leng, Yujie

    2016-04-01

    The application of powdered layer double hydroxides (LDHs) in constructed rapid infiltration system (CRIS) appears to be an appreciable problem still unsolved due to the small particle size and the low density. Therefore, the core-shell zeolites/MgFe-LDHs composites were prepared via using co-precipitation method in present study. To investigate the practical applicability, a detailed organics, ammonia, and total phosphorus removal study were carried out in columns to treat the municipal wastewater. The scanning electron microscope (SEM) and energy dispersive spectrometer (EDS) results confirmed the successful synthesis of core-shell zeolites/MgFe-LDHs through coating on the surface of zeolites. Accordingly, the zeolites/MgFe-LDHs largely reduced the COD by 81.14 %, NH4 (+)-N by 81.50%, and TP by 83.29%. Phosphate adsorption study revealed that the equilibrium adsorption data were better fitted by Langmuir isothermal model, with the maximum adsorption capacity of 79.3651 mg/kg for zeolites/MgFe-LDHs and 38.4615 mg/kg for the natural zeolites. In addition, economic analysis indicated that the reagent cost of synthesis of zeolites/MgFe-LDHs was economical. Herein, the zeolites/MgFe-LDHs solved the natural zeolites problem for poor P removal and the application of powdered LDHs in the solid/liquid separation process, suggesting that it was applicable as potential substrates for the removal of organics, ammonia, and total phosphorus in CRIS.

  2. Impact of size, secondary structure, and counterions on the binding of small ribonucleic acids to layered double hydroxide nanoparticles

    Science.gov (United States)

    Rodriguez, Blanca V.; Pescador, Jorge; Pollok, Nicole; Beall, Gary W.; Maeder, Corina; Lewis, L. Kevin

    2015-01-01

    Use of ribonucleic acid (RNA) interference to regulate protein expression has become an important research topic and gene therapy tool, and therefore, finding suitable vehicles for delivery of small RNAs into cells is of crucial importance. Layered double metal hydroxides such as hydrotalcite (HT) have shown great promise as nonviral vectors for transport of deoxyribose nucleic acid (DNA), proteins, and drugs into cells, but the adsorption of RNAs to these materials has been little explored. In this study, the binding of small RNAs with different lengths and levels of secondary structure to HT nanoparticles has been analyzed and compared to results obtained with small DNAs in concurrent experiments. Initial experiments established the spectrophotometric properties of HT in aqueous solutions and determined that HT particles could be readily sedimented with near 100% efficiencies. Use of RNA+HT cosedimentation experiments as well as electrophoretic mobility shift assays demonstrated strong adsorption of RNA 25mers to HT, with twofold greater binding of single-stranded RNAs relative to double-stranded molecules. Strong affinities were also observed with ssRNA and dsRNA 54mers and with more complex transfer RNA molecules. Competition binding and RNA displacement experiments indicated that RNA-HT associations were strong and were only modestly affected by the presence of high concentrations of inorganic anions. PMID:26620852

  3. The decomposition of the layered double hydroxides of Co and Al: Phase segregation of a new single phase spinel oxide

    Science.gov (United States)

    Babay, Salem; Bulou, Alain; Mercier, Anne Marie; Toumi, Mouhamed

    2015-04-01

    Monophasic Co-Al-CO3-like layered double hydroxides has been prepared by the coprecipitation method. It has been characterised by Rietveld refinement of the X-ray powder diffraction pattern, DTA-TGA, infrared and Raman spectroscopies. Its structure is trigonal, R 3 bar m with cell parameters a = 0.3061(4) nm and c = 2.252 (3) nm. The decomposition of this hydrotalcite-like structure on heating up to 800 °C yields to a single phase spinel oxide. Besides, infrared and Raman spectroscopies showed the presence of spinel-like domains. The results of Rietveld refinement have revealed that this compound has the Fd 3 bar m space group (a = 0.8088(4) nm), with crystallographic formula [CoII0.75Al0.25]8a[CoII0.252CoIII0.77Al0.98]16dO4, which is of the general formula Co1.77Al1.23O4. This structure is also validated by the charge distribution (CD) analysis.

  4. Removal of arsenate from aqueous solution by nanocrystalline Mg/Al layered double hydroxide: sorption characteristics, prospects, and challenges.

    Science.gov (United States)

    Goh, K H; Lim, T T; Dong, Z L

    2010-01-01

    Removal of arsenate (As(V)) from aqueous solution using both nanocrystalline and coprecipitated Mg/Al layered double hydroxides (LDHs) was examined under different sorption/desorption conditions. The surface area, pore volume, and pore size of the nanocrystalline LDH were significantly higher than those of the coprecipitated LDH, thus resulting in a higher As(V) sorption maximum than the coprecipitated LDH. The calculated activation energy (E(a)) value was 24.7 kJ/mol, suggesting the occurrence of anion exchange process for As(V) removal by the nanocrystalline LDH. The predominance of anion exchange process was further supported by the investigation of ionic strength effect, and XRD and FTIR analyses. The effect of aqueous matrix on As(V) sorption by the nanocrystalline LDH was found to increase in the order of nitrate nanocrystalline LDH besides the predominant anion exchange process. Prospects and challenges for practical application of the nanocrystalline LDH were also discussed in the latter part of this study.

  5. In situ real time infrared spectroscopy of sorption of (poly)molybdate ions into layered double hydroxides.

    Science.gov (United States)

    Davantès, A; Lefèvre, G

    2013-12-05

    The sorption of (poly)molybdate ions into layered double hydroxides (LDHs), with Zn(2+) and Al(3+) cations, has been followed by in situ infrared spectroscopy using the attenuated total reflection technique. The exchange between solution molybdate species and interlayer anions has been followed in real time, illustrating the different behavior of molybdate ions and polymolybdate species. In a first part, the Mo(VI) speciation in solution was performed by comparison of thermodynamical calculations and infrared spectroscopy of solutions with different pH. Decomposition of bands between 800 to 1000 cm(-1), corresponding to the (Mo-O) stretching vibration, has permitted to identify major (poly)molybdate species. In the presence of LDH, the measurements have shown a high affinity for heptamolybdate (Mo7O24(6-)) species, and its preferential sorption in comparison with molybdate ions or other protonated polymolybdate species even if it represents very small fractions. From these measurements, the affinity series Mo7O24(6-) > CO3(2-) > MoO4(2-) > SO4(2-) have been directly obtained.

  6. Controlled drug release from antibiotic-loaded layered double hydroxide coatings on porous titanium implants in a mouse model.

    Science.gov (United States)

    Badar, Muhammad; Rahim, Muhammad Imran; Kieke, Marc; Ebel, Thomas; Rohde, Manfred; Hauser, Hansjörg; Behrens, Peter; Mueller, Peter P

    2015-06-01

    As an alternative to degradable organic coatings the possibility of using layered double hydroxides (LDHs) to generate implant coatings for controlled drug delivery was evaluated in vivo and in vitro. Coatings prepared from LDH suspensions dissolved slowly and appeared compatible with cultured cells. LDH coatings loaded with an antibiotic resulted in antibacterial effects in vitro. The LDH coating prolonged the drug release period and improved the proliferation of adherent cells in comparison to pure drug coatings. However, during incubation in physiological solutions the LDH coatings became brittle and pieces occasionally detached from the surface. For stress protection porous titanium implants were investigated as a substrate for the coatings. The pores prevented premature detachment of the coatings. To evaluate the coated porous implants in vivo a mouse model was established. To monitor bacterial infection of implants noninvasive in vivo imaging was used to monitor luminescently labeled Pseudomonas aeruginosa. In this model porous implants with antibiotic-loaded LDH coatings could antagonize bacterial infections for over 1 week. The findings provide evidence that delayed drug delivery from LDH coatings could be feasible in combination with structured implant surfaces.

  7. Layered Double Hydroxide Nanoplatelets with Excellent Tribological Properties under High Contact Pressure as Water-Based Lubricant Additives

    Science.gov (United States)

    Wang, Hongdong; Liu, Yuhong; Chen, Zhe; Wu, Bibo; Xu, Sailong; Luo, Jianbin

    2016-03-01

    High efficient and sustainable utilization of water-based lubricant is essential for saving energy. In this paper, a kind of layered double hydroxide (LDH) nanoplatelets is synthesized and well dispersed in water due to the surface modification with oleylamine. The excellent tribological properties of the oleylamine-modified Ni-Al LDH (NiAl-LDH/OAm) nanoplatelets as water-based lubricant additives are evaluated by the tribological tests in an aqueous environment. The modified LDH nanoplatelets are found to not only reduce the friction but also enhance the wear resistance, compared with the water-based cutting fluid and lubricants containing other particle additives. By adding 0.5 wt% LDH nanoplatelets, under 1.5 GPa initial contact pressure, the friction coefficient, scar diameter, depth and width of the wear track dramatically decrease by 83.1%, 43.2%, 88.5% and 59.5%, respectively. It is considered that the sufficiently small size and the excellent dispersion of NiAl-LDH/OAm nanoplatelets in water are the key factors, so as to make them enter the contact area, form a lubricating film and prevent direct collision of asperity peaks. Our investigations demonstrate that the LDH nanoplatelet as a water-based lubricant additive has a great potential value in industrial application.

  8. Characterization of a dextran–coated layered double hydroxide acetylsalicylic acid delivery system and its pharmacokinetics in rabbit

    Directory of Open Access Journals (Sweden)

    Li-e Dong

    2013-12-01

    Full Text Available The aim of this study was to prepare a dextran–coated layered double hydroxide acetylsalicylic acid (DEX–LDH–ASA delivery system by co-precipitation of LDH–ASA and its in-situ compositing with DEX. The structure of the system was investigated using X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR and thermogravimetry (TG. Its in vitro drug release properties and in vivo pharmacokinetics in rabbit were also determined. The results show that the DEX–LDH–ASA system retained the crystal structure of LDH–ASA and gave a marked improvement in its dispersion. It also prolonged the release of ASA and shifted the release pattern from first-order to zero-order kinetics. The pharmacokinetics of ASA administered in the DEX–LDH–ASA system to rabbits produced two absorption peaks with a Cmax of 14.8±1.7 mg/L at 2.11±0.69 h and an elimination half-life of 2.25±0.84 h for the first peak. The fact that delivery of ASA in the DEX–LDH–ASA system was sustained with improved bioavailability indicates the potential of the system as a controlled release formulation with application to other drugs.

  9. Influence of Metallic Molar Ratio on the Electron Spin Resonance and Thermal Diffusivity of Zn–Al Layered Double Hydroxide

    Directory of Open Access Journals (Sweden)

    Abdullah Ahmed Ali Ahmed

    2013-01-01

    Full Text Available The coprecipitation method was used to prepare Zn–Al layered double hydroxide (Zn–Al–NO3-LDH at pH 7.5 and different Zn2+/Al3+ molar ratios of 2, 3, 4, 5, and 6. The elemental, structural, and textural properties of prepared samples were studied. The crystallinity of prepared LDH nanostructure decreases as Zn2+/Al3+ molar ratio increases. The electron spin resonance (ESR spectroscopy of different LDH samples showed new ESR spectra. These spectra were produced due to the presence of different phases with formed LDH such as ZnO phase and ZnAl2O4 spinel. At low Zn2+/Al3+ molar ratio, the ESR signals were produced from the presence of free nitrate anions in the LDH interlayer. Above Zn2+/Al3+ = 2, the ESR signals were attributed to the existence of ZnO phase and ZnAl2O4 spinel in the samples. Because the nuclear magnetic moment of 67Zn is lower than 27Al, the increasing in Zn2+/Al3+ molar ratio causes a reduction of the magnetic activity of ZnAl2O4 spinel. Thermal diffusivity versus in situ temperature showed nonlinear relation for different samples due to the changing in the water content of LDH as temperature increases. The dc conductivity of samples decreased as Zn2+/Al3+ molar ratio.

  10. Mechanical and Morphological Properties of Poly-3-hydroxybutyrate/Poly(butyleneadipate-co-terephthalate/Layered Double Hydroxide Nanocomposites

    Directory of Open Access Journals (Sweden)

    Yen Leng Pak

    2013-01-01

    Full Text Available Nanocomposites of poly-3-hydroxybutyrate/poly(butyleneadipate-co-terephthalate/layered double hydroxide (PHB/PBAT/LDH were prepared from a binary blend of PHB/PBAT and stearate-Zn3Al LDH via a solution casting method using chloroform as solvent in this study. The pristine Zn3Al LDH was synthesized from nitrate salts solution at pH 7 by using coprecipitation technique and then was modified by stearate anions surfactant via ion exchange reaction. As a result, the basal spacing of the LDH was increased from 8.77 to 24.94 Å after the modification. Intercalated nanocomposites were formed due to the presence of diffraction peak in XRD diffractograms. The infrared spectrum of stearate-Zn3Al LDH exhibited the existence of stearate anions in the synthesized Zn3Al LDH. Mechanical properties with 2 wt% stearate-Zn3Al LDH loading nanocomposites showed 56 wt% improvements in elongation at break compared to those of the blend.

  11. Highly Enhanced Photoelectrochemical Water Oxidation Efficiency Based on Triadic Quantum Dot/Layered Double Hydroxide/BiVO4 Photoanodes.

    Science.gov (United States)

    Tang, Yanqun; Wang, Ruirui; Yang, Ye; Yan, Dongpeng; Xiang, Xu

    2016-08-03

    The water oxidation half-reaction is considered to be a bottleneck for achieving highly efficient solar-driven water splitting due to its multiproton-coupled four-electron process and sluggish kinetics. Herein, a triadic photoanode consisting of dual-sized CdTe quantum dots (QDs), Co-based layered double hydroxide (LDH) nanosheets, and BiVO4 particles, that is, QD@LDH@BiVO4, was designed. Two sets of consecutive Type-II band alignments were constructed to improve photogenerated electron-hole separation in the triadic structure. The efficient charge separation resulted in a 2-fold enhancement of the photocurrent of the QD@LDH@BiVO4 photoanode. A significantly enhanced oxidation efficiency reaching above 90% in the low bias region (i.e., E < 0.8 V vs RHE) could be critical in determining the overall performance of a complete photoelectrochemical cell. The faradaic efficiency for water oxidation was almost 90%. The conduction band energy of QDs is ∼1.0 V more negative than that of LDH, favorable for the electron injection to LDH and enabling a more efficient hole separation. The enhanced photon-to-current conversion efficiency and improved water oxidation efficiency of the triadic structure may result from the non-negligible contribution of hot electrons or holes generated in QDs. Such a band-matching and multidimensional triadic architecture could be a promising strategy for achieving high-efficiency photoanodes by sufficiently utilizing and maximizing the functionalities of QDs.

  12. Multi-level three-dimensional Mg-Al layered double hydroxide hierarchical microstructures with enhanced basic catalytic property.

    Science.gov (United States)

    Yu, Jiaying; Fan, Guoli; Yang, Yang; Li, Feng

    2014-10-15

    Novel three-dimensional (3D) rosette-like carbonate-type Mg-Al layered double hydroxide (MgAl-LDH) hierarchical microstructures were fabricated successfully by a surfactant-assisted coprecipitation method in the presence of hexamethylenetetramine as precipitant, and the morphology-dependent basic catalytic property was exploited. The morphologies of MgAl-LDH aggregates were diversified depending on the synthesis parameters including the type of precipitant, concentration of sodium stearate surfactant, and hydrothermal aging time. Specifically, the morphology of MgAl-LDH particles could change progressively from platelet-like aggregates to rosette-like microspheres with the increasing concentration of sodium stearate. A possible formation mechanism for special 3D flower-like MgAl-LDH microstructures was proposed based on the synergistic effect of precipitant with surfactant. Moreover, the resulting activated rosette-like MgAl-LDH, which was prepared through calcination-rehydration process, showed a higher catalytic activity in the transesterification of tributyrin with methanol, compared with that derived from the conventional platelet-like MgAl-LDH precursor, which was attributed to its higher specific basicity originating from multi-level hierarchical superstructure offering an advantage in contact with more exposed base sites.

  13. Impact of size, secondary structure, and counterions on the binding of small ribonucleic acids to layered double hydroxide nanoparticles.

    Science.gov (United States)

    Rodriguez, Blanca V; Pescador, Jorge; Pollok, Nicole; Beall, Gary W; Maeder, Corina; Lewis, L Kevin

    2015-12-30

    Use of ribonucleic acid (RNA) interference to regulate protein expression has become an important research topic and gene therapy tool, and therefore, finding suitable vehicles for delivery of small RNAs into cells is of crucial importance. Layered double metal hydroxides such as hydrotalcite (HT) have shown great promise as nonviral vectors for transport of deoxyribose nucleic acid (DNA), proteins, and drugs into cells, but the adsorption of RNAs to these materials has been little explored. In this study, the binding of small RNAs with different lengths and levels of secondary structure to HT nanoparticles has been analyzed and compared to results obtained with small DNAs in concurrent experiments. Initial experiments established the spectrophotometric properties of HT in aqueous solutions and determined that HT particles could be readily sedimented with near 100% efficiencies. Use of RNA+HT cosedimentation experiments as well as electrophoretic mobility shift assays demonstrated strong adsorption of RNA 25mers to HT, with twofold greater binding of single-stranded RNAs relative to double-stranded molecules. Strong affinities were also observed with ssRNA and dsRNA 54mers and with more complex transfer RNA molecules. Competition binding and RNA displacement experiments indicated that RNA-HT associations were strong and were only modestly affected by the presence of high concentrations of inorganic anions.

  14. Sorption Removal of Pb(Ⅱ) from Solution by Uncalcined and Calcined MgAl-Layered Double Hydroxides

    Institute of Scientific and Technical Information of China (English)

    ZHANG, Shu-Qin; HOU, Wan-Guo

    2007-01-01

    Layered double hydroxide (LDH) with a Mg/Al molar ratio of 1∶1 was synthesized by using a co-precipitation method and its calcined product (CLDH) was obtained by calcination of the MgAl-LDH at 500 ℃. The sorption removal of Pb2+ from solution was investigated, finding that both LDH and CLDH show good sorption ability and they could be used as a new type of environmental sorbent for the removal of Pb2+ from water. The sorption kinetics and the sorption isotherms of Pb2+ on both LDH and CLDH can be described by the pseudo-second order kinetics and Freundlich isotherm, respectively, under the studied conditions. The sorption amounts of Pb2+ on LDH and CLDH are independent of pH in a pH range of about 3-10. The presence of NaNO3 may inhibit the sorption of Pb2+ on LDH while hardly affect that on CLDH. The sorption mechanism of Pb2+ on LDH and CLDH may be attributed to the surface precipitation and the surface complex adsorption. The surface complex adsorption may be further distinguished to the chemical binding adsorption forming the inner-sphere surface complexes and the electrostatic binding adsorption forming the outer-sphere surface complexes. The sorption mechanism of Pb2+ on LDH may be attributed to the surface precipitation and the electrostatic binding adsorption, while that on CLDH may be attributed to the surface precipitation and the chemical binding adsorption.

  15. Improvement of pharmacokinetic and antitumor activity of layered double hydroxide nanoparticles by coating with PEGylated phospholipid membrane

    Directory of Open Access Journals (Sweden)

    Yan MN

    2014-10-01

    Full Text Available Mina Yan,1,2 Zhaoguo Zhang,2 Shengmiao Cui,3 Ming Lei,2 Ke Zeng,2 Yunhui Liao,2 Weijing Chu,2 Yihui Deng,1 Chunshun Zhao2 1School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, People’s Republic of China; 2School of Pharmaceutical Sciences, Sun Yat-sen University, 3Guangdong Pharmaceutical University, Guangzhou, People’s Republic of China Abstract: Layered double hydroxide (LDH has attracted considerable attention as a drug carrier. However, because of its poor in vivo behavior, polyethylene glycolylated (PEGylated phospholipid must be used as a coformer to produce self-assembled core–shell nanoparticles. In the present study, we prepared a PEGylated phospholipid-coated LDH (PLDH (PEG-PLDH delivery system. The PEG-PLDH nanoparticles had an average size of 133.2 nm. Their core–shell structure was confirmed by transmission electron microscopy and X-ray photoelectron spectroscopy. In vitro liposome-cell-association and cytotoxicity experiments demonstrated its ability to be internalized by cells. In vivo studies showed that PEGylated phospholipid membranes greatly reduced the blood clearance rate of LDH nanoparticles. PEG-PLDH nanoparticles demonstrated a good control of tumor growth and increased the survival rate of mice. These results suggest that PEG-PLDH nanoparticles can be a useful drug delivery system for cancer therapy. Keywords: lipid membrane, positive charge, delivery system, cancer therapy

  16. Synthesis, Characterization, and In Vitro Drug Delivery Capabilities of (Zn, Al-Based Layered Double Hydroxide Nanoparticles

    Directory of Open Access Journals (Sweden)

    Vinay J. Nagaraj

    2015-01-01

    Full Text Available There is an urgent need for the development of alternative strategies for effective drug delivery to improve the outcome of patients suffering from deadly diseases such as cancer. Nanoparticles, in particular layered double hydroxide (LDH nanoparticles, have great potential as nanocarriers of chemotherapeutic molecules. In this study, we synthesized (Zn, Al-LDH nanoparticles and report their enhanced pH-dependent stability in comparison to the commonly used (Mg, Al-LDH nanoparticles. Fluorescein isothiocyanate (FITC and valproate (VP were intercalated into (Zn, Al-LDH nanoparticles to study cellular uptake, biocompatibility, and drug delivery capabilities using cultured pancreatic adenocarcinoma BxPC3 cells. Fluorescence measurements indicated that FITC-intercalated LDH nanoparticles showed a greater degree of energy-dependent uptake rather than passive uptake by BxPC3 cells, especially at high concentrations of nanoparticles. Tetrazolium-based colorimetric assays indicated that BxPC3 cells treated with VP-intercalated LDH nanoparticles showed a significant reduction in cell viability along with about 30-fold reduction in IC50 compared to the drug alone. In contrast, the non-drug-intercalated LDH nanoparticles did not affect the cell viability indicating very low innate cytotoxicity. Our research indicates that the superior properties of (Zn, Al-LDH nanoparticles make them ideal candidates for further development as in vivo chemotherapy drug delivery agents.

  17. Precursor preparation for Ca-Al layered double hydroxide to remove hexavalent chromium coexisting with calcium and magnesium chlorides

    Science.gov (United States)

    Zhong, Lihua; He, Xiaoman; Qu, Jun; Li, Xuewei; Lei, Zhiwu; Zhang, Qiwu; Liu, Xinzhong

    2017-01-01

    Al(OH)3 and Ca(OH)2 powders are co-ground to prepare a precursor which hydrates into a layered double hydroxide (LDH) phase by agitation in aqueous solution with target hexavalent chromium (Cr(VI)) at room temperature, to achieve an obvious improvement in removal efficiency of Cr(VI) through an easy incorporation into the structure. Although the prepared precursor transforms into LDH phases also when agitated in the solutions of calcium and magnesium chlorides, it incorporates Cr(VI) preferentially to the chloride salts when they coexist. The adsorption isotherm and kinetic studies show that the phenomena occurring on the Al-Ca precursor fit a pseudo-second-order kinetics with a Langmuir adsorption capacity of 59.45 mg/g. Besides, characterizations of the prepared precursor and the samples after adsorption are also performed by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscope (TEM) to understand the reason of the preferential incorporation of Cr(VI) to the coexisting chloride salts during the LDH phase formation.

  18. Effect of Electrolytes and Polymers on the Thixotropy of Mg-AI-Layered Double Hydroxides/Kaolinite Dispersions

    Institute of Scientific and Technical Information of China (English)

    戴肖南; 侯万国; 段洪东

    2011-01-01

    The effect of electrolytes (NaCl and CaCl2) and polymers (CPAM and HPAM) on the thixotropy of Mg-Al-layered double hydroxide (LDHs)/kaolinite dispersions has been investigated. It was observed that the type of thixotropy in LDH/kaolinite dispersions may be affected by NaCl, but not by CaCl2 in range of concentration of interest. The type of thixotropy in LDH/kaolinite dispersion with R=0 transformed from positive thixotropy to complex thixotropy and at last positive thixotropy again with the concentration of NaC1 in range of 0.00-0.10 mol·L^-1; the type of thixotropy in LDHs/kaolinite dispersions with R = 0.25 transformed from complex thixotropy to positive thixotropy and then complex thixotropy again with the concentration of NaC1 in range of 0.00-0.10 mol·L^-. The type of thixotropy in LDH/kaolinite dispersion with R=0 may be not affected by cationic polyacrylamide (CPAM) and hydrolyzed polyacrylamide (HPAM); but the LDHs/kaolinite dispersions with R=0.25 transformed from complex thixotropy to positive thixotropy with the both polymers concentration in range of interest, which indicated that the microstructure of the dispersion changed from weak folc sediments structure to steric network structure.

  19. Ag/AgBr/Co-Ni-NO3 layered double hydroxide nanocomposites with highly adsorptive and photocatalytic properties.

    Science.gov (United States)

    Fan, Hai; Zhu, Jianying; Sun, Jianchao; Zhang, Shenxiang; Ai, Shiyun

    2013-02-11

    A facile anion-exchange precipitation method was used to synthesize bifunctional Ag/AgBr/Co-Ni-NO(3) layered double hydroxide (LDH) nanocomposites by adding AgNO(3) solution to a suspension of Co-Ni-Br LDH. The Ag/AgBr nanoparticles were highly dispersed on the sheets of Co-Ni-NO(3) LDH. The prepared nanocomposites were used to adsorb and photocatalytically degrade organic pollutants from water. Without light illumination, the nanocomposites quickly adsorbed methyl orange, and the adsorptive capacity, which can reach 230 mg g(-1), is much higher than those of Co-Ni-Br LDH, Ag/AgBr, and activated carbon. The photocatalytic activities of the nanocomposites for the removal of dyes and phenol are higher than those of Co-Ni-Br LDH and Ag/AgBr. The proposed method can be applied to prepare other LDH/silver salt composites. The high absorptive capacity and good photocatalytic activity of such nanostructures could have wide applications in wastewater treatment.

  20. In vitro antioxidant activity and in vivo antifatigue effect of layered double hydroxide nanoparticles as delivery vehicles for folic acid

    Directory of Open Access Journals (Sweden)

    Qin LL

    2014-12-01

    Full Text Available Lili Qin,1,* Wenrui Wang,2,* Songhui You,1 Jingmei Dong,1 Yunhe Zhou,1 Jibing Wang1 1Department of Physical Education, 2School of Life Science and Technology, Tongji University, Shanghai, People’s Republic of China *These authors contributed equally to this work Abstract: Folic acid antioxidants were successfully intercalated into layered double hydroxides (LDH nanoparticles according to a previous method with minor modification. The resultant folic acid-LDH constructs were then characterized by X-ray powder diffraction and transmission electron microscopy. The in vitro antioxidant activities, cytotoxicity effect, and in vivo anti­fatigue were examined by a series of assays. The results showed that folic acid-LDH antioxidant system can scavenge 1,1-diphenyl-2-picrylhydrazyl and hydroxyl free radicals and chelate pro-oxidative Cu2+. The in vitro cytotoxicity assays indicated that folic acid-LDH antioxidant system had no significant cytotoxic effect or obvious toxicity to normal cells. It also prolonged the forced swimming time of the mice by 32% and 51% compared to folic acid and control groups, respectively. It had an obvious effect on decreasing the blood urea nitrogen and blood lactic acid, while increasing muscle and hepatic glycogen levels. Therefore, folic acid-LDH might be used as a novel antioxidant and antifatigue nutritional supplement. Keywords: antioxidant supplementation, free radicals, biomaterials, drug delivery

  1. Coagulation Behavior of Graphene Oxide on Nanocrystallined Mg/Al Layered Double Hydroxides: Batch Experimental and Theoretical Calculation Study.

    Science.gov (United States)

    Zou, Yidong; Wang, Xiangxue; Ai, Yuejie; Liu, Yunhai; Li, Jiaxing; Ji, Yongfei; Wang, Xiangke

    2016-04-01

    Graphene oxide (GO) has attracted considerable attention because of its remarkable enhanced adsorption and multifunctional properties. However, the toxic properties of GO nanosheets released into the environment could lead to the instability of biological system. In aqueous phase, GO may interact with fine mineral particles, such as chloridion intercalated nanocrystallined Mg/Al layered double hydroxides (LDH-Cl) and nanocrystallined Mg/Al LDHs (LDH-CO3), which are considered as coagulant molecules for the coagulation and removal of GO from aqueous solutions. Herein the coagulation of GO on LDHs were studied as a function of solution pH, ionic strength, contact time, temperature and coagulant concentration. The presence of LDH-Cl and LDH-CO3 improved the coagulation of GO in solution efficiently, which was mainly attributed to the surface oxygen-containing functional groups of LDH-Cl and LDH-CO3 occupying the binding sites of GO. The coagulation of GO by LDH-Cl and LDH-CO3 was strongly dependent on pH and ionic strength. Results of theoretical DFT calculations indicated that the coagulation of GO on LDHs was energetically favored by electrostatic interactions and hydrogen bonds, which was further evidenced by FTIR and XPS analysis. By integrating the experimental results, it was clear that LDH-Cl could be potentially used as a cost-effective coagulant for the elimination of GO from aqueous solutions, which could efficiently decrease the potential toxicity of GO in the natural environment.

  2. In Situ Transformation of MOFs into Layered Double Hydroxide Embedded Metal Sulfides for Improved Electrocatalytic and Supercapacitive Performance.

    Science.gov (United States)

    Yilmaz, Gamze; Yam, Kah Meng; Zhang, Chun; Fan, Hong Jin; Ho, Ghim Wei

    2017-07-01

    Direct adoption of metal-organic frameworks (MOFs) as electrode materials shows impoverished electrochemical performance owing to low electrical conductivity and poor chemical stability. In this study, we demonstrate self-templated pseudomorphic transformation of MOF into surface chemistry rich hollow framework that delivers highly reactive, durable, and universal electrochemically active energy conversion and storage functionalities. In situ pseudomorphic transformation of MOF-derived hollow rhombic dodecahedron template and sulfurization of nickel cobalt layered double hydroxides (NiCo-LDHs) lead to the construction of interlayered metal sulfides (NiCo-LDH/Co9 S8 ) system. The embedment of metal sulfide species (Co9 S8 ) at the LDH intergalleries offers optimal interfacing of the hybrid constituent elements and materials stability. The hybrid NiCo-LDH/Co9 S8 system collectively presents an ideal porous structure, rich redox chemistry, and high electrical conductivity matrix. This leads to a significant enhancement in its complementary electrocatalytic hydrogen evolution and supercapacitive energy storage properties. This work establishes the potential of MOF derived scaffold for designing of novel class hybrid inorganic-organic functional materials for electrochemical applications and beyond. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Synthesis and Characteristics of Valeric Acid-Zinc Layered Hydroxide Intercalation Material for Insect Pheromone Controlled Release Formulation

    Directory of Open Access Journals (Sweden)

    Rozita Ahmad

    2016-01-01

    Full Text Available A new intercalation compound of insect pheromone, valeric acid (VA, based on zinc layered hydroxide (ZLH as host release material, was successfully prepared through coprecipitation method. The as-produced organic-inorganic nanolayered material, valerate nanohybrid, VAN, shows the formation of a new peak at lower 2θ angle with basal spacing of 19.8 Å with no ZnO reflections, which indicate that the intercalation of anion between the inorganic ZLH interlamellae was accomplished. The elemental, FTIR, and ATR analyses of the nanohybrid supported the fact that the intercalation with the percentage anion loading was calculated to be 23.0% (w/w. The thermal stability property of the resulting nanohybrid was enhanced compared to the unbound anion. Field emission scanning electron micrograph of the ZnO has a nonuniform granular structure but transforms into flake-like structure with various sizes after the intercalation process. Release kinetics of anion from the interlayer of intercalated compound exhibited a slow release behavior governed by the pseudo-second-order kinetic model at different pHs of aqueous media. The valerate anion was released from VAN with the highest release rate at pH 4. These findings provide the basis to further development of controlled release formulation for insect pheromone based on ZLH intercalation.

  4. Enhancement photocatalytic degradation of rhodamine B on nanoPt intercalated Zn–Ti layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Guixiang; Qian, Shengming; Tu, Xinman, E-mail: tuxinman@126.com; Wei, Xiaoyong; Zou, Jianping; Leng, Lehui; Luo, Shenglian, E-mail: sllou@hnu.edu.cn

    2014-02-28

    NanoPt intercalated Zn–Ti layered double hydroxides (LDHs) have been synthesized by ionic exchange and photochemical reduction method from Zn–Ti LDHs in H{sub 2}PtCl{sub 6} solution. X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), N{sub 2} adsorption at 77 K, UV–vis analysis and the electrochemical impedance were adopted to investigate the structure, surface, micromorphology, photoresponsive and electrochemical properties of the as-synthesized samples. The combination of Zn–Ti-LDHs and Pt introduces some properties of Pt into photocatalysis such as excellent conductivity and controllability. Remarkable 17-fold enhancement in the degradation of rhodamine B (RhB) reaction was observed on as-prepared Pt/Zn–Ti LDHs compared with pure Zn–Ti LDHs under simulated sunlight irradiation. The enhanced photocatalytic activity could be attributed to high specific surface (111.46 m{sup 2}/g), extended photoresponding range, the negative shift in the flat-band potentials and the high migration efficiency of photoinduced electrons, which may suppress the charge recombination effectively.

  5. A solid state NMR study of layered double hydroxides intercalated with para-amino salicylate, a tuberculosis drug

    DEFF Research Database (Denmark)

    Jensen, Nicholai Daugaard; Bjerring, Morten; Nielsen, Ulla Gro

    2016-01-01

    Para-amino salicylate (PAS), a tubercolosis drug, was intercalated in three different layered double hydroxides (MgAl, ZnAl, and CaAl-LDH) and the samples were studied by multi-nuclear (1H, 13C, and 27Al) solid state NMR (SSNMR) spectroscopy in combination with powder X-ray diffraction (PXRD......), elemental analysis and IR-spectroscopy to gain insight into the bulk and atomic level structure of these LDHs especially with a view to the purity of the LDH-PAS materials and the concentration of impurities. The intercalations of PAS in MgAl-, ZnAl-, and CaAl-LDH's were confirmed by 13C SSNMR and PXRD...... showed that the M(II):Al ratio was higher than predicted from the bulk metal composition of MgAl-PAS and ZnAl-PAS. Moreover, the first high-resolution 1H SSNMR spectra of a CaAl LDH is reported and assigned using 1H single and double quantum experiments in combination with 27Al{1H} HETCOR....

  6. Synthesis and characterization of Zn-Ti layered double hydroxide intercalated with cinnamic acid for cosmetic application

    Science.gov (United States)

    Li, Yong; Tang, Liping; Ma, Xinxu; Wang, Xinrui; Zhou, Wei; Bai, Dongsheng

    2017-08-01

    The use of sunscreen is recently growing and their efficacy and safety must be taken into account since they are applied on the skin frequently. In this work, an organic ultraviolet (UV) ray absorbent, cinnamic acid (CA) was intercalated into Zn-Ti layered double hydroxide (LDH) by anion-exchange reaction. ZnTi-CA-LDH, a new type of host-guest UV-blocking material has been synthesized. Detailed structural and surface morphology of ZnTi-CA-LDH were characterized by XRD, FT-IR, SEM and TEM. ZnTi-CA-LDH exhibits a superior UV blocking ability compared to pure CA and ZnTi-CO3-LDH. The thermal stability of the intercalated ZnTi-CA-LDH was investigated by TG-DTA, which showed that the thermostability of CA was markedly enhanced after intercalation into ZnTi-CO3-LDH. The EPR data showed greatly decreased photocatalytic activity compared to common inorganic UV blocking agents TiO2 and ZnO. Furthermore, the sample was formulated in a sunscreen cream to study the matrix protective effect towards UV rays.

  7. Effect of rare Earth ions on the properties of composites composed of ethylene vinyl acetate copolymer and layered double hydroxides.

    Directory of Open Access Journals (Sweden)

    Lili Wang

    Full Text Available BACKGROUND: The study on the rare earth (RE-doped layered double hydroxides (LDHs has received considerable attention due to their potential applications in catalysts. However, the use of RE-doped LDHs as polymer halogen-free flame retardants was seldom investigated. Furthermore, the effect of rare earth elements on the hydrophobicity of LDHs materials and the compatibility of LDHs/polymer composite has seldom been reported. METHODOLOGY/PRINCIPAL FINDINGS: The stearate sodium surface modified Ni-containing LDHs and RE-doped Ni-containing LDHs were rapidly synthesized by a coprecipitation method coupled with the microwave hydrothermal treatment. The influences of trace amounts of rare earth ions La, Ce and Nd on the amount of water molecules, the crystallinity, the morphology, the hydrophobicity of modified Ni-containing LDHs and the adsorption of modifier in the surface of LDHs were investigated by TGA, XRD, TEM, contact angle and IR, respectively. Moreover, the effects of the rare earth ions on the interfacial compatibility, the flame retardancy and the mechanical properties of ethylene vinyl acetate copolymer (EVA/LDHs composites were also explored in detail. CONCLUSIONS/SIGNIFICANCE: S-Ni₀.₁MgAl-La displayed more uniform dispersion and better interfacial compatibility in EVA matrix compared with other LDHs. Furthermore, the S-Ni₀.₁MgAl-La/EVA composite showed the best fire retardancy and mechanical properties in all composites.

  8. Layered double hydroxide nanoparticles promote self-renewal of mouse embryonic stem cells through the PI3K signaling pathway

    Science.gov (United States)

    Wu, Youjun; Zhu, Rongrong; Zhou, Yang; Zhang, Jun; Wang, Wenrui; Sun, Xiaoyu; Wu, Xianzheng; Cheng, Liming; Zhang, Jing; Wang, Shilong

    2015-06-01

    Embryonic stem cells (ESCs) hold great potential for regenerative medicine due to their two unique characteristics: self-renewal and pluripotency. Several groups of nanoparticles have shown promising applications in directing the stem cell fate. Herein, we investigated the cellular effects of layered double hydroxide nanoparticles (LDH NPs) on mouse ESCs (mESCs) and the associated molecular mechanisms. Mg-Al-LDH NPs with an average diameter of ~100 nm were prepared by hydrothermal methods. To determine the influences of LDH NPs on mESCs, cellular cytotoxicity, self-renewal, differentiation potential, and the possible signaling pathways were explored. Evaluation of cell viability, lactate dehydrogenase release, ROS generation and apoptosis demonstrated the low cytotoxicity of LDH NPs. The alkaline phosphatase activity and the expression of pluripotency genes in mESCs were examined, which indicated that exposure to LDH NPs could support self-renewal and inhibit spontaneous differentiation of mESCs under feeder-free culture conditions. The self-renewal promotion was further proved to be independent of the leukemia inhibitory factor (LIF). Furthermore, cells treated with LDH NPs maintained the potential to differentiate into all three germ layers both in vitro and in vivo through formation of embryoid bodies and teratomas. In addition, we observed that LDH NPs initiated the activation of the PI3K/Akt pathway, while treatment with the PI3K inhibitor LY294002 could block the effects of LDH NPs on mESCs. The results confirmed that the promotion of self-renewal by LDH NPs was associated with activation of the PI3K/Akt signaling pathway. Altogether, our studies identified a new role of LDH NPs in maintaining self-renewal of mouse ES cells which could potentially be applied in stem cell research.Embryonic stem cells (ESCs) hold great potential for regenerative medicine due to their two unique characteristics: self-renewal and pluripotency. Several groups of nanoparticles

  9. Uptake and Speciation of Inorganic Arsenic with Cellulose Fibre Coated with Yttrium Hydroxide Layer as a Novel Green Sorbent

    Institute of Scientific and Technical Information of China (English)

    安明日; 张晓星; 杨婷; 陈明丽; 王建华

    2012-01-01

    A novel adsorbent was developed by coating yttrium hydroxide precipitate layer on cellulose fibre. This material takes up ca. 98% of 5 μg·L 1 As(Ⅲ) and As(V) at low pH (pH〈7), while a favorable selectivity for As(V) was achieved within pH 11--12. In practice, a mini-column packed with Y(OH)3 precipitate layer coated cellulose fibre particles was incorporated into a sequential injection system for selective uptake of arsenate at pH 11.5. The retained arsenate was afterwards recovered with 50μL of 0.8 mol.L l NaOH solution as eluent, followed by hydride generation in a reaction medium of 2.0 mol·L-1 HCl and 1.0% NaBH4 solution (W/V, in 0.5% NaOH) after pre-reduction of arsenate to arsenite by KI-ascorbic acid (5%, W/V), with detection by atomic fluorescence spec- trometry. Total inorganic arsenic was quantitatively taken up at pH 6.0 by following the same procedure and arsenic speciation was performed by difference. With a sample volume of 1.0 mL, an enrichment factor of 16.4 was derived with a detection limit of 17 ng.L-1 within a linear range of 0.05--2.0μg.L ]. A relative standard deviation (RSD) of 2.6% (0.5 μg·L-1, n= 11) was achieved. The procedure was validated by analyzing arsenic in a certified refer- ence material GBW 09101 (human hair), and speciation process requires no organic solvents, thus Y(OH)3 coated of inorganic arsenic in natural water samples. The entire cellulose fibre provides a green adsorbent.

  10. Two-Dimensional Layered Double Hydroxide Derived from Vermiculite Waste Water Supported Highly Dispersed Ni Nanoparticles for CO Methanation

    Directory of Open Access Journals (Sweden)

    Panpan Li

    2017-03-01

    Full Text Available Expanded multilayered vermiculite (VMT was successfully used as catalyst support and Ni/VMT synthesized by microwave irradiation assisted synthesis (MIAS exhibited excellent performance in our previous work. We also developed a two-dimensional porous SiO2 nanomesh (2D VMT-SiO2 by mixed-acid etching of VMT. Compared with three-dimensional (3D MCM-41, 2D VMT-SiO2 as a catalyst support provided a superior position for implantation of NiO species and the as-obtained catalyst exhibited excellent performance. In this paper, we successfully synthesized a layered double hydroxide (LDH using the spent liquor after mixed-acid etching of VMT, which mainly contained Mg2+ and Al3+. The as-calcined layered double oxide (LDO was used as a catalyst support for CO methanation. Compared with Ni/MgAl-LDO, Ni/VMT-LDO had smaller active component particles; therefore, in this study, it exhibited excellent catalytic performance over the whole temperature range of 250–500 °C. Ni/VMT-LDO achieved the best activity with 87.88% CO conversion, 89.97% CH4 selectivity, and 12.47 × 10−2·s−1 turn over frequency (TOF at 400 °C under a gas hourly space velocity of 20,000 mL/g/h. This study demonstrated that VMT-LDO as a catalyst support provided an efficient way to develop high-performance catalysts for synthetic natural gas (SNG from syngas.

  11. Synthesis of carbon nanotube/layered double hydroxide nanocomposite as a novel fiber coating for the headspace solid-phase microextraction of phenols from water samples.

    Science.gov (United States)

    Abolghasemi, Mir Mahdi; Yousefi, Vahid; Piryaei, Marzieh

    2015-05-01

    In this research, a carbon nanotube/layered double hydroxide nanocomposite was synthesized by an in situ growth route by electrostatic force. The prepared carbon nanotube/layered double hydroxide nanocomposite was successfully prepared and deposited on a stainless-steel wire for the fabrication of the solid-phase microextraction fiber. The fiber was evaluated for the extraction of phenolic compounds from water samples. Analytical merits of the method, under optimum conditions (extraction temperature: 75°C, extraction time: 30 min, desorption time: 2 min, desorption temperature 260°C, salt concentration: 10% w/v) are 0.01-300 ng/mL for the linear dynamic range and 0.005-0.08 for the limit of detection. In optimum conditions, the repeatability for one fiber (n = 3), expressed as relative standard deviation, was between 6.5 and 9.9% for the phenolic compounds.

  12. Effect of reaction time and (Ca+Mg)/Al molar ratios on crystallinity of Ca-Mg-Al layered double Hydroxide

    Science.gov (United States)

    Heraldy, E.; Nugrahaningtyas, K. D.; Sanjaya, F. B.; Darojat, A. A.; Handayani, D. S.; Hidayat, Y.

    2016-02-01

    Ca-Mg-Al Layered Double Hydroxides (Ca-Mg-Al-LDH) compounds were successfully synthesized from brine water and AlCl3.6H2O as the starting materials by coprecipitation method. The product result was characterized by X-ray powder diffraction (XRD) and Fourier transform infrared (FT-IR). The effects of the reaction time and the molar ratios of the raw material on the crystallinity of Ca-Mg-Al-LDH were examining. Results show that increasing reaction time (30; 60 and 90 min.) could improve the crystallinity and monodispersity of layered double hydroxide compounds particles. The well-defined Ca-Mg- Al-LDH could be prepared with (Ca+Mg)/Al molar ratios 0.5.

  13. Preparation of Tween 80-Zn/Al-levodopa-layered double hydroxides nanocomposite for drug delivery system.

    Science.gov (United States)

    Kura, Aminu Umar; Hussein-Al-Ali, Samer Hasan; Hussein, Mohd Zobir; Fakurazi, Sharida

    2014-01-01

    We incorporated anti-Parkinsonian drug, levodopa (dopa), in Zn/Al-LDH by coprecipitation method to form dopa-LDH nanocomposite. Further coating of Tween-80 on the external surfaces of dopa-LDH nanocomposite was achieved through the oxygen of C=O group of Tween-80 with the layer of dopa-LDH nanocomposite. The final product is called Tween-dopa-LDH nanocomposite. The X-ray diffraction indicates that the Tween-dopa-LDH nanocomposite was formed by aggregation structure. From the TGA data, the Tween-80 loading on the surface of LDH and dopa-LDH was 8.6 and 7.4%, respectively. The effect of coating process on the dopa release from Tween-dopa-LDH nanocomposite was also studied. The release from Tween-dopa-LDH nanocomposite shows slower release compared to the release of the drug from dopa-LDH nanocomposite as done previously in our study, presumably due to the retarding shielding effect. The cell viability study using PC12 showed improved viability with Tween-80 coating on dopa-LDH nanocomposite as studied by mitochondrial dehydrogenase activity (MTT assay).

  14. Catalytic characterization of bi-functional catalysts derived from Pd–Mg–Al layered double hydroxides

    Indian Academy of Sciences (India)

    N N Das; S C Srivastava

    2002-08-01

    Hydrotalcite like precursors containing PdII–MgII–AlIII with varying molar ratios, (Pd + Mg)/Al ≈ 3 and Mg/Pd ≈ 750 to 35, were prepared by coprecipitation of metal nitrates at constant pH. Characterization of samples as synthesized and their calcined products by elemental analyses, powder XRD, TG–DTA, FT–IR spectroscopy, TPR and N2 physisorption indicated a well crystalline hydrotalcite like structure with incorporation of Pd2+ in the brucite layers. Thermal decomposition of hydrotalcite precursors at intermediate temperatures led to amorphous mixed oxides, Pd/MgAl(O), which on reduction yielded bi-functional catalyst, Pd°/MgAl(O). The resultant catalysts with acid, base and hydrogenating sites, were highly active and selective for one-step synthesis of methyl isobutyl ketone (MIBK) from acetone and hydrogen. The results showed an optimal balance between acid-base and metallic sites were required to increase the selectivity of MIBK and stability of the catalysts.

  15. Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy

    DEFF Research Database (Denmark)

    Boisen Staal, Line; Lipton, Andrew S.; Zorin, Vadim

    2014-01-01

    Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle...

  16. Comparative study of Mg/Al- and Zn/Al-layered double hydroxide-perindopril erbumine nanocomposites for inhibition of angiotensin-converting enzyme

    Directory of Open Access Journals (Sweden)

    Hussein Al Ali SH

    2012-08-01

    Full Text Available Samer Hasan Hussein Al Ali,1 Mothanna Al-Qubaisi,2 Mohd Zobir Hussein,1,3 Maznah Ismail,2,4 Zulkarnain Zainal,1 Muhammad Nazrul Hakim51Department of Chemistry, Faculty of Science, 2Laboratory of Molecular Biomedicine, Institute of Bioscience, 3Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, 4Department of Nutrition and Health Science, 5Department of Biomedical Science, Faculty of Medicine and Health Science, Universiti Putra Malaysia, Selangor, MalaysiaAbstract: The intercalation of a drug active, perindopril, into Mg/Al-layered double hydroxide for the formation of a new nanocomposite, PMAE, was accomplished using a simple ion exchange technique. A relatively high loading percentage of perindopril of about 36.5% (w/w indicates that intercalation of the active took place in the Mg/Al inorganic interlayer. Intercalation was further supported by Fourier transform infrared spectroscopy, and thermal analysis shows markedly enhanced thermal stability of the active. The release of perindopril from the nanocomposite occurred in a controlled manner governed by pseudo-second order kinetics. MTT assay showed no cytotoxicity effects from either Mg/Al-layered double hydroxide or its nanocomposite, PMAE. Mg/Al-layered double hydroxide showed angiotensin-converting enzyme inhibitory activity, with 5.6% inhibition after 90 minutes of incubation. On incubation of angiotensin-converting enzyme with 0.5 µg/mL of the PMAE nanocomposite, inhibition of the enzyme increased from 56.6% to 70.6% at 30 and 90 minutes, respectively. These results are comparable with data reported in the literature for Zn/Al-perindopril.Keywords: magnesium, aluminum, layered double hydroxide, perindopril erbumine, ion exchange, angiotensin-converting enzyme, Chang cells line

  17. Insights into the Synthesis of Layered Double Hydroxide (LDH) Nanoparticles: Part 1. Optimization and Controlled Synthesis of Chloride-Intercalated LDH

    OpenAIRE

    Sun, Xiaodi; Neuperger, Erica; Dey, Sandwip K.

    2015-01-01

    Layered double hydroxide (LDH) nanoparticles have excellent anion-intercalating property, and their potential as theranostic nanovectors is high. However, understanding of the control of the mean particle size (MPS) and achievement of monodispersed particle size distribution (PSD) remains elusive. Herein, with the aid of statistical design of experiments on a model system of Cl−-intercalated (Zn, Al)-LDH, controlled synthesis of single crystalline nanoparticles using the coprecipitation metho...

  18. Nitrogen-enriched, double-shelled carbon/layered double hydroxide hollow microspheres for excellent electrochemical performance

    Science.gov (United States)

    Xu, Jie; He, Fei; Gai, Shili; Zhang, Shenghuan; Li, Lei; Yang, Piaoping

    2014-08-01

    A unique, double-shelled, hollow, carbon-based composite with enriched nitrogen has been prepared through a facile and versatile synthetic strategy. The hierarchical composite employs the nitrogen-enriched carbon hollow sphere as an interior shell and intercrossed Ni/Al layered double hydroxide (LDH) nanosheets as an exterior shell. The obtained N-C@LDH hollow microspheres (HMS) have high nitrogen enrichment, large specific surface area (337 m2 g-1), and uniform and open mesoporous structure. Taking advantage of these characteristics, the composite exhibits obviously superior capacitive behavior, including high specific capacitance, excellent rate capability and good cycling stability, compared with nitrogen-free carbon@LDH composite and hollow LDH without carbon shell. The composite displays high specific capacitance of 1711.51 F g-1 at a current density of 1 A g-1. In particular, the high specific capacitance can be kept to 997.3 F g-1 at a high current density of 10 A g-1, which still retains 94.97% of the initial specific capacitance after 500 cycles at this high current density. This N-enriched, hollow carbon/LDH composite can be expected to be a promising electrode material for electrochemical capacitors due to its high electrochemical performance.A unique, double-shelled, hollow, carbon-based composite with enriched nitrogen has been prepared through a facile and versatile synthetic strategy. The hierarchical composite employs the nitrogen-enriched carbon hollow sphere as an interior shell and intercrossed Ni/Al layered double hydroxide (LDH) nanosheets as an exterior shell. The obtained N-C@LDH hollow microspheres (HMS) have high nitrogen enrichment, large specific surface area (337 m2 g-1), and uniform and open mesoporous structure. Taking advantage of these characteristics, the composite exhibits obviously superior capacitive behavior, including high specific capacitance, excellent rate capability and good cycling stability, compared with nitrogen

  19. ZnO/Mg-Al Layered Double Hydroxides as a Photocatalytic Bleaching of Methylene Orange - A Black Box Modeling by Artificial Neural Network

    Directory of Open Access Journals (Sweden)

    Seyed Ali Hosseini

    2016-10-01

    Full Text Available The paper reports the development of ZnO-MgAl layered double hydroxides as an adsorbent-photo catalyst to remove the dye pollutants from aqueous solution and the experiments of a photocatalytic study were designed and modeled by response surface methodology (RSM and artificial neural network (ANN. The co-precipitation and urea methods were used to synthesize the ZnO-MgAl layered double hydroxides and FT-IR, XRD and SEM analysis were done for characterization of the catalyst.The performance of the ANN model was determined and showed the efficiency of the model in comparison to the RSM method to predict the percentage of dye removal accurately with a determination coefficient (R2 of 0.968. The optimized conditions were obtained as follows: 600 oC, 120 min, 0.05 g and 20 ppm for the calcination temperature, irradiation time, catalyst amount and dye pollutant concentration, respectively. Copyright © 2016 BCREC GROUP. All rights reserved Received: 22nd January 2016; Revised: 14th March 2016; Accepted:15th March 2016 How to Cite: Hosseini, S.A., Akbari, M. (2016. ZnO/Mg-Al Layered Double Hydroxides as a Photocatalytic Bleaching of Methylene Orange - A Black Box Modeling by Artificial Neural Network. Bulletin of Chemical Reaction Engineering & Catalysis, 11 (3: 299-315 (doi: 10.9767/bcrec.11.3.570.299-315 Permalink/DOI: http://doi.org/10.9767/bcrec.11.3.570.299-315

  20. Improving the low-temperature capacitance of CoNiAl three-component layered double hydroxide in a redox electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Su, Linghao, E-mail: qauslh@163.com; Song, Zuwei; Lu, Lihua; Pang, Guanglong

    2013-09-01

    Graphical abstract: The specific capacitance of CoNiAl layered double hydroxide in 6 M KOH reduces sharply from room temperature to −20 °C, which is effectively enhanced by adding redox pair Fe(CN){sub 6}{sup 3−}/Fe(CN){sub 6}{sup 4−} in the electrolyte. - Highlights: • CoNiAl layered double hydroxide is synthesized by homogeneous precipitation. • The specific capacitance reduces sharply with the decrease of temperature. • At −20 °C the specific capacitance is increased by 178% in a redox electrolyte. - Abstract: CoNiAl three-component layered double hydroxide with a lamellar structure similar to hydrotalcite-like compounds is synthesized via homogeneous precipitation and the effect of temperature on its capacitive performances in 6 M KOH is investigated. Electrochemical tests show its specific capacitance reduces sharply with the decrease of temperature from 18 to −20 °C. At −20 °C an increase of specific capacitance by 178% is achieved by adding redox pair Fe(CN){sub 6}{sup 3−}/Fe(CN){sub 6}{sup 4−} as the electron shuttle in the electrolyte due to their cooperation with the electrode reaction during the charge/discharge processes.

  1. Preparation of single phase Zn2TiO4 spinel from a new ZnTi layered double hydroxide precursor.

    Science.gov (United States)

    Song, Jianye; Leng, Mingzhe; Xiao, Hongdi; Zhang, Liangji; Qin, Yaowei; Hou, Wanguo; Du, Na; Liu, Jianqiang

    2014-06-01

    A single-source ZnTi-layered double hydroxide precursor was used to prepare single phase Zn2TiO4. This approach involves two steps: the calcination of a ZnTi-layered double hydroxide precursor and selective leaching zinc oxide from the resultant calcined products. The materials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) thermogravimetric and differential thermal analysis (TG-DTA), transmission electron microscope (TEM), surface area measurement and UVvis diffuse reflection spectroscopy. The results indicated that a single phase Zn2TiO4 could be successfully obtained from a ZnTi-layered double hydroxide precursor at a relatively low temperature in short calcination time. The TEM and SEM show that the diameter of Zn2TiO4 particles prepared at 900 degrees C is in the range of 20-100 nm and smaller than that prepared by the solid-state method. UV-Vis diffuse reflection spectroscopy demonstrates that the material has an energy bandgap around 3.7 eV.

  2. Comparative study of Mg/Al- and Zn/Al-layered double hydroxide-perindopril erbumine nanocomposites for inhibition of angiotensin-converting enzyme.

    Science.gov (United States)

    Hussein Al Ali, Samer Hasan; Al-Qubaisi, Mothanna; Hussein, Mohd Zobir; Ismail, Maznah; Zainal, Zulkarnain; Hakim, Muhammad Nazrul

    2012-01-01

    The intercalation of a drug active, perindopril, into Mg/Al-layered double hydroxide for the formation of a new nanocomposite, PMAE, was accomplished using a simple ion exchange technique. A relatively high loading percentage of perindopril of about 36.5% (w/w) indicates that intercalation of the active took place in the Mg/Al inorganic interlayer. Intercalation was further supported by Fourier transform infrared spectroscopy, and thermal analysis shows markedly enhanced thermal stability of the active. The release of perindopril from the nanocomposite occurred in a controlled manner governed by pseudo-second order kinetics. MTT assay showed no cytotoxicity effects from either Mg/Al-layered double hydroxide or its nanocomposite, PMAE. Mg/Al-layered double hydroxide showed angiotensin-converting enzyme inhibitory activity, with 5.6% inhibition after 90 minutes of incubation. On incubation of angiotensin-converting enzyme with 0.5 μg/mL of the PMAE nanocomposite, inhibition of the enzyme increased from 56.6% to 70.6% at 30 and 90 minutes, respectively. These results are comparable with data reported in the literature for Zn/Al-perindopril.

  3. Development of efficient electrocatalysts via molecular hybridization of NiMn layered double hydroxide nanosheets and graphene

    Science.gov (United States)

    Ma, Wei; Ma, Renzhi; Wu, Jinghua; Sun, Pengzhan; Liu, Xiaohe; Zhou, Kechao; Sasaki, Takayoshi

    2016-05-01

    Ni2+Mn3+ layered double hydroxide (LDH) nanoplatelets have been hydrothermally synthesized in a homogeneous precipitation of mixed Ni2+/Mn2+ salts at a molar ratio of 2 : 1 via the hydrolysis of hexamethylenetetramine (HMT) and in situ oxidation with H2O2. After anion-exchange, NiMn LDH was exfoliated into unilamellar nanosheets. Subsequent flocculation of NiMn LDH nanosheets with (reduced) graphene oxide (GO/rGO) into superlattice composites was achieved and further tested as electrocatalysts for oxygen evolution reaction (OER). The face-to-face heteroassembly of NiMn LDH nanosheets with conductive rGO at an alternating sequence resulted in a small overpotential of 0.26 V and a Tafel slope of 46 mV per decade, which is much superior to as-exfoliated nanosheets. The analyses of electrochemical activity surface area (ECSA) and impedance spectra clearly indicated that the superlattice structure was ideal in facilitating the migration/transfer of the charge and reactants, revealing the electrochemical energetics and mechanism behind the synergistic effect arising from molecular hybridization. The proof of concept toward total water splitting using the newly developed hybrid electrocatalyst was demonstrated by an electrolysis cell powered by a single AA battery.Ni2+Mn3+ layered double hydroxide (LDH) nanoplatelets have been hydrothermally synthesized in a homogeneous precipitation of mixed Ni2+/Mn2+ salts at a molar ratio of 2 : 1 via the hydrolysis of hexamethylenetetramine (HMT) and in situ oxidation with H2O2. After anion-exchange, NiMn LDH was exfoliated into unilamellar nanosheets. Subsequent flocculation of NiMn LDH nanosheets with (reduced) graphene oxide (GO/rGO) into superlattice composites was achieved and further tested as electrocatalysts for oxygen evolution reaction (OER). The face-to-face heteroassembly of NiMn LDH nanosheets with conductive rGO at an alternating sequence resulted in a small overpotential of 0.26 V and a Tafel slope of 46 mV per decade

  4. Interlayer intercalation and arrangement of 2-mercaptobenzothiazolate and 1,2,3-benzotriazolate anions in layered double hydroxides: In situ X-ray diffraction study

    Science.gov (United States)

    Serdechnova, Maria; Salak, Andrei N.; Barbosa, Filipe S.; Vieira, Daniel E. L.; Tedim, João; Zheludkevich, Mikhail L.; Ferreira, Mário G. S.

    2016-01-01

    2-mercaptobenzothiazole (MBT) and 1,2,3-benzotriazole (BTA) are very promising inhibitors for the corrosion protection of aluminum alloys. These inhibitors can be incorporated in protective coatings in the form of anions intercalated into interlayers of layered double hydroxides (LDHs). Capacity and performance of such LDH-nanocontainers depend on the arrangement of the anions in their interlayers. In this work, intercalation of MBT- and BTA- into Mg-Al-NO3 and Zn-Al-NO3 LDHs were studied in detail using X-ray diffraction (XRD) methods including in situ XRD. The nitrate-to-MBT(BTA) anion exchange is much faster than considered previously. Well-formed Mg-Al-MBT, Zn-Al-MBT, Mg-Al-BTA LDHs were obtained after a 20-min exchange reaction at pH 11.5 at room temperature. It was demonstrated that Zn-Al-BTA LDH cannot be obtained under the same conditions due to the reaction between BTA and the Zn-Al hydroxide layers. Substitution of nitrates by organic anions occurs with the participation of hydroxide anions. Although no intermediate LDH phase intercalated with the combination of NO3 - and OH- appears, formation of the LDH-MBT and LDH-BTA phases results also in appearance of an LDH phase intercalated with OH- at the final stage of the anion exchange. In the LDH interlayer, MBT- and BTA- form a double layer in which these species have a tilted orientation against the layer plane (herringbone-like arrangement). Such an arrangement meets the LDH layer-interlayer electroneutrality and matches well with the observed values of the layer-interlayer distance.

  5. Investigation of γ-(2,3-Epoxypropoxypropyltrimethoxy Silane Surface Modified Layered Double Hydroxides Improving UV Ageing Resistance of Asphalt

    Directory of Open Access Journals (Sweden)

    Canlin Zhang

    2017-01-01

    Full Text Available γ-(2,3-Epoxypropoxypropyltrimethoxy silane surface modified layered double hydroxides (KH560-LDHs were prepared and used to improve the ultraviolet ageing resistance of asphalt. The results of X-ray photoelectron spectrometry (XPS indicated that KH560 has been successfully grafted onto the surface of LDHs. The agglomeration of LDHs particles notably reduced after KH560 surface modification according to scanning electron microscopy (SEM, which implied that the KH560 surface modification was helpful to promote the dispersibility of LDHs in asphalt. Then, the influence of KH560-LDHs and LDHs on the physical and rheological properties of asphalt before and after UV ageing was thoroughly investigated. The storage stability test showed that the difference in softening point (ΔS of LDHs modified asphalt decreased from 0.6 °C to 0.2 °C at an LDHs content of 1% after KH560 surface modification, and the tendency became more pronounced with the increase of LDH content, indicating that KH560 surface modification could improve the stability of LDHs in asphalt. After UV ageing, the viscous modulus (G’’ of asphalt significantly reduced, and correspondingly, the elastic modulus (G’ and rutting factor (G*/sin δ rapidly increased. Moreover, the asphaltene increased and the amount of “bee-like” structures of the asphalt decreased. Compared with LDHs, KH560-LDHs obviously restrained performance deterioration of the asphalt, and helped to relieve the variation of the chemical compositions and morphology of asphalt, which suggested that the improvement of KH560-LDHs on UV ageing resistance of asphalt was superior to LDHs.

  6. Organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides with intercalated phacolysin as ocular delivery system

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Zhiguo; Zhang, Jie; Chi, Huibo; Cao, Feng, E-mail: cpufengc@163.com [China Pharmaceutical University, Department of Pharmaceutics, School of Pharmacy (China)

    2015-12-15

    This study was mainly aimed to evaluate the potential use of a novel ocular drug delivery system, organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides (LDH). Organic polymers of chitosan–glutathione (CG) and pre-activated chitosan–glutathione (CG-2MNA) were successfully synthesized and characterized. LDH with intercalated phacolysin (PCL), including larger hexagonal LDH–PCL (Lh-LDH–PCL), larger spherical LDH–PCL (Ls-LDH–PCL), smaller hexagonal LDH–PCL (Sh-LDH–PCL), CG hybrid LDH–PCL (LDH–PCL-CG), and CG-2MNA hybrid LDH–PCL (LDH–PCL-CG-2MNA), were prepared. The nanocomposites with particle size of 107.2–274.9 nm were characterized by powder X-ray diffraction, Fourier transform infrared, transmission electron micrographs, etc. In vivo precorneal retention studies showed that the detectable time of all nanocomposites was prolonged from 2 to 6 h in comparison to PCL saline. Accordingly, the AUC{sub 0–6h} values of Lh-LDH–PCL, Ls-LDH–PCL, Sh-LDH–PCL, LDH–PCL-CG, and LDH–PCL-CG-2MNA nanocomposites were increased by 2.27-, 2.08-, 3.08-, 4.67-, and 3.36-fold, respectively. The Draize test and hematoxylin and eosin staining demonstrated that modified LDH had no eye irritation after single and repeated administration. These results indicated that chitosan derivatives-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs.Graphical AbstractThiolated chitosan-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs and may facilitate penetration of drugs into tissues of the eyes.

  7. An optical sensor based on H-acid/layered double hydroxide composite film for the selective detection of mercury ion.

    Science.gov (United States)

    Sun, Zhiyong; Jin, Lan; Zhang, Shitong; Shi, Wenying; Pu, Min; Wei, Min; Evans, David G; Duan, Xue

    2011-09-19

    A novel optical chemosensor was fabricated based on 1-amino-8-naphthol-3,6-disulfonic acid sodium (H-acid) intercalated layered double hydroxide (LDH) film via the electrophoretic deposition (EPD) method. The film of H-acid/LDH with the thickness of 1 μm possesses a well c-orientation of the LDH microcrystals confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The fluorescence detection for Hg(II) in aqueous solution was performed by using the H-acid/LDH film sensor at pH 7.0, with a linear response range in 1.0 × 10(-7) to 1.0 × 10(-5) mol L(-1) and a detection limit of 6.3 × 10(-8) mol L(-1). Furthermore, it exhibits excellent selectivity for Hg(II) over a large number of competitive cations including alkali, alkaline earth, heavy metal and transitional metals. The specific fluorescence response of the optical sensor is attributed to the coordination between Hg(II) and sulfonic group in the H-acid immobilized in the LDH matrix, which was verified by NMR spectroscopy and UV-vis spectra. In addition, density functional theory (DFT) calculation further confirms that the coordination occurs between one Hg(2+) and two O atoms in the sulfonic group, which is responsible for the significant fluorescence quenching of the H-acid/LDH film. The results indicate that the H-acid/LDH composite film can be potentially used as a chemosensor for the detection of Hg(2+) in the environmental and biomedical field.

  8. Aluminum doped nickel oxide thin film with improved electrochromic performance from layered double hydroxides precursor in situ pyrolytic route

    Science.gov (United States)

    Shi, Jingjing; Lai, Lincong; Zhang, Ping; Li, Hailong; Qin, Yumei; Gao, Yuanchunxue; Luo, Lei; Lu, Jun

    2016-09-01

    Electrochromic materials with unique performance arouse great interest on account of potential application values in smart window, low-power display, automobile anti-glare rearview mirror, and e-papers. In this paper, high-performing Al-doped NiO porous electrochromic film grown on ITO substrate has been prepared via a layered double hydroxides(LDHs) precursor in situ pyrolytic route. The Al3+ ions distributed homogenously within the NiO matrix can significantly influence the crystallinity of Ni-Al LDH and NiO:Al3+ films. The electrochromic performance of the films were evaluated by means of UV-vis absorption spectroscopy, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry(CA) measurements. In addition, the ratio of Ni3+/Ni2+ also varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range (58.4%), fast switching speed (bleaching/coloration times are 1.8/4.2 s, respectively) and excellent durability (30% decrease after 2000 cycles). The improved performance was owed to the synergy of large NiO film specific surface area and porous morphology, as well as Al doping stifled the formation of Ni3+ making bleached state more pure. This LDHs precursor pyrolytic method is simple, low-cost and environmental benign and is feasible for the preparation of NiO:Al and other Al-doped oxide thin film.

  9. Synthesis of mesoporous Cu/Mg/Fe layered double hydroxide and its adsorption performance for arsenate in aqueous solutions

    Institute of Scientific and Technical Information of China (English)

    Yanwei Guo; Zhiliang Zhu; Yanling Qiu; Jianfu Zhao

    2013-01-01

    The mesoporous Cu/Mg/Fe layered double hydroxide (Cu/Mg/Fe-LDH) with carbonate intercalation was synthesized and used for the removal of arsenate from aqueous solutions.The Cu/Mg/Fe-LDH was characterized by Fourier transform infrared spectrometry,X-ray diffraction crystallography,scanning electron microscopy,X-ray photoelectron spectroscopy and Brunauer-Emmett-Teller.Effects of various physico-chemical parameters such as pH,adsorbent dosage,contact time and initial arsenate concentration on the adsorption of arsenate onto Cu/Mg/Fe-LDH were investigated.Results showed that it was efficient for the removal of arsenate,and the removal efficiency of arsenate increased with the increment of the adsorbent dosage,while the arsenate adsorption capacity decreased with increase of initial pH from 3 to 11.The adsorption isotherms can be well described by the Langmuir model with R2 > 0.99.Its adsorption kinetics followed the pseudo second-order kinetic model.Coexisting ions such as HPO42-,CO32-,SO42-and NO3-could compete with arsenate for adsorption sites on the Cu/Mg/Fe-LDH.The adsorption of arsenate on the adsorbent can be mainly attributed to the ion exchange process.It was found that the synthesized Cu/Mg/Fe-LDH can reduce the arsenate concentration down to a final level of < 10 μg/L under the experimental conditions,and makes it a potential material for the decontamination of arsenate polluted water.

  10. Topotactic Synthesis of Porous Cobalt Ferrite Platelets from a Layered Double Hydroxide Precursor and Their Application in Oxidation Catalysis.

    Science.gov (United States)

    Ortega, Klaus Friedel; Anke, Sven; Salamon, Soma; Özcan, Fatih; Heese, Justus; Andronescu, Corina; Landers, Joachim; Wende, Heiko; Schuhmann, Wolfgang; Muhler, Martin; Lunkenbein, Thomas; Behrens, Malte

    2017-09-12

    Monocrystalline, yet porous mosaic platelets of cobalt ferrite, CoFe2 O4 , can be synthesized from a layered double hydroxide (LDH) precursor by thermal decomposition. Using an equimolar mixture of Fe(2+) , Co(2+) , and Fe(3+) during co-precipitation, a mixture of LDH, (Fe(II) Co(II) )2/3 Fe(III)1/3 (OH)2 (CO3 )1/6 ⋅m H2 O, and the target spinel CoFe2 O4 can be obtained in the precursor. During calcination, the remaining Fe(II) fraction of the LDH is oxidized to Fe(III) leading to an overall Co(2+) :Fe(3+) ratio of 1:2 as required for spinel crystallization. This pre-adjustment of the spinel composition in the LDH precursor suggests a topotactic crystallization of cobalt ferrite and yields phase pure spinel in unusual anisotropic platelet morphology. The preferred topotactic relationship in most particles is [111]Spinel ∥[001]LDH . Due to the anion decomposition, holes are formed throughout the quasi monocrystalline platelets. This synthesis approach can be used for different ferrites and the unique microstructure leads to unusual chemical properties as shown by the application of the ex-LDH cobalt ferrite as catalyst in the selective oxidation of 2-propanol. Compared to commercial cobalt ferrite, which mainly catalyzes the oxidative dehydrogenation to acetone, the main reaction over the novel ex-LDH cobalt is dehydration to propene. Moreover, the oxygen evolution reaction (OER) activity of the ex-LDH catalyst was markedly higher compared to the commercial material. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Zn–Al layered double hydroxides intercalated with carbonate, nitrate, chloride and sulphate ions: Synthesis, characterisation and dye removal properties

    Directory of Open Access Journals (Sweden)

    Fatima Zahra Mahjoubi

    2017-01-01

    Full Text Available In this work, Zn–Al layered double hydroxides intercalated with carbonate, nitrate, chloride and sulphate ions were synthesised via a co-precipitation method at a constant solution pH. The as-synthesised samples were characterised by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, transmission electron microscopy (TEM and simultaneous thermogravimetric/differential thermal analysis (TGA-DTA. The XRD patterns showed that Zn-Al-SO4 had the greatest interlayer spacing, followed by Zn-Al-Cl, Zn-Al-NO3 and Zn-Al-CO3. The FTIR spectra clearly confirmed the presence of intercalated anions in the structure of the LDHs. Batch experiments for methyl orange (MO adsorption onto synthesised samples were investigated under various conditions such as contact time, initial dye concentration and solution pH. The experimental results show that pH is the most influencing factor. The effective pH range for the MO removal was found to be 3.5–4.5. The kinetics data can be described accurately by a pseudo-second-order kinetic model instead of a pseudo-first-order model. The equilibrium data were analysed using the Langmuir, Freundlich and Dubinin–Radushkevich models. The results showed that the Langmuir and Dubinin–Radushkevich isotherm models fit well to the experimental data. The Zn-Al-LDH samples exhibited exceptional Langmuir maximum adsorption capacities of 2758, 2455, 2270 and 1684 mg/g for Zn-Al-SO4, Zn-Al-Cl, Zn-Al-NO3 and Zn-Al-CO3, respectively.

  12. Layered Double Hydroxides with Hydrotalcite—type Structure Containing Fe3+,Al3+ and Mg2+

    Institute of Scientific and Technical Information of China (English)

    GUOXiong-hua; LIShu-ping; HOUWan-guo; HANShu-hua; HUJi-fan; LIDong-qing

    2003-01-01

    Layered double hydroxides(LDHs)with hydrotalcite-type structure containing Fe3+,Al3+ and Mg2+ were prepared by means of a coprecipitation method.The products were characterized by element analysis, X-ray powder diffraction and transmission electron microscopy.It was found that even if the molar ratio of n(Fe+Al)/n(Fe+Al+Mg)>0.33,yet a pure hydrotalcite-like compound(HTlc)phase was gained when n(Fe)/n(Al+Mg+Fe)≤0.30 and n(Al+Mg+Fe)≤0.30;the Al(OH)3 phase appeared in the products when n(Al)/n(Al+Mg+Fe)>0.30;and an amorphous phase emerged when n(Fe)/n(Al+Mg+Fe)>0.33.These results show that there is no concentration superposition effect between Fe3+ and Al3+ on the crystalline state of the produced samples.In our previous work,the concentration superposition effect between Zn2+ and Mg2+ in the synthesis of Zn-Mg-Al-LDHs was found.For the prepared Fe-Al-Mg-LDHs samples,the value of lattice parameter a is between 0.30-0.32nm;and the value of lattice parameter c is between 2.30-2.47nm,the bassl spacing is in the range of 0.76-0.83nm.When the ratio of n(Fe)/n(Al)is a constant,the values of a and c increase with the increase of the Mg2+ content of the produced samples.The mean particle size and the mean crystal grain were determined by virtue of a particle-size instrument,XRD-Scherrer formulsa and TEM method,respectively.

  13. Layered double hydroxides as an effective additive in polymer gelled electrolyte based dye-sensitized solar cells.

    Science.gov (United States)

    Ho, Hsu-Wen; Cheng, Wei-Yun; Lo, Yu-Chun; Wei, Tzu-Chien; Lu, Shih-Yuan

    2014-10-22

    Layered double hydroxides (LDH), a class of anionic clay materials, were developed as an effective additive for polymer gelled electrolytes for use in dye-sensitized solar cells (DSSC). Carbonate and chloride intercalated Zn-Al LDHs, ZnAl-CO3 LDH, and ZnAl-Cl LDH were prepared with coprecipitation methods. The addition of the two LDHs significantly improved, in terms of power conversion efficiency (PCE), over the plain poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) gelled electrolyte and competed favorably with the liquid electrolyte based DSSCs, 8.13% for the liquid electrolyte, 7.48% for the plain PVDF-HFP gelled electrolyte, 8.11% for the ZnAl-CO3 LDH/PVDF-HFP gelled electrolyte, and 8.00% for the ZnAl-Cl LDH/PVDF-HFP gelled electrolyte based DSSCs. The good performance in PCEs achieved by the LDH-loaded DSSCs came mainly from the significant boost in open circuit voltages (Voc), from 0.74 V for both the liquid electrolyte and PVDF-HFP gelled electrolyte based DSSCs to 0.79 V for both the ZnAl-CO3 LDH/PVDF-HFP and ZnAl-Cl LDH/PVDF-HFP gelled electrolyte based DSSCs. The boost in Voc was contributed mainly by the positive shift in redox potential of the redox couple, I(-)/I3(-), as revealed from cyclic voltammetry analyses. As for the long-term stability, PCE retention rates of 96 and 99% after 504 h were achieved by the ZnAl-CO3 LDH/PVDF-HFP and ZnAl-Cl LDH/PVDF-HFP gelled electrolyte based DSSCs, respectively, appreciably better than 92% achieved by the liquid electrolyte based one after 480 h.

  14. Mn(II removal from aqueous solutions by Co/Mo layered double hydroxide: Kinetics and thermodynamics

    Directory of Open Access Journals (Sweden)

    A.A. Bakr

    2016-06-01

    Full Text Available This paper deals with the experimental investigation related to the Mn(II removal from aqueous solutions by the adsorption onto a synthesized Co/Mo layered double hydroxide (Co/Mo-LDH. The adsorption behavior was studied as a function of initial Mn(II concentration (40–145 mg/L, contact time (15–90 min, solution pH (2–9 and adsorbent mass (0.05–0.35 g per 1.0 L. All adsorption processes were rapidly carried out at different temperatures (298, 308 and 318 K and constant stirring rate 160 rpm. The results showed that the Co/Mo-LDH is a very promising material for removing of Mn(II from the aqueous solutions. Particularly, the solution pH range of 4–7 has the most significant effect on the adsorption capacity. The results revealed that the maximum adsorption capacities were 20.2, 26.75 and 38.1 mg/g from the initial Mn(II concentration (145 mg/L at pH 5, adsorbent mass (0.2 g/1.0 L, and contact time (60 min at different temperatures, 298, 308 and 318 K, respectively. The adsorption kinetics data are well fitted by the pseudo-second-order model, while the adsorption isotherms data were better fitted by the Langmuir equation. Also, this paper discusses the thermodynamic parameters of the adsorption and the results demonstrate that the adsorption process is spontaneous and endothermic.

  15. Synergistic coagulation of GO and secondary adsorption of heavy metal ions on Ca/Al layered double hydroxides.

    Science.gov (United States)

    Yao, Wen; Wang, Jian; Wang, Pengyi; Wang, Xiangxue; Yu, Shujun; Zou, Yidong; Hou, Jing; Hayat, Tasawar; Alsaedi, Ahmed; Wang, Xiangke

    2017-10-01

    With the extensive application of graphene oxide (GO), it is noticeable that part of GO is directly/indirectly released into the environment and widespread research indicated that it had adverse influences on human health and ecological balance. In this work, a novel nanobelt-like Ca/Al layered double hydroxides (CA-LDH) was synthesized and applied as efficient coagulant for the removal of GO from aqueous solutions. The results indicated that neutral pH, co-existing cations and higher temperature were beneficial to the coagulation of GO. The sequence of cation effect for promoting of GO coagulation was Ca(2+) > Mg(2+) > K(+) > Na(+), whereas the effect of anions on GO coagulation was PO4(3-) > CO3(2-) > SO4(2-) > Cl(-). Comparing with anions, the cations showed more dominate effect for GO coagulation than anions. Hydrogen bonds and electrostatic interaction were the main coagulation mechanisms for GO coagulation, which were evidenced by FT-IR and XPS analysis. Specifically, for the first time, the reclaimed product of CA-LDH after GO coagulation (CA-LDH + GO) was applied as adsorbents for the secondary application in the removal of heavy metal ions from aqueous solutions. Interestingly, the CA-LDH + GO still had high adsorption capacities, i.e., the maximum adsorption capacities (qmax) for Cu(II), Pb(II), and Cr(VI) were 122.7 mg/g, 221.2 mg/g and 64.4 mg/g, respectively, higher than other similar materials. This paper highlighted the LDH-based nanomaterials are promising materials for the elimination of environmental pollutants and the migration and transformation of carbon nanomaterials in the natural environment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. In-syringe extraction using dissolvable layered double hydroxide-polymer sponges templated from hierarchically porous coordination polymers.

    Science.gov (United States)

    Ghani, Milad; Frizzarin, Rejane M; Maya, Fernando; Cerdà, Víctor

    2016-07-01

    Herein we report the use of cobalt porous coordination polymers (PCP) as intermediates to prepare advanced extraction media based on layered double hydroxides (LDH) supported on melamine polymer foam. The obtained dissolvable Ni-Co LDH composite sponges can be molded and used as sorbent for the in-syringe solid-phase extraction (SPE) of phenolic acids from fruit juices. The proposed sorbent is obtained due to the surfactant-assisted self-assembly of Co(II)/imidazolate PCPs on commercially available melamine foam, followed by the in situ conversion of the PCP into the final dissolvable LDH coating. Advantageous features for SPE are obtained by using PCPs with hierarchical porosity (HPCPs). The LDH-sponge prepared using intermediate HPCPs (HLDH-sponge) is placed in the headspace of a glass syringe, enabling flow-through extraction followed by analyte elution by the dissolution of the LDH coating in acidic conditions. Three phenolic acids (gallic acid, p-hydroxybenzoic acid and caffeic acid) were extracted and quantified using high performance liquid chromatography. Using a 5mL sample volume, the obtained detection limits were 0.15-0.35μgL(-1). The proposed method for the preparation of HLDH-sponges showed a good reproducibility as observed from the intra- and inter-day RSD's, which were <10% for all analytes. The batch-to-batch reproducibility for three different batches of HLDH-sponges was 10.6-11.2%. Enrichment factors of 15-21 were obtained. The HLDH-sponges were applied satisfactorily to the determination of phenolic acids in natural and commercial fruit juices, obtaining relative recoveries among 89.7-95.3%.

  17. Chemical reactive features of novel amino acids intercalated layered double hydroxides in As(III) and As(V) adsorption.

    Science.gov (United States)

    Shen, Liang; Jiang, Xiuli; Chen, Zheng; Fu, Dun; Li, Qingbiao; Ouyang, Tong; Wang, Yuanpeng

    2017-06-01

    Layered double hydroxides (LDHs) intercalated with amino acids such as methionine (Met) were synthesized as new adsorbents to remediate arsenic-polluted water. This Zn2Al-Met-LDHs, identified with the formula of Zn0.7Al0.3(OH)2(Met)0.3·0.32H2O, has good thermal stability. Adsorption experiments with Zn2Al-Met-LDHs showed that the residual arsenic in solution could be reduced below the regulation limit, and this adsorption process fitted Langmuir isotherm and the pseudo-second-order kinetics well. A remarkably high removal efficiency and the maximum adsorption capacity for As(III) were achieved, 96.7% and 94.1 mg/g, respectively, at 298 K. The desorption efficiency of As(III) from the arsenic-saturated Zn2Al-Met-LDHs (<8.7%), far less than that of As(V), promises a specific and reliable uptake of As(III) in sorts of solutions. More importantly, a complete and in-depth spectra analysis through FTIR, XPS and NMR was conducted to explain the excellent performance of Zn2Al-Met-LDHs in arsenic removal. Herein, two special chemical reactions were proposed as the dominant mechanisms, i.e., hydrogen bonding between the carboxyl group of the host Met and the hydroxyl group of As(III) or As(V), and the formation of a chelate ring between the guest As(III) and the S, N bidentate ligands of the intercalated Met in the LDHs.

  18. Preparation of Rh-TPPTS complex intercalated layered double hydroxide and influences of host and guest compositions on its catalytic performances in hydroformylation reaction

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xian; LU Jun; JIN Lan; WEI Min

    2008-01-01

    Based on the concept of intercalation chemistry of layered double hydroxides (LDHs), RhCI(GO)-(TPPTS)2 (TPPTS: P(m-C6H4SO3Na)3) and TPPTS co-intercalated LDHs were successfully synthesized by in situ complexation method. Characterizations of structure and composition of composite materials by powder XRD, FT-IR, and ICP-AES techniques confirmed the supramolecular structures of the catalytic species intercalated LDHs. The correlation between catalytic performance of intercalated catalyst and the composition of both host layers and interlayer guest species was also investigated.

  19. Single-crystalline organic-inorganic layered cobalt hydroxide nanofibers: facile synthesis, characterization, and reversible water-induced structural conversion.

    Science.gov (United States)

    Guo, Xiaodi; Wang, Lianying; Yue, Shuang; Wang, Dongyang; Lu, Yanluo; Song, Yufei; He, Jing

    2014-12-15

    New pink organic-inorganic layered cobalt hydroxide nanofibers intercalated with benzoate ions [Co(OH)(C6H5COO)·H2O] have been synthesized by using cobalt nitrate and sodium benzoate as reactants in water with no addition of organic solvent or surfactant. The high-purity nanofibers are single-crystalline in nature and very uniform in size with a diameter of about 100 nm and variable lengths over a wide range from 200 μm down to 2 μm by simply adjusting reactant concentrations. The as-synthesized products are well-characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), fast Fourier transforms (FFT), X-ray diffraction (XRD), energy dispersive X-ray spectra (EDX), X-ray photoelectron spectra (XPS), elemental analysis (EA), Fourier transform infrared (FT-IR), thermogravimetric analysis (TGA), and UV-vis diffuse reflectance spectra (UV-vis). Our results demonstrate that the structure consists of octahedral cobalt layers and the benzoate anions, which are arranged in a bilayer due to the π-π stacking of small aromatics. The carboxylate groups of benzoate anions are coordinated to Co(II) ions in a strong bridging mode, which is the driving force for the anisotropic growth of nanofibers. When NaOH is added during the synthesis, green irregular shaped platelets are obtained, in which the carboxylate groups of benzoate anions are coordinated to the Co(II) ions in a unidentate fashion. Interestingly, the nanofibers exhibit a reversible transformation of the coordination geometry of the Co(II) ions between octahedral and pseudotetrahedral with a concomitant color change between pink and blue, which involves the loss and reuptake of unusual weakly coordinated water molecules without destroying the structure. This work offers a facile, cost-effective, and green strategy to rationally design and synthesize functional nanomaterials for future applications in catalysis, magnetism

  20. Sustained-Release of Cefepime from Cefepime-Intercalated Layered Double Hydroxides%头孢吡肟插层水滑石的缓释性能

    Institute of Scientific and Technical Information of China (English)

    孙志茵; 倪哲明; 李远; 夏盛杰

    2013-01-01

    用共沉淀法将头孢吡肟(Cefepime)插层到含NO3-的Zn-Al水滑石(layered double hydroxides,LDHs)层间,组装得到杂化材料Cefepime-LDHs.X射线衍射结果表明:Cefepime-LDHs晶型良好,为典型的水滑石类层状材料,其层间距为2.18rm.通过对Cefepime三维尺寸的理论模拟,推测该杂化材料中的Cefepime以沿长轴方向与层板呈一定角度倾斜的方式排布于水滑石层间.此外,与Cefepime相比,该杂化材料中层间药物的释放具有一定的缓释效果,缓释过程符合一级动力学及Higuchi扩散模型.%Cefepime pillared Zn-Al layered double hydroxides (LDHs) was assembled via coprecipitation process. Cefepime intercalated Zn-Al layered double hydroxides with good crystallinity was obtained. The results by X-ray diffraction reflected that the in-terlayer spaces of as-synthesized Cefepime-LDHs was 2.18nm. According to the simulated three-dimensional molecular size, the Cefepime guests could be arranged along the long axis orientation with a constant angle in the layers. The sustained-release of Cefepime pillared hydrotalcite were enhanced to a certain extent, compared to those of Cefepime. The release process followed both the Higuchi models and first order kinetics.

  1. Controlled release and angiotensin-converting enzyme inhibition properties of an antihypertensive drug based on a perindopril erbumine-layered double hydroxide nanocomposite

    Directory of Open Access Journals (Sweden)

    Hussein Al Ali SH

    2012-04-01

    Full Text Available Samer Hasan Hussein Al Ali1, Mothanna Al-Qubaisi2, Mohd Zobir Hussein1,3, Maznah Ismail2,4, Zulkarnain Zainal1, Muhammad Nazrul Hakim51Department of Chemistry, Faculty of Science, 2Laboratory of Molecular Biomedicine, Institute of Bioscience, 3Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, 4Department of Nutrition and Dietetics, Faculty of Medicine and Health Science, 5Department of Biomedical Science, Faculty of Medicine and Health Science, Universiti Putra Malaysia, Serdang, Selangor, MalaysiaBackground: The intercalation of perindopril erbumine into Zn/Al-NO3-layered double hydroxide resulted in the formation of a host-guest type of material. By virtue of the ion-exchange properties of layered double hydroxide, perindopril erbumine was released in a sustained manner. Therefore, this intercalated material can be used as a controlled-release formulation.Results: Perindopril was intercalated into the interlayers and formed a well ordered, layered organic-inorganic nanocomposite. The basal spacing of the products was expanded to 21.7 Å and 19.9 Å by the ion-exchange and coprecipitation methods, respectively, in a bilayer and a monolayer arrangement, respectively. The release of perindopril from the nanocomposite synthesized by the coprecipitation method was slower than that of its counterpart synthesized by the ion-exchange method. The rate of release was governed by pseudo-second order kinetics. An in vitro antihypertensive assay showed that the intercalation process results in effectiveness similar to that of the antihypertensive properties of perindopril.Conclusion: Intercalated perindopril showed better thermal stability than its free counterpart. The resulting material showed sustained-release properties and can therefore be used as a controlled-release formulation.Keywords: perindopril erbumine, layered double hydroxides, ion-exchange, coprecipitation, sustained release, angiotensin-converting enzyme

  2. Zn-Al layered double hydroxide prepared at different molar ratios: Preparation, characterization, optical and dielectric properties

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Abdullah Ahmed Ali [Department of Physics, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Talib, Zainal Abidin, E-mail: zainalat@science.upm.edu.my [Department of Physics, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Zobir bin Hussein, Mohd [Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Zakaria, Azmi [Department of Physics, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia)

    2012-07-15

    The co-precipitation method was used to prepare Zn-Al-NO{sub 3}-LDH at different Zn{sup 2+}/Al{sup 3+} molar ratios (2, 3, 4, 5 and 6) and pH value of 7.5. The structure, textural, composition and morphological properties were investigated using powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) and scanning electron microscope (SEM), respectively. The crystallinity of LDH samples were found to improve as molar ratio decreased which is attributed to the distortion of the hydroxide layers networks of the LDH crystal by the larger difference in ionic radii of Zn{sup 2+} and Al{sup 3+}. The optical band gap energy of LDH samples were evaluated using absorbance data from UV-Vis-NIR Diffuse reflectance spectroscopy. Band gaps were affected by the variation of the Zn{sup 2+}/Al{sup 3+} molar ratio is due to the formation of the low crystalline phases (ZnO and ZnAl{sub 2}O{sub 4}). The water molecules and anionic NO{sub 3}{sup -} in the LDH interlayer were responsible for the generation of the dielectric response. This response can be described by an anomalous low frequency dispersion using the second type of Universal Power Law. The dominance of ZnO dipoles and charge carriers (NO{sub 3}{sup -} ions) in the dielectric relaxation increases with the increasing molar ratio. - Graphical abstract: (a) Schematic diagram of Zn-Al- NO{sub 3}-LDH shows the LDH structure, (b) Kubelka-Munk transformed reflectance spectra and c. The dielectric constant versus frequency of Zn-Al- NO{sub 3}-LDH samples. Highlights: Black-Right-Pointing-Pointer Zn-Al-NO{sub 3}-LDH was prepared at different Zn{sup 2+}/Al{sup 3+} molar ratios (2, 3, 4, 5 and 6). Black-Right-Pointing-Pointer The crystallinity of LDH phase decreased with increase of Zn{sup 2+}/Al{sup 3+} molar ratio. Black-Right-Pointing-Pointer The optical band gaps of LDH samples have been measured. Black-Right-Pointing-Pointer Dielectric response of LDH can be described by anomalous low

  3. Formation of Zn-rich phyllosilicate, Zn-layered double hydroxide and hydrozincite in contaminated calcareous soils

    Energy Technology Data Exchange (ETDEWEB)

    Jacquat, Olivier; Voegelin, Andreas; Villard, Andre; Marcus, Matthew A.; Kretzschmar, Ruben

    2007-10-15

    Recent studies demonstrated that Zn-phyllosilicate- and Zn-layered double hydroxide-type (Zn-LDH) precipitates may form in contaminated soils. However, the influence of soil properties and Zn content on the quantity and type of precipitate forming has not been studied in detail so far. In this work, we determined the speciation of Zn in six carbonate-rich surface soils (pH 6.2 to 7.5) contaminated by aqueous Zn in the runoff from galvanized power line towers (1322 to 30090 mg/kg Zn). Based on 12 bulk and 23 microfocused extended X-ray absorption fine structure (EXAFS) spectra, the number, type and proportion of Zn species were derived using principal component analysis, target testing, and linear combination fitting. Nearly pure Zn-rich phyllosilicate and Zn-LDH were identified at different locations within a single soil horizon, suggesting that the local availabilities of Al and Si controlled the type of precipitate forming. Hydrozincite was identified on the surfaces of limestone particles that were not in direct contact with the soil clay matrix. With increasing Zn loading of the soils, the percentage of precipitated Zn increased from {approx}20% to {approx}80%, while the precipitate type shifted from Zn-phyllosilicate and/or Zn-LDH at the lowest studied soil Zn contents over predominantly Zn-LDH at intermediate loadings to hydrozincite in extremely contaminated soils. These trends were in agreement with the solubility of Zn in equilibrium with these phases. Sequential extractions showed that large fractions of soil Zn ({approx}30% to {approx}80%) as well as of synthetic Zn-kerolite, Zn-LDH, and hydrozincite spiked into uncontaminated soil were readily extracted by 1 M NH{sub 4}NO{sub 3} followed by 1 M NH{sub 4}-acetate at pH 6.0. Even though the formation of Zn precipitates allows for the retention of Zn in excess to the adsorption capacity of calcareous soils, the long-term immobilization potential of these precipitates is limited.

  4. Aluminum doped nickel oxide thin film with improved electrochromic performance from layered double hydroxides precursor in situ pyrolytic route

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Jingjing; Lai, Lincong; Zhang, Ping; Li, Hailong; Qin, Yumei; Gao, Yuanchunxue; Luo, Lei; Lu, Jun, E-mail: lujun@mail.buct.edu.cn

    2016-09-15

    Electrochromic materials with unique performance arouse great interest on account of potential application values in smart window, low-power display, automobile anti-glare rearview mirror, and e-papers. In this paper, high-performing Al-doped NiO porous electrochromic film grown on ITO substrate has been prepared via a layered double hydroxides(LDHs) precursor in situ pyrolytic route. The Al{sup 3+} ions distributed homogenously within the NiO matrix can significantly influence the crystallinity of Ni-Al LDH and NiO:Al{sup 3+} films. The electrochromic performance of the films were evaluated by means of UV–vis absorption spectroscopy, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry(CA) measurements. In addition, the ratio of Ni{sup 3+}/Ni{sup 2+} also varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range (58.4%), fast switching speed (bleaching/coloration times are 1.8/4.2 s, respectively) and excellent durability (30% decrease after 2000 cycles). The improved performance was owed to the synergy of large NiO film specific surface area and porous morphology, as well as Al doping stifled the formation of Ni{sup 3+} making bleached state more pure. This LDHs precursor pyrolytic method is simple, low-cost and environmental benign and is feasible for the preparation of NiO:Al and other Al-doped oxide thin film. - Graphical abstract: The ratio of Ni{sup 3+}/Ni{sup 2+} varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range, fast switching speed and excellent durability. Display Omitted.

  5. Preparation and controlled-release studies of a protocatechuic acid-magnesium/aluminum-layered double hydroxide nanocomposite

    Directory of Open Access Journals (Sweden)

    Barahuie F

    2013-05-01

    Full Text Available Farahnaz Barahuie,1 Mohd Zobir Hussein,1 Samer Hasan Hussein-Al-Ali,2 Palanisamy Arulselvan,3 Sharida Fakurazi,3,4 Zulkarnain Zainal11Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA, 2Laboratory of Molecular Biomedicine, Institute of Bioscience, 3Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, 4Department of Human Anatomy, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, Serdang, MalaysiaAbstract: In the study reported here, magnesium/aluminum (Mg/Al-layered double hydroxide (LDH was intercalated with an anticancer drug, protocatechuic acid, using ion-exchange and direct coprecipitation methods, with the resultant products labeled according to the method used to produce them: “PANE” (ie, protocatechuic acid-Mg/Al nanocomposite synthesized using the ion-exchange method and “PAND” (ie, protocatechuic acid-Mg/Al nanocomposite synthesized using the direct method, respectively. Powder X-ray diffraction and Fourier transform infrared spectroscopy confirmed the intercalation of protocatechuic acid into the inter-galleries of Mg/Al-LDH. The protocatechuic acid between the interlayers of PANE and PAND was found to be a monolayer, with an angle from the z-axis of 8° for PANE and 15° for PAND. Thermogravimetric and differential thermogravimetric analysis results revealed that the thermal stability of protocatechuic acid was markedly enhanced upon intercalation. The loading of protocatechuic acid in PANE and PAND was estimated to be about 24.5% and 27.5% (w/w, respectively. The in vitro release study of protocatechuic acid from PANE and PAND in phosphate-buffered saline at pH 7.4, 5.3, and 4.8 revealed that the nanocomposites had a sustained release property. After 72 hours incubation of PANE and PAND with MCF-7 human breast cancer and HeLa human cervical cancer cell lines, it was found that the nanocomposites had suppressed the growth of these cancer cells

  6. Study of 2,4-dichlorophenoxyacetic acid (2,4-D) removal by Cu-Fe-layered double hydroxide from aqueous solution

    Science.gov (United States)

    Nejati, Kamellia; Davary, Soheila; Saati, Marziye

    2013-09-01

    The hydrotalcite-like compound of Cu-Fe-layered double hydroxide was studied as a potential adsorbent of herbicide 2,4-dichlorophenoxyacetic acid (2,4-D). The nanoparticles of Cu-Fe layered double hydroxide were prepared by Cu/Fe molar ratio of 2:1 using a coprecipitation method at pH 8.5 and characterized by the X-ray powder diffraction (XRD), the Fourier transform infrared spectroscopy (FT-IR), the thermal gravimetric analysis (TGA) and the elemental analysis. The size and morphology of nanoparticles were examined by the transmission electron microscopy (TEM). The adsorption experiments on LDH, on the other hand, were conducted in three different procedures, namely, time-dependent, pH-dependent and temperature-dependent. Characterization of the adsorption products by the XRD method indicates that the intercalation of 2,4-D between the LDH layers has not occurred and the surface adsorption had taken place. The adsorption kinetic was tested for pseudo-first-order, pseudo-second-order, Elovich and Intra-particle diffusion kinetic models and the rate constants were calculated. The equilibrium adsorption data were described by Langmuir and Freundlich equations. It was observed that, the Langmuir isotherm slightly better fitted to the experimental data rather than that of Freundlich. In the adsorption experiments, the Gibbs free energy values, ΔG°, the enthalpy, ΔH°, and the entropy, ΔS° were also determined.

  7. Removal of Evans Blue and Yellow thiazole dyes from aqueous solution by Mg-Al-CO3 Layered Double Hydroxides as anion-exchanger

    OpenAIRE

    Mohamed Bouraada; Louis Charles de Ménorval; Hassiba Bessaha

    2014-01-01

    Mg-Al-CO3 Layered double hydroxide (LDH) was prepared by co-precipitation method at constant pH, and subsequently used to remove Evans Blue (EB) and Yellow thiazole (YT) dyes from aqueous solutions. The obtained material was characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), thermal analysis and BET. The kinetic and equilibrium aspects of sorption of the anionic dyes from aqueous solution by Mg-Al-CO3 were investigated in batch mode. The sorp...

  8. Drug delivery system for an anticancer agent, chlorogenate-Zn/Al-layered double hydroxide nanohybrid synthesised using direct co-precipitation and ion exchange methods

    Energy Technology Data Exchange (ETDEWEB)

    Barahuie, Farahnaz [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Hussein, Mohd Zobir, E-mail: mzobir@putra.upm.edu.my [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Arulselvan, Palanisamy [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Fakurazi, Sharida [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Department of Human Anatomy, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Zainal, Zulkarnain [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia)

    2014-09-15

    A nano-structured drug-inorganic clay hybrid involving an active anticancer compound, which is chlorogenic acid (CA) intercalated into Zn/Al-layered double hydroxide, has been assembled via ion-exchange and co-precipitation methods to form a nanohybrid CZAE (a chlorogenic acid-Zn/Al nanohybrid synthesised using an ion-exchange method) and CZAC (a chlorogenic acid-Zn/Al nanohybrid synthesised using a direct method), respectively. The X-ray diffraction (XRD) results confirmed that the CA-LDH had a hybrid structure in which the anionic chlorogenate is arranged between the interlayers as a horizontal monolayer at 90 and 20° angles from the x axis for CZAE and CZAC, respectively. Both nanohybrids have the properties of mesoporous materials. The high loading percentage of chlorogenic acid (approximately 43.2% for CZAE and 45.3% for CZAC) with basal spacings of 11.7 and 12.6 Å for CZAE and CZAC, respectively, corroborates the successful intercalation of chlorogenic acid into the interlayer gallery of layered double hydroxides. Free chlorogenic acid and the synthesised nanocomposites (CZAE, CZAC) were assessed for their cytotoxicity against various cancer cells. The Fourier transform infrared data supported the formation of both nanohybrids, and a thermal analysis showed that the nanohybrids are more thermally stable than their counterparts. The chlorogenate shows a sustained release, and the release rate of chlorogenate from CZAE and CZAC nanohybrids at pH 7.4 is remarkably lower than that at pH 4.8 due to their different release mechanisms. The release rate of chlorogenate from both nanohybrids can be described as pseudo-second order. The present investigation revealed the potential of the nanohybrids to enhance the in vitro anti-tumour effect of chlorogenic acid in liver and lung cancer cells in vitro. - Highlights: • We intercalated chlorogenic into Zn/Al-layered double hydroxide by ion-exchange and coprecipitation methods. • The two methods gave nanocomposites

  9. Transesterification of edible, non-edible and used cooking oils for biodiesel production using calcined layered double hydroxides as reusable base catalysts.

    Science.gov (United States)

    Sankaranarayanan, Sivashunmugam; Antonyraj, Churchil A; Kannan, S

    2012-04-01

    Fatty acid methyl esters (FAME) were produced from edible, non-edible and used cooking oils with different fatty acid contents by transesterification with methanol using calcined layered double hydroxides (LDHs) as solid base catalysts. Among the catalysts, calcined CaAl2-LDH (hydrocalumite) showed the highest activity with >90% yield of FAME using low methanol:oil molar ratio (catalyzed process for production of biodiesel in high yields from a wide variety of triglyceride oils including used oils is possible using optimized conditions.

  10. 5-Fluorouracil intercalated iron oxide@layered double hydroxide core-shell nano-composites with isotropic and anisotropic architectures for shape-selective drug delivery applications.

    Science.gov (United States)

    Tuncelli, Gülsevde; Ay, Ahmet Nedim; Zümreoglu-Karan, Birgül

    2015-10-01

    We report the synthesis, characterization and in vitro release behavior of anti-cancer drug carrying iron oxide@layered double hydroxide core-shell nanocomposites with sizes ranging from 40 to 300 nm, good drug loading capacities and soft ferromagnetic properties. HRTEM analyses verified that nearly spherical isotropic carriers were obtained by coating spherical magnetite particles while anisotropic carriers were obtained by coating spindle-shaped hematite particles. They both displayed a fluctuating in vitro release profile with a higher release percentage for the anisotropic carrier.

  11. New treatment method for boron in aqueous solutions using Mg–Al layered double hydroxide: Kinetics and equilibrium studies

    Energy Technology Data Exchange (ETDEWEB)

    Kameda, Tomohito, E-mail: kameda@env.che.tohoku.ac.jp; Oba, Jumpei; Yoshioka, Toshiaki

    2015-08-15

    Highlights: • NO{sub 3}·Mg–Al LDHs and Cl·Mg–Al LDHs could take up boron from aqueous solutions. • Boron was removed by anion exchange of B(OH){sub 4}{sup −} with intercalated NO{sub 3}{sup −} and Cl{sup −}. • The residual concentration of B was less than the effluent standards in Japan. • The removal of B was well described by a pseudo second-order kinetic equation. • The adsorption of B followed a Langmuir-type adsorption. - Abstract: Mg–Al layered double hydroxides (LDHs) intercalated with NO{sub 3}{sup −} (NO{sub 3}·Mg–Al LDHs) and with Cl{sup −} (Cl·Mg–Al LDHs) were found to take up boron from aqueous solutions. Boron was removed by anion exchange of B(OH){sub 4}{sup −} in solution with NO{sub 3}{sup −} and Cl{sup −} intercalated in the interlayer of the LDH. Using three times the stoichiometric quantity of NO{sub 3}·Mg–Al LDH, the residual concentration of B decreased from 100 to 1.9 mg L{sup −1} in 120 min. Using five times the stoichiometric quantity of Cl·Mg–Al LDH, the residual concentration of B decreased from 100 to 5.6 mg L{sup −1} in 120 min. It must be emphasized that, in both cases, the residual concentration of B was less than the effluent standards in Japan (10 mg L{sup −1}). The rate-determining step of B removal by the NO{sub 3}·Mg–Al and Cl·Mg–Al LDHs was found to be chemical adsorption involving anion exchange of B(OH){sub 4}{sup −} with intercalated NO{sub 3}{sup −} and Cl{sup −}. The removal of B was well described by a pseudo second-order kinetic equation. The adsorption of B by NO{sub 3}·Mg–Al LDH and Cl·Mg–Al LDH followed a Langmuir-type adsorption. The values of the maximum adsorption and the equilibrium adsorption constant were 3.6 mmol g{sup −1} and 1.7, respectively, for NO{sub 3}·Mg–Al LDH, and 3.8 mmol g{sup −1} and 0.7, respectively, for Cl·Mg–Al LDH. The B(OH){sub 4}{sup −} in B(OH){sub 4}·Mg–Al LDH produced by removal of B was found to undergo

  12. Lubrication performance and mechanisms of Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxide nanoparticles as lubricant additives

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shuo [School of Materials Science and Technology, China University of Geosciences (Beijing), 29 Xueyuan Road, Haidian Distract, Beijing 100083 (China); Nanoprobe Laboratory for Bio- & Nanotechnology and Biomimetics (NLBB), The Ohio State University, 201 W. 19th Avenue Columbus, OH 43210-1142 (United States); Bhushan, Bharat, E-mail: bhushan.2@osu.edu [Nanoprobe Laboratory for Bio- & Nanotechnology and Biomimetics (NLBB), The Ohio State University, 201 W. 19th Avenue Columbus, OH 43210-1142 (United States)

    2016-08-15

    Highlights: • Mg/Al-, Zn/Al- and Zn/Mg/Al-layered double hydroxide were synthesized. • Mg/Al-LDH had superior tribological performance compared to other LDHs. • The best thermal stability of Mg/Al-LDH was responsible for its friction property. - Abstract: Solid lubricant particles are commonly used as oil additives for low friction and wear. Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxides (LDH) were synthesized by coprecipitation method. The benefits of LDH nanoparticles are that they can be synthesized using chemical methods where size and shape can be controlled, and can be modified organically to allow dispersal in fluids. The LDH nanoparticles were characterized by X-ray diffraction, scanning electron microscope, thermogravimetry, and differential scanning calorimetry. A pin-on-disk friction and wear tester was used for evaluating the friction and wear properties of LDH nanoparticles as lubricant additives. LDH nanoparticles have friction-reducing and anti-wear properties compared to oil without LDHs. Mg/Al-LDH has the best lubrication, possibly due to better thermal stability in severe conditions.

  13. The influence of the UV irradiation intensity on photocatalytic activity of ZnAl layered double hydroxides and derived mixed oxides

    Directory of Open Access Journals (Sweden)

    Hadnađev-Kostić Milica S.

    2012-01-01

    Full Text Available Layered double hydroxides (LDHs have been studied to a great extent as environmental-friendly complex materials that can be used as photocatalysts or photocatalyst supports. ZnAl layered double hydroxides and their derived mixed oxides were chosen for the investigation of photocatalytic performances in correlation with the UV intensities measured in the South Pannonia region. Low supersaturation coprecipitation method was used for the ZnAl LDH synthesis. For the characterization of LDH and thermal treated samples powder X-ray diffraction (XRD, scanning electron microscopy (SEM, electron dispersive spectroscopy (EDS, nitrogen adsorption-desorption were used. The decomposition of azodye, methylene blue was chosen as photocatalytic test reaction. The study showed that the ZnAl mixed oxide obtained by thermal decomposition of ZnAl LDH has stable activity in the broader UV light irradiation range characterizing the selected region. Photocatalytic activity could be mainly attributed to the ZnO phase, detected both in LDH and thermally treated samples. The study showed that the ZnAl mixed oxide obtained by the calcination of ZnAl LDH has a stable activity within the measured UV light irradiation range; whereas the parent ZnAl LDH catalyst did not perform satisfactory when low UV irradiation intensity is implied.

  14. One-pot synthesis of carbon supported calcined-Mg/Al layered double hydroxides for antibiotic removal by slow pyrolysis of biomass waste

    Science.gov (United States)

    Tan, Xiaofei; Liu, Shaobo; Liu, Yunguo; Gu, Yanling; Zeng, Guangming; Cai, Xiaoxi; Yan, Zhili; Yang, Chunping; Hu, Xinjiang; Chen, Bo

    2016-12-01

    A biochar supported calcined-Mg/Al layered double hydroxides composite (CLDHs/BC) was synthesized by a one-pot slow pyrolysis of LDHs preloaded bagasse biomass. Multiple characterizations of the product illustrated that the calcined-Mg/Al layered double hydroxides (CLDHs) were successfully coated onto the biochar in slow pyrolysis of pre-treated biomass. The as-synthesized CLDHs/BC could efficiently remove antibiotic tetracycline from aqueous solutions. The coating of CLDHs significantly increased the adsorption ability of biochar, and CLDHs/BC exhibited more than 2 times higher adsorption capacity than that of the pristine biochar (BC) in the tested pH range. The maximum adsorption capacity of CLDHs/BC for tetracycline was 1118.12 mg/g at 318 K. The experimental results suggested that the interaction with LDHs on biochar played a dominant role in tetracycline adsorption, accompanied with π-π interaction and hydrogen bond. This study provides a feasible and simple approach for the preparation of high-performance material for antibiotics contaminated wastewater treatment in a cost-effective way.

  15. Electrosynthesized Ni-Al Layered Double Hydroxide-Pt Nanoparticles as an Inorganic Nanocomposite and Potentate Anodic Material for Methanol Electrooxidation in Alkaline Media

    Directory of Open Access Journals (Sweden)

    Biuck Habibi

    2017-04-01

    Full Text Available In this study, Ni-Al layered double hydroxide (LDH-Pt nanoparticles (PtNPs as an inorganic nano-composite was electrosynthesized on the glassy carbon electrode (GCE by a facile and fast two-step electrochemical process. Structure and physicochemical properties of PtNPs/Ni-Al LDH/GCE were characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry and electrochemical methods. Then, electrocatalytic and stability characterizations of the PtNPs/Ni-Al LDH/GCE for methanol oxidation in alkaline media were investigated in detail by cyclic voltammetry, chronoamperometry, and chronopotentiometry measurements. PtNPs/Ni-Al LDH/GCE exhibited higher electrocatalytic activity than PtNPs/GCE and Ni-Al LDH/GCE. Also, the resulted chronoam-perograms indicated that the PtNPs/Ni-Al LDH/GCE has a better stability. Copyright © 2017 BCREC GROUP. All rights reserved Received: 30th March 2016; Revised: 29th July 2016; Accepted: 9th September 2016 How to Cite: Habibi, B., Ghaderi, S. (2017. Electro Synthesized Ni-Al Layered Double Hydroxide-Pt Nanoparticles as an Inorganic Nanocomposite and Potentate Anodic Material for Methanol Electro-Oxidation in Alkaline Media. Bulletin of Chemical Reaction Engineering & Catalysis, 12(1: 1-13 (doi:10.9767/bcrec.12.1.460.1-13 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.1.460.1-13

  16. Dissolvable layered double hydroxide coated magnetic nanoparticles for extraction followed by high performance liquid chromatography for the determination of phenolic acids in fruit juices.

    Science.gov (United States)

    Saraji, Mohammad; Ghani, Milad

    2014-10-31

    A magnesium-aluminum layered double hydroxide coated on magnetic nanoparticles was synthesized and used as a sorbent to extract some phenolic acids including p-hydroxy benzoic acid, caffeic acid, syringic acid, p-coumaric acid and ferulic acid from fruit juices. After extraction, the elution step was performed through dissolving double hydroxide layers containing the analytes by changing the solution pH. The extracted phenolic acids were separated and quantified using high performance liquid chromatography-photodiode array detection. Experimental parameters such as sorbent amount, solution pH, desorption solvent volume and extraction time were studied and optimized. The linearity range of the method was between 2 and 500μgL(-1) with the determination coefficient (r(2)) higher than 0.991. Relative standard deviations for intra- and inter-day precision for the analytes at 100μgL(-1) were in the range of 4.3-9.2% and 4.9-8.6%, respectively. Batch-to-batch reproducibility at 100μgL(-1) concentration level was in the range of 7.8-11% (n=3). The limits of detection were between 0.44 and 1.3μgL(-1). Relative recoveries higher than 81% with RSDs in the range of 4.2-9.7% were obtained in the analysis of fruit juice samples.

  17. Three dimensionally honeycomb layered double hydroxides framework as a novel fiber coating for headspace solid-phase microextraction of phenolic compounds.

    Science.gov (United States)

    Abolghasemi, Mir Mahdi; Yousefi, Vahid

    2014-06-06

    A new solid phase microextraction (SPME) fiber based on high-temperature three dimensionally honeycomb layered double hydroxide (TDH-LDH) material is presented. The fiber coating can be prepared easily, it is mechanically stable and exhibits relatively high thermal stability. This study shows that three dimensionally honeycomb layered double hydroxide generated porous morphology. The TDH-LDH material was tested for the extraction of some phenolic and polycyclic aromatic hydrocarbon compounds from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). The TDH-LDH fiber contains polar groups and its efficiency for non-polar polycyclic aromatic hydrocarbon compounds was lower than phenolic compounds. On the other hand, a high tendency towards the adsorption of polar phenolic compounds was observed for the proposed fiber. The effects of the extraction and desorption parameters including extraction temperature, extraction time, ionic strength, stirring rate, pH and desorption temperature and time have been studied. In optimum conditions, the repeatability for one fiber (n=5), expressed as relative standard deviation (R.S.D. %), was between 2.8% and 7.1% for the phenolic compounds. The detection limits for the studied phenolic compounds were between 0.02 and 5.8 ng mL(-1). The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis.

  18. In Vitro Inhibition of Histamine Release Behavior of Cetirizine Intercalated into Zn/Al- and Mg/Al-Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Muhammad Nazru