Photo-Catalytic Properties of TiO2 Supported on MWCNTs, SBA-15 and Silica-Coated MWCNTs Nanocomposites.

Science.gov (United States)

Ramoraswi, Nteseng O; Ndungu, Patrick G

2015-12-01

Mesoporous silica, specifically SBA-15, acid-treated multi-walled carbon nanotubes and a hybrid nanocomposite of SBA-15 coated onto the sidewalls acid-treated multi-walled carbon nanotubes (CNTs) were prepared and used as supports for anatase TiO2. Sol-gel methods were adapted for the synthesis of selected supports and for coating the materials with selected wt% loading of titania. Physical and chemical properties of the supports and catalyst composite materials were investigated by powder X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis, scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-vis diffuse reflectance spectroscopy and fluorescence spectroscopy. The photo-activity of the catalyst composites were evaluated on the decolorisation of methylene blue as a model pollutant. Coating CNTs with SBA-15 improved the thermal stability and textural properties of the nanotubes. All supported titania composites had high surface areas (207-301 m(2)/g), altered band gap energies and reduced TiO2 crystallite sizes. The TiO2/SBA-CNT composite showed enhanced photo-catalytic properties and activity than the TiO2/SBA-15 and TiO2/CNT composites. In addition, an interesting observation was noted with the TiO2/SBA-15 nanocomposites, which had a significantly greater photo-catalytic activity than the TiO2/CNT nanocomposites in spite of the high electron-hole recombination phenomena observed with the photoluminescence results. Discussions in terms of morphological, textural and physical-chemical aspects to account for the result are presented.

Size and spatial distribution of micropores in SBA-15 using CM-SANS

International Nuclear Information System (INIS)

Pollock, Rachel A.; Walsh, Brenna R.; Fry, Jason A.; Ghampson, Tyrone; Centikol, Ozgul; Melnichenko, Yuri B.; Kaiser, Helmut; Pynn, Roger; Frederick, Brian G.

2011-01-01

Diffraction intensity analysis of small-angle neutron scattering measurements of dry SBA-15 have been combined with nonlocal density functional theory (NLDFT) analysis of nitrogen desorption isotherms to characterize the micropore, secondary mesopore, and primary mesopore structure. The radial dependence of the scattering length density, which is sensitive to isolated surface hydroxyls, can only be modeled if the NLDFT pore size distribution is distributed relatively uniformly throughout the silica framework, not localized in a 'corona' around the primary mesopores. Contrast matching-small angle neutron scattering (CM-SANS) measurements, using water, decane, tributylamine, cyclohexane, and isooctane as direct probes of the size of micropores indicate that the smallest pores in SBA-15 have diameter between 5.7 and 6.2 (angstrom). Correlation of the minimum pore size with the onset of the micropore size distribution provides direct evidence that the shape of the smallest micropores is cylinderlike, which is consistent with their being due to unraveling of the polymer template.

Direct hydrothermal synthesis of iron-containing mesoporous silica SBA-15 : potential as a support for gold nanoparticles

NARCIS (Netherlands)

Li, Y.; Guan, Y.; Santen, van R.A.; Kooyman, P.J.; Dugulan, A.I.; Li, C.; Hensen, E.J.M.

2009-01-01

The preparation of mesoporous silica SBA-15 with high iron loadings (14-90 wt % Fe2O3) as a suitable support for gold nanoparticles to be used in CO oxidation catalysis has been investigated. The support materials were prepared by a direct hydrothermal two-step pH adjusting method which consisted of

The Multi-Template Molecularly Imprinted Polymer Based on SBA-15 for Selective Separation and Determination of Panax notoginseng Saponins Simultaneously in Biological Samples

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Chenghong Sun

2017-11-01

Full Text Available The feasible, reliable and selective multi-template molecularly imprinted polymers (MT-MIPs based on SBA-15 (SBA-15@MT-MIPs for the selective separation and determination of the trace level of ginsenoside Rb1 (Rb1, ginsenoside Rg1 (Rg1 and notoginsenoside R1 (R1 simultaneously from biological samples were developed. The polymers were constructed by SBA-15 as support, Rb1, Rg1, R1 as multi-template, acrylamide (AM as functional monomer and ethylene glycol dimethacrylate (EGDMA as cross-linker. The new synthetic SBA-15@MT-MIPs were satisfactorily applied to solid-phase extraction (SPE coupled with high performance liquid chromatography (HPLC for the separation and determination of trace Rb1, Rg1 and R1 in plasma samples. Under the optimized conditions, the limits of detection (LODs and quantitation (LOQs of the proposed method for Rb1, Rg1 and R1 were in the range of 0.63–0.75 ng·mL−1 and 2.1–2.5 ng·mL−1, respectively. The recoveries of R1, Rb1 and Rg1 were obtained between 93.4% and 104.3% with relative standard deviations (RSDs in the range of 3.3–4.2%. All results show that the obtained SBA-15@MT-MIPs could be a promising prospect for the practical application in the selective separation and enrichment of trace Panax notoginseng saponins (PNS in the biological samples.

Au and AuCu Nanoparticles Supported on SBA-15 Ordered Mesoporous Titania-Silica as Catalysts for Methylene Blue Photodegradation

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Isabel Barroso-Martín

2018-05-01

Full Text Available The photocatalytic degradation of methylene blue (MB dye has been performed under UV irradiation in aqueous suspension, employing photocatalysts based on Au (1.5 wt % and AuCu (Au/Cu = 1, 2.0 wt %, and supported on SBA-15-ordered mesoporous silica, with and without titania (Si/Ti = 3, in order to evaluate the versatility of this mesoporous support in this type of reaction of great impact from the environmental point of view. Samples were characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, N2 adsorption-desorption at −196 °C, and X-ray photoelectron spectroscopy (XPS, so as to study their structural, optical, and chemical properties. All the prepared catalysts were found to be active in the test reaction. The bimetallic AuCu-based catalysts attained very high MB degradation values, in particular AuCu/SBA-15 titania-silica sample reached 100% of dye oxidation after the monitored reaction period (120 min.

Development of TREN dendrimers over mesoporous SBA-15 for CO2 adsorption

International Nuclear Information System (INIS)

Bhagiyalakshmi, Margandan; Park, Sang Do; Cha, Wang Seog; Jang, Hyun Tae

2010-01-01

Mesoporous SBA-15 was synthesized using rice husk ash (RHA) as the silica source and their defective Si-OH groups were grafted with tris(2-aminoethyl) amine (TREN) dendrimers generation through step-wise growth technique. The X-ray diffraction (XRD) and nitrogen adsorption/desorption results of parent SBA-15 obtained from RHA, suggests its resemblance with SBA-15 synthesized using conventional silica sources. Furthermore, the nitrogen adsorption/desorption results of SBA-15/TREN dendrimer generations (G1-G3) illustrates the growth of dendrimer inside the mesopores of SBA-15 and their CO 2 adsorption capacity was determined at 25 deg. C. The maximum CO 2 adsorption capacity of 5-6 and 7-8 wt% over second and third dendrimer generation was observed which is discernibly higher than the reported melamine and PAMAM dendrimers. The experimental CO 2 adsorption capacity was found to be less than theoretically calculated CO 2 adsorption capacity due to inter and intra molecular amidation as result of steric hindrance during the dendrimer growth. These SBA-15/TREN dendrimer generations also exhibit thermal stability up to 350 deg. C and CO 2 adsorption capacity remains unaltered upon seven consecutive runs.

Immobilization of lipase and keratinase on functionalized SBA-15 nanostructured materials

Science.gov (United States)

Le, Hy G.; Vu, Tuan A.; Tran, Hoa T. K.; Dang, Phuong T.

2013-12-01

SBA-15 nanostructured materials were synthesized via hydrothermal treatment and were functionalized with 3- aminopropyltriethoxysilane (APTES). The obtained samples were characterized by different techniques such as XRD, BET, TEM, IR and DTA. After functionalization, it showed that these nanostrucrured materials still maintained the hexagonal pore structure of the parent SBA-15. The model enzyms chosen in this study were lipase and keratinase. Lipase was a biocatalyst for hydrolyzation of long chain triglycerides or methyl esters of long chain alcohols and fatty acids; keratinase is a proteolytic enzyme that catalyzes the cleavage of keratin. The functionalized SBA-15 materials were used to immobilize lipase and keratinase, exhibiting higher activity than that of the unfunctionalized pure silica SBA-15 ones. This might be due to the enhancing of surface hydrophobicity upon functionalization. The surface functionalization of the nanostructured silicas with organic groups can favor the interaction between enzyme and the supports and consequently increasing the operational stability of the immobilized enzymes. The loading of lipase on functionalized SBA-15 materials was higher than that of keratinase. This might be rationalized by the difference in size of enzyms.

Characterization and comprehension of zeolite NaY/mesoporous SBA-15 composite as adsorbent for paraquat

Energy Technology Data Exchange (ETDEWEB)

Osakoo, Nattawut, E-mail: natawut.work@gmail.com [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Pansakdanon, Chaianun [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Department of Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 (Thailand); Sosa, Narongrit; Deekamwong, Krittanun; Keawkumay, Chalermpan; Rongchapo, Wina [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Chanlek, Narong [Synchrotron Light Research Institute, Nakhon Ratchasima, 30000 (Thailand); Jitcharoen, Juthamas [Department of Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 (Thailand); Prayoonpokarach, Sanchai [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand); Wittayakun, Jatuporn, E-mail: jatuporn@g.sut.ac.th [School of Chemistry, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima, 30000 (Thailand)

2017-06-01

NaY was synthesized from fumed silica and further modified to form a composite with SBA-15. Textural properties and basicity of the composite NaY-SBA-15 were between those of the parent materials. Paraquat adsorption on NaY was 204.1 mg/g, higher than that on NaY synthesized with rice husk silica from the previous work. SBA-15 was a poor adsorbent for paraquat. Based on the weight of NaY, the adsorption capacity of analytical-grade paraquat on the NaY-SBA-15 composite was 241.5 mg/g-NaY. Moreover, the composite adsorbed blue dye from a commercial grade paraquat. Interaction between the NaY-SBA-15 and paraquat could be from C and N atoms in paraquat with oxygen atom on NaY-SBA-15. - Highlights: • Zeolite NaY/mesoporous SBA-15 composite was synthesized with a simple method. • NaY and SBA-15 coexisted in the composite confirmed by FTIR, CO{sub 2}-TPD and XPS. • Adsorption capacity of paraquat (mg/g-NaY) was improved by NaY and SBA-15 composite. • C and N atoms in paraquat could interact with oxygen atom on NaY-SBA-15 composite.

Preparation of mesoporous silica films SBA-15 over different substrates

International Nuclear Information System (INIS)

Campos, V.O.; Sousa, E.M.B. de; Macedo, W.A.A.

2010-01-01

Mesoporous materials have been target of frequent interest due to its wide application possibilities, for example development of gas sensors, catalysis, molecules transportation, pharmaceuticals release, synthesis of auto-organized nanostructures, among others. The possibilities of application are enhanced when such materials are disposed in the form of thin and ultrathin films. In this work the preparation of mesoporous SBA-15 silica films is explored by means of the dipcoating technique of a sol-gel on different substrates (glass slides, stainless steel, copper), using the surfactant poly(ethylene glycol)-block-poly(propylene glycol)- block-poly(ethylene glycol), known as P123, a block copolymer. Synthesis parameters surfactant concentration, aging time and temperature were investigated. In this work we present the morphological and structural characterization of the prepared films, which were obtained using atomic force microscopy and x-ray fluorescence and diffraction. (author)

Physical properties of ordered mesoporous SBA-15 silica as immunological adjuvant

Science.gov (United States)

Mariano-Neto, F.; Matos, J. R.; Cides da Silva, L. C.; Carvalho, L. V.; Scaramuzzi, K.; Sant'Anna, O. A.; Oliveira, C. P.; Fantini, M. C. A.

2014-10-01

This work reports a detailed analysis of the ordered mesoporous SBA-15 silica synthesis procedure that provides a matrix with mean pore diameter around 10 nm. The encapsulation of bovine serum albumin (BSA) by four different methods allowed the determination of the best imbibition condition, which is keeping the mixture under rest and solvent evaporation. Simulation of the in situ SAXS scattered intensity of the BSA release in potassium buffer solution, gastrointestinal fluids revealed a slow evolution of BSA content, independent of the media. Proton induced x-ray emission results obtained in calcined mouse organs revealed that silica is only present in the spleen after 35 days and is completely eliminated from all mouse organs after 10 weeks. Biological studies showed that Santa Barbara Amorphous-15 is an effective adjuvant when compared to the traditional Al(OH)3, and is non-toxic to mice, rats, dogs and even cells, such as macrophages and dendritic cells. Recent studies showed that the immunological response is improved by enhancing the inflammatory response and the recruitment of immune competent cells to the site of injection as by the oral route and, most importantly, by increasing the number of phagocytes of a particulate antigen by antigen presenting cells. This research is under the scope of the International Patent WO 07030901, IN248654,ZA2008/02277, KR 1089400, MX297263, JP5091863, CN101287491B.

In Situ Loading of Drugs into Mesoporous Silica SBA-15.

Science.gov (United States)

Wan, Mi Mi; Li, Yan Yan; Yang, Tian; Zhang, Tao; Sun, Xiao Dan; Zhu, Jian Hua

2016-04-25

In a new strategy for loading drugs into mesoporous silica, a hydrophilic (heparin) or hydrophobic drug (ibuprofen) is encapsulated directly in a one-pot synthesis by evaporation-induced self-assembly. In situ drug loading significantly cuts down the preparation time and dramatically increases the loaded amount and released fraction of the drug, and appropriate drug additives favor a mesoporous structure of the vessels. Drug loading was verified by FTIR spectroscopy and release tests, which revealed much longer release with a larger amount of heparin or ibuprofen compared to postloaded SBA-15. Besides, the in vitro anticoagulation properties of the released heparin and the biocompatibility of the vessels were carefully assessed, including activated partial thromboplastin time, thrombin time, hemolysis, platelet adhesion experiments, and the morphologies of red blood cells. A concept of new drug-release agents with soft core and hard shell is proposed and offers guidance for the design of novel drug-delivery systems. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fe3O4@mesoporous SBA-15: A magnetically recoverable catalyst for photodegradation of malachite green

International Nuclear Information System (INIS)

Aliyan, Hamid; Fazaeli, Razieh; Jalilian, Rahil

2013-01-01

Surface of mesostructured silica (SBA-15) was modified by immobilizing Fe 3 O 4 . This modified-nanosized mesoporous silica Fe 3 O 4 @SBA-15 was characterized by FTIR, XRD, BET and SEM. A comparison of the photoefficiency of Fe 3 O 4 @SBA-15 toward photodegradation of malachite green (MG) was investigated in a photocatalytic reactor using UV lamp as a light source. The effect of various experimental parameters on the degradation performance of the process was evaluated by examining catalyst dosage, initial dye concentration and pH of the dye solution in the presence of Fe 3 O 4 @SBA-15 as photocatalyst. It was found that the photocatalyst exhibited significantly high catalytic stability, and the activity loss is negligible after five MG degradation cycles.

Inclusion of cefalexin in SBA-15 mesoporus material and release property

International Nuclear Information System (INIS)

Zhai, Qing-Zhou

2012-01-01

SBA-15 (Santa Barbara Amorphous-15) is a high ordered mesoporous material. It has the advantages of a non-toxic property, good hydrothermal stability and thermal stability, etc. Inside inner surface a lot of silanols exist. Pore diameter size is uniform and pore size distribution is narrow. This structural feature makes SBA-15 have a higher loading drug amount and be able to effectively extend the drug release cycle. In this paper, polyethylene glycol-block-polypropylene glycol-block-polyethylene glycol was used as template and tetraethyl orthosilicate was used as silica source to prepare SBA-15 by hydrothermal synthesis method. Cefalexin was included in SBA-15 and the included cefalexin drug content was 158.72 mg/g. The composite materials were characterized by using chemical analysis, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared (IR) spectroscopy, and low temperature nitrogen adsorption–desorption. The results showed that cefalexin had been successfully included in host SBA-15 pore channels. Rational analyses of the release processes of cefalexin drug from the pores of SBA-15 to the simulated body fluid, simulated gastric juice and simulated intestinal fluid were made and sustained-release effects of the drug in complex system were studied. The results showed that in simulated body fluid within 1–5 h cefalexin was fast released and the cumulative release reached 50.00% at 5 h. In 15–20 h, the sustained release speed of cefalexin drug in the composite material decreased and the sustained-release cumulative amount reached 99.87% at 20 h. The release of cefalexin was basically complete. In simulated gastric fluid, composite material sustained-release ended at 4 h, the cumulative sustained release ratio reaching 26.10%. In simulated gastric fluid, the sustained-release was complete at 7 h, the cumulative sustained release ratio reaching 32.46%. The composite material of SBA-15 and cefalexin

Determination of Thallium(I by Hybrid Mesoporous Silica (SBA-15 Modified Electrode

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Geeta Rani

2016-01-01

Full Text Available Chemically modified mesoporous silica material (SBA-15 was used for the construction of Tl(I selective carbon paste electrode. The best response was found with the electrode containing 10% modifier as electrode material. The electrode has a lower detection limit of 6.0 × 10−9 M in a working concentration range of 1.0 × 10−8–1.0 × 10−1 M. The selectivity coefficient calculated by match potential method (MPM shows the high selectivity of electrode towards Tl(I over other tested ions. The electrode was successfully applied as an indicator electrode for the titration of 0.01 M TlNO3 solution with standards EDTA solution and for sequential titration of mixture of different anions.

Physical state of poorly water soluble therapeutic molecules loaded into SBA-15 ordered mesoporous silica carriers: a case study with itraconazole and ibuprofen.

Science.gov (United States)

Mellaerts, Randy; Jammaer, Jasper A G; Van Speybroeck, Michiel; Chen, Hong; Van Humbeeck, Jan; Augustijns, Patrick; Van den Mooter, Guy; Martens, Johan A

2008-08-19

The ordered mesoporous silica material SBA-15 was loaded with the model drugs itraconazole and ibuprofen using three different procedures: (i) adsorption from solution, (ii) incipient wetness impregnation, and (iii) heating of a mixture of drug and SBA-15 powder. The location of the drug molecules in the SBA-15 particles and molecular interactions were investigated using nitrogen adsorption, TGA, DSC, DRS UV-vis, and XPS. The in vitro release of hydrophobic model drugs was evaluated in an aqueous environment simulating gastric fluid. The effectiveness of the loading method was found to be strongly compound dependent. Incipient wetness impregnation using a concentrated itraconazole solution in dichloromethane followed by solvent evaporation was most efficient for dispersing itraconazole in SBA-15. The itraconazole molecules were located on the mesopore walls and inside micropores of the mesopore walls. When SBA-15 was loaded by slurrying it in a diluted itraconazole solution from which the solvent was evaporated, the itraconazole molecules ended up in the mesopores that they plugged locally. At a loading of 30 wt %, itraconazole exhibited intermolecular interactions inside the mesopores revealed by UV spectroscopy and endothermic events traced with DSC. The physical mixing of itraconazole and SBA-15 powder followed by heating above the itraconazole melting temperature resulted in formulations in which glassy itraconazole particles were deposited externally on the SBA-15 particles. Loading with ibuprofen was successful with each of the three loading procedures. Ibuprofen preferably is positioned inside the micropores. In vitro release experiments showed fast release kinetics provided the drug molecules were evenly deposited over the mesoporous surface.

Study on the adsorption of heavy metal ions from aqueous solution on modified SBA-15

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Liliana Giraldo

2013-01-01

Full Text Available Amino-functionalized SBA-15 mesoporous silica was prepared, characterized, and used as an adsorbent for heavy metal ions. The organic - inorganic hybrid material was obtained by a grafting procedure using SBA-15 silica with 3-aminopropyl-triethoxysilane and bis(2,4,4-trimethylpentyl phosphinic acid (Cyanex 272, respectively. The structure and physicochemical properties of the materials were characterized by means of elemental analysis, X-ray diffraction (XRD, nitrogen adsorption - desorption, thermogravimetric analysis, FTIR spectroscopy and immersion calorimetry. The organic functional groups were successfully grafted onto the SBA-15 surface and the ordering of the support was not affected by the chemical modification. The behavior of the grafted solids was investigated for the adsorption of heavy metal ions from aqueous solutions. The hybrid materials showed high adsorption capacity and high selectivity for zinc ions. Other ions, such as cooper and cobalt were absorbed by the modified SBA-15 material.

SBA-15 mesoporous silica free-standing thin films containing copper ions bounded via propyl phosphonate units - preparation and characterization

Energy Technology Data Exchange (ETDEWEB)

Laskowski, Lukasz, E-mail: lukasz.laskowski@kik.pcz.pl [Czestochowa University of Technology, Institute of Computational Intelligence, Unit of Microelectronics and Nanotechnology, Al. Armii Krajowej 36, 42–201 Czestochowa (Poland); Laskowska, Magdalena, E-mail: magdalena.laskowska@onet.pl [H. Niewodniczanski Institute of Nuclear Physics, Polish Academy of Sciences, 31-342 Krakow, ul. Radzikowskiego 152 (Poland); Jelonkiewicz, Jerzy, E-mail: jerzy.jelonkiewicz@kik.pcz.pl [Czestochowa University of Technology, Institute of Computational Intelligence, Unit of Microelectronics and Nanotechnology, Al. Armii Krajowej 36, 42–201 Czestochowa (Poland); Dulski, Mateusz, E-mail: mateusz.dulski@us.edu.pl [University of Silesia, Faculty of Computer Science and Materials Science, Institute of Materials Science, Silesian Center for Education and Interdisciplinary Research, ul. 75 Pułku Piechoty 1A, 41–500 Chorzów (Poland); Wojtyniak, Marcin, E-mail: marcin.wojtyniak@us.edu.pl [University of Silesia, Institute of Physics, Silesian Center for Education and Interdisciplinary Research, ul. 75 Pułku Piechoty 1A, 41–500 Chorzów (Poland); Fitta, Magdalena, E-mail: magdalena.fitta@ifj.edu.pl [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, 31–342 Krakow, ul. Radzikowskiego 152 (Poland); Balanda, Maria, E-mail: Maria.Balanda@ifj.edu.pl [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, 31–342 Krakow, ul. Radzikowskiego 152 (Poland)

2016-09-15

The SBA-15 silica thin films containing copper ions anchored inside channels via propyl phosphonate groups are investigated. Such materials were prepared in the form of thin films, with hexagonally arranged pores, laying rectilinear to the substrate surface. However, in the case of our thin films, their free standing form allowed for additional research possibilities, that are not obtainable for typical thin films on a substrate. The structural properties of the samples were investigated by X-ray reflectometry, atomic force microscopy (AFM) and transmission electron microscopy (TEM). The molecular structure was examined by Raman spectroscopy supported by numerical simulations. Magnetic measurements (SQUID magnetometry and EPR spectroscopy) showed weak antiferromagnetic interactions between active units inside silica channels. Consequently, the pores arrangement was determined and the process of copper ions anchoring by propyl phosphonate groups was verified in unambiguous way. Moreover, the type of interactions between magnetic atoms was determined. - Highlights: • Functionalized free-standing SBA-15 thin films were synthesized for a first time. • Thin films synthesis procedure was described in details. • Structural properties of the films were thoroughly investigated and presented. • Magnetic properties of the novel material was investigated and presented.

Research on the Ordered Mesoporous Silica for Tobacco Harm Reduction

Science.gov (United States)

Wang, Y.; Y Li, Z.; Ding, J. X.; Hu, Z. J.; Liu, Z.; Zhou, G.; Huang, T. H.

2017-12-01

For reducting tobacco harm, this paper prepared an ordered mesoporous silica by using triblock copolymer Pluronic P123 as template. The property of this material was characterized by the X-ray scattering spectrum(XRD), Transmission electron microscopy(TEM), Scanning electron microscopy (SEM) and Nitrogen adsorption/desorption. Then this ordered mesoporous silica was added into the cigarette filter in order to researching its effect of cigarette harm index. The result shows that the feature of SBA-15 was grain morphology, ordered arrangement, tubular porous 2-D hexagonal structure. The application of SBA-15 in cigarette filter can selectively reduce harmful components in cigarette smoke such as crotonaldehyde, hydrogen cyanide, benzo pyrene and tar. The synthesized SBA-15 could properly reduce cigarette harm index.

Hydroxyapatite/MCM-41 and SBA-15 Nano-Composites: Preparation, Characterization and Applications

Science.gov (United States)

Anunziata, Oscar A.; Martínez, Maria L.; Beltramone, Andrea R.

2009-01-01

Composites of hydroxyapatite (HaP) and highly ordered large pore mesoporous silica molecular sieves such as, Al-SBA-15 and Al-MCM-41 (denoted as SBA-15 and MCM-41, respectively) were developed, characterized by XRD, BET, FTIR, HRTEM and NMR-MAS, and applied to fluoride retention from contaminated water. The proposed procedure by a new route to prepare the HaP/SBA-15 and HaP/MCM-41, composites generates materials with aluminum only in tetrahedral coordination, according to the 27Al NMR-MAS results. Free OH- groups of HaP nanocrystals, within the hosts, allowed high capacity fluoride retention. The activity of fluoride retention using HaP/MCM-41 or HaP/SBA-15 was 1-2 orders of magnitude greater, respectively, than with pure HaP.

Fluorescence properties of riboflavin-functionalized mesoporous silica SBA-15 and riboflavin solutions in presence of different metal and organic cations

Science.gov (United States)

Lewandowski, Dawid; Schroeder, Grzegorz; Sawczak, Mirosław; Ossowski, Tadeusz

2015-10-01

Riboflavin was covalently linked to mesoporous SBA-15 silica surface via grafting technique. Then fluorescence properties of the system obtained were analyzed in the presence of several metal and organic cations. Both quenching and strengthening of fluorescence as well as significant changes in the maximum fluorescence wavelength were observed. The results were compared with absorption and fluorescence data obtained for riboflavin water solutions.

Preparation and characterization of glycidyl methacrylate organo bridges grafted mesoporous silica SBA-15 as ibuprofen and mesalamine carrier for controlled release

Energy Technology Data Exchange (ETDEWEB)

Rehman, Fozia, E-mail: fozia@iqm.unicamp.br [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil); Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Rahim, Abdur [Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Airoldi, Claudio; Volpe, Pedro L.O. [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil)

2016-02-01

Mesoporous silica SBA-15 was synthesized and functionalized with bridged polysilsesquioxane monomers obtained by the reaction of 3-aminopropyltriethoxy silane with glycidyl methacrylate in 2:1 ratio. The synthesized mesoporous silica materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-ray diffraction, thermogravimetry and scanning electron microscopy. The nuclear magnetic resonance in the solid state is in agreement with the sequence of carbon distributed in the attached organic chains, as expected for organically functionalized mesoporous silica. After functionalization with organic bridges the BET surface area was reduced from 1311.80 to 494.2 m{sup 2} g{sup −1} and pore volume was reduced from 1.98 to 0.89 cm{sup 3} g{sup −1}, when compared to original precursor silica. Modification of the silica surface with organic bridges resulted in high loading capacity and controlled release of ibuprofen and mesalamine in biological fluids. The Korsmeyer–Peppas model better fits the release data indicating Fickian diffusion and zero order kinetics for synthesized mesoporous silica. The drug release rate from the modified silica was slow in simulated gastric fluid, (pH 1.2) where less than 10% of mesalamine and ibuprofen were released in initial 8 h, while comparatively high release rates were observed in simulated intestinal (pH 6.8) and simulated body fluids (pH 7.2). The preferential release of mesalamine at intestinal pH suggests that the modified silica could be a simple, efficient, inexpensive and convenient carrier for colon targeted drugs, such a mesalamine and also as a controlled drug release system. - Highlights: • Modified SBA-15 silica with long hydrophobic chains was evaluated as drug carrier. • This silica showed improved loading capacity and controlled release of ibuprofen. • Compared to gastric pH high release rate of mesalamine was observed at colonic pH. �

Preparation and characterization of glycidyl methacrylate organo bridges grafted mesoporous silica SBA-15 as ibuprofen and mesalamine carrier for controlled release

International Nuclear Information System (INIS)

Rehman, Fozia; Rahim, Abdur; Airoldi, Claudio; Volpe, Pedro L.O.

2016-01-01

Mesoporous silica SBA-15 was synthesized and functionalized with bridged polysilsesquioxane monomers obtained by the reaction of 3-aminopropyltriethoxy silane with glycidyl methacrylate in 2:1 ratio. The synthesized mesoporous silica materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-ray diffraction, thermogravimetry and scanning electron microscopy. The nuclear magnetic resonance in the solid state is in agreement with the sequence of carbon distributed in the attached organic chains, as expected for organically functionalized mesoporous silica. After functionalization with organic bridges the BET surface area was reduced from 1311.80 to 494.2 m 2 g −1 and pore volume was reduced from 1.98 to 0.89 cm 3 g −1 , when compared to original precursor silica. Modification of the silica surface with organic bridges resulted in high loading capacity and controlled release of ibuprofen and mesalamine in biological fluids. The Korsmeyer–Peppas model better fits the release data indicating Fickian diffusion and zero order kinetics for synthesized mesoporous silica. The drug release rate from the modified silica was slow in simulated gastric fluid, (pH 1.2) where less than 10% of mesalamine and ibuprofen were released in initial 8 h, while comparatively high release rates were observed in simulated intestinal (pH 6.8) and simulated body fluids (pH 7.2). The preferential release of mesalamine at intestinal pH suggests that the modified silica could be a simple, efficient, inexpensive and convenient carrier for colon targeted drugs, such a mesalamine and also as a controlled drug release system. - Highlights: • Modified SBA-15 silica with long hydrophobic chains was evaluated as drug carrier. • This silica showed improved loading capacity and controlled release of ibuprofen. • Compared to gastric pH high release rate of mesalamine was observed at colonic pH. • Modified silica

Preparation of Pd-Diimine@SBA-15 and Its Catalytic Performance for the Suzuki Coupling Reaction

Directory of Open Access Journals (Sweden)

Jiahuan Yu

2016-11-01

Full Text Available A highly efficient and stable Pd-diimine@SBA-15 catalyst was successfully prepared by immobilizing Pd onto diimine-functionalized mesoporous silica SBA-15. With the help of diimine functional groups grafted onto the SBA-15, Pd could be anchored on a support with high dispersion. Pd-diimine@SBA-15 catalyst exhibited excellent catalytic performance for the Suzuki coupling reaction of electronically diverse aryl halides and phenylboronic acid under mild conditions with an ultralow amount of Pd (0.05 mol % Pd. When the catalyst amount was increased, it could catalyze the coupling reaction of chlorinated aromatics with phenylboronic acid. Compared with the catalytic performances of Pd/SBA-15 and Pd-diimine@SiO2 catalysts, the Pd-diimine@SBA-15 catalyst exhibited higher hydrothermal stability and could be repeatedly used four times without a significant decrease of its catalytic activity.

Organically functionalized mesoporous SBA-15 as sorbents for removal of selected pharmaceuticals from water

Energy Technology Data Exchange (ETDEWEB)

Bui, Tung Xuan [School of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of); Kang, Seo-Young [International Environmental Research Center (IERC), Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of); Lee, Sang-Hyup [Water Environment Center, Korea Institute of Science and Technology, Cheongryang, Seoul 130-650 (Korea, Republic of); Choi, Heechul, E-mail: hcchoi@gist.ac.kr [School of Environmental Science and Engineering, Gwangju Institute of Science and Technology (GIST), 261 Cheomdan-gwagiro, Buk-gu, Gwangju 500-712 (Korea, Republic of)

2011-10-15

Highlights: {yields} SBA-15 grafted with aminopropyl, hydroxymethyl, and trimethylsilyl groups as sorbents. {yields} Sorbents for removal of a mixture of 12 pharmaceuticals from water. {yields} Hydroxymethyl-SBA-15 shows similar adsorption efficiency like SBA-15. {yields} Aminopropyl-SBA-15 makes increase for clofibric acid, diclofenac, decrease for atenolol, estrone, trimethoprim. {yields} Trimethylsilyl-SBA-15 makes increase for 9 compounds; 7 compounds from 70.6% to 98.9%. - Abstract: Mesoporous silica SBA-15 and its postfunctionalized counterparts with hydroxymethyl (HM-SBA-15), aminopropyl (AP-SBA-15), and trimethylsilyl (TMS-SBA-15) were prepared and characterized by powder X-ray diffraction, N{sub 2} adsorption-desorption measurement, Fourier-transform infrared spectroscopy, and elemental analysis. The removal of a mixture of 12 selected pharmaceuticals was investigated by batch adsorption experiments onto SBA-15 and the grafted materials. SBA-15 showed to have moderate adsorption affinity with amino-containing (atenolol, trimethoprim) and hydrophobic pharmaceuticals, but it displayed minimal adsorption affinity toward hydrophilic compounds. HM-SBA-15 was analogous with SBA-15 in terms of the adsorption efficiency toward all pharmaceuticals. AP-SBA-15 exhibited an increase in the adsorption of two acidic compounds (clofibric acid, diclofenac) but a decrease in the adsorption of estrone and the two amino-containing compounds. Among the grafted materials, TMS-SBA-15 had the highest adsorption affinity toward most pharmaceuticals. Moreover, the adsorption of nine pharmaceuticals to TMS-SBA-15 was significantly higher than that to SBA-15; seven of which showed the removal percentages from 70.6% to 98.9% onto TMS-SBA-15. The number of pharmaceuticals showing high adsorption efficiency onto TMS-SBA-15 did not alter significantly as the pH changed in the range of 5.5-7.6. The results suggest that TMS-SBA-15 is a promising material for the removal of pharmaceuticals

Organically functionalized mesoporous SBA-15 as sorbents for removal of selected pharmaceuticals from water

International Nuclear Information System (INIS)

Bui, Tung Xuan; Kang, Seo-Young; Lee, Sang-Hyup; Choi, Heechul

2011-01-01

Highlights: → SBA-15 grafted with aminopropyl, hydroxymethyl, and trimethylsilyl groups as sorbents. → Sorbents for removal of a mixture of 12 pharmaceuticals from water. → Hydroxymethyl-SBA-15 shows similar adsorption efficiency like SBA-15. → Aminopropyl-SBA-15 makes increase for clofibric acid, diclofenac, decrease for atenolol, estrone, trimethoprim. → Trimethylsilyl-SBA-15 makes increase for 9 compounds; 7 compounds from 70.6% to 98.9%. - Abstract: Mesoporous silica SBA-15 and its postfunctionalized counterparts with hydroxymethyl (HM-SBA-15), aminopropyl (AP-SBA-15), and trimethylsilyl (TMS-SBA-15) were prepared and characterized by powder X-ray diffraction, N 2 adsorption-desorption measurement, Fourier-transform infrared spectroscopy, and elemental analysis. The removal of a mixture of 12 selected pharmaceuticals was investigated by batch adsorption experiments onto SBA-15 and the grafted materials. SBA-15 showed to have moderate adsorption affinity with amino-containing (atenolol, trimethoprim) and hydrophobic pharmaceuticals, but it displayed minimal adsorption affinity toward hydrophilic compounds. HM-SBA-15 was analogous with SBA-15 in terms of the adsorption efficiency toward all pharmaceuticals. AP-SBA-15 exhibited an increase in the adsorption of two acidic compounds (clofibric acid, diclofenac) but a decrease in the adsorption of estrone and the two amino-containing compounds. Among the grafted materials, TMS-SBA-15 had the highest adsorption affinity toward most pharmaceuticals. Moreover, the adsorption of nine pharmaceuticals to TMS-SBA-15 was significantly higher than that to SBA-15; seven of which showed the removal percentages from 70.6% to 98.9% onto TMS-SBA-15. The number of pharmaceuticals showing high adsorption efficiency onto TMS-SBA-15 did not alter significantly as the pH changed in the range of 5.5-7.6. The results suggest that TMS-SBA-15 is a promising material for the removal of pharmaceuticals from aqueous phase

Highly Sensitive Fluorescence Probe Based on Functional SBA-15 for Selective Detection of Hg2+

Directory of Open Access Journals (Sweden)

Wang Xiaoyu

2010-01-01

Full Text Available Abstract An inorganic–organic hybrid fluorescence chemosensor (DA/SBA-15 was prepared by covalent immobilization of a dansylamide derivative into the channels of mesoporous silica material SBA-15 via (3-aminopropyltriethoxysilane (APTES groups. The primary hexagonally ordered mesoporous structure of SBA-15 was preserved after the grafting procedure. Fluorescence characterization shows that the obtained inorganic–organic hybrid composite is highly selective and sensitive to Hg2+ detection, suggesting the possibility for real-time qualitative or quantitative detection of Hg2+ and the convenience for potential application in toxicology and environmental science.

Synthesis of α-MoC1-x Nanoparticles with a Surface-Modified SBA-15 Hard Template: Determination of Structure-Function Relationships in Acetic Acid Deoxygenation.

Science.gov (United States)

Baddour, Frederick G; Nash, Connor P; Schaidle, Joshua A; Ruddy, Daniel A

2016-07-25

Surface modification of mesoporous SBA-15 silica generated a hydrophobic environment for a molybdenum diamine (Mo-diamine) precursor solution, enabling direct growth of isolated 1.9±0.4 nm α-MoC1-x nanoparticles (NPs) inside the pores of the support. The resulting NP catalysts are bifunctional, and compared to bulk α-MoC1-x and β-Mo2 C, the NPs exhibit a greater acid-site:H-site ratio and a fraction of stronger acid sites. The greater acid-site:H-site ratio results in higher decarbonylation (DCO) selectivity during acetic acid hydrodeoxygenation (HDO) reactions, and the stronger acid sites lead to higher activity and ketonization (KET) selectivity at high temperatures. The hard-templating synthetic method could be a versatile route toward carbide NPs of varying size, composition, and phase, on a range of mesoporous oxide supports. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Carbon material formation on SBA-15 and Ni-SBA-15 and residue constituents during acetylene decomposition

Energy Technology Data Exchange (ETDEWEB)

Chiang, Hung-Lung, E-mail: hlchiang@mail.cmu.edu.tw [Department of Risk Management, China Medical University, Taichung 40402, Taiwan (China); Wu, Trong-Neng [Department of Public Health, China Medical University, Taichung 40402, Taiwan (China); Ho, Yung-Shou [Department of Applied Chemistry and Materials Science, Fooyin University, Kaohsiung 831, Taiwan (China); Zeng, Li-Xuan [Department of Risk Management, China Medical University, Taichung 40402, Taiwan (China)

2014-07-15

Highlights: • Acetylene was decomposed on SBA-15 and Ni-SBA-15 at 650–850 °C. • Carbon spheres and filaments were formed after acetylene decomposition. • PAHs were determined in tar and residues. • Exhaust constituents include CO{sub 2}, H{sub 2}, NO{sub x} and hydrocarbon species. - Abstract: Carbon materials including carbon spheres and nanotubes were formed from acetylene decomposition on hydrogen-reduced SBA-15 and Ni-SBA-15 at 650–850 °C. The physicochemical characteristics of SBA-15, Ni-SBA-15 and carbon materials were analyzed by field emission scanning electronic microscopy (FE-SEM), Raman spectrometry, and energy dispersive spectrometry (EDS). In addition, the contents of polyaromatic hydrocarbons (PAHs) in the tar and residue and volatile organic compounds (VOCs) in the exhaust were determined during acetylene decomposition on SBA-15 and Ni-SBA-15. Spherical carbon materials were observed on SBA-15 during acetylene decomposition at 750 and 850 °C. Carbon filaments and ball spheres were formed on Ni-SBA-15 at 650–850 °C. Raman spectroscopy revealed peaks at 1290 (D-band, disorder mode, amorphous carbon) and 1590 (G-band, graphite sp{sup 2} structure) cm{sup −1}. Naphthalene (2 rings), pyrene (4 rings), phenanthrene (3 rings), and fluoranthene (4 rings) were major PAHs in tar and residues. Exhaust constituents of hydrocarbon (as propane), H{sub 2}, and C{sub 2}H{sub 2} were 3.9–2.6/2.7–1.5, 1.4–2.8/2.6–4.3, 4.2–2.4/3.2–1.7% when acetylene was decomposed on SBA-15/Ni-SBA-15, respectively, corresponding to temperatures ranging from 650 to 850 °C. The concentrations of 52 VOCs ranged from 9359 to 5658 and 2488 to 1104 ppm for SBA-15 and Ni-SBA-15 respectively, at acetylene decomposition temperatures from 650 to 850 °C, and the aromatics contributed more than 87% fraction of VOC concentrations.

Synthesis of Pt-Sn core-shell nanoparticles deposited on SBA-15 modified

Energy Technology Data Exchange (ETDEWEB)

Alvarez-Contreras, L.; Alonso-Lemus, I. [Centro de Investigacion en Materiales Avanzados S.C., Laboratorio Nacional de Nanotecnologia (Mexico); Botte, G. G. [Ohio University, Center for Electrochemical Engineering Research, Department of Chemical and Biomolecular Engineering (United States); Verde-Gomez, Y., E-mail: ysmaelverde@yahoo.com [Instituto Tecnologico de Cancun (Mexico)

2013-07-15

A novel one-step synthesis method to prepare Pt-Sn bimetallic nanoparticles supported on mesoporous silica with high surface area (SBA-15, 700 m{sup 2}/g) and narrow pore size distribution (around 9.5 nm) was developed. Tin incorporation plays an important dual role, to create active sites into the silica walls that serve as particles anchors center, and to grow Pt-Sn core-shell nanoparticles. High-resolution transmission and scanning electron microscopy, and X-ray diffraction pattern confirm the formation of the Pt-Sn core-shell type nanoparticles ( Almost-Equal-To 1-10 nm). The metal loading was 2.2 and 2.3 wt% for Pt and Sn, respectively. Electron microscopy results show that the metal nanoparticles were deposited not only on the matrix, but also inside of it. Structural, textural, and morphological features of the SBA-15 were slightly affected after the nanoparticles deposition, maintaining its high surface area. The results obtained suggest that Pt-Sn on SBA-15 could be attractive material for several catalytic applications, due to the narrow particle size distribution achieved (from 1 to 10 nm) the high dispersion on the support, as well as the Pt-Sn alloy developed.Graphical Abstract.

Effect of silica/titania ratio on enhanced photooxidation of industrial hazardous materials by microwave treated mesoporous SBA-15/TiO{sub 2} nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Mehta, Akansha; Mishra, Amit; Sharma, Manisha; Singh, Satnam; Basu, Soumen, E-mail: soumen.basu@thapar.edu [Thapar University, School of Chemistry and Biochemistry (India)

2016-07-15

In this study microwave assisted technique has been adopted for the synthesis of different weight ratios of TiO{sub 2} dispersed on Santa barbara amorphous-15 (SBA-15) support. Morphological study revealed TiO{sub 2} particles (4–10 nm) uniformly distributed on SBA-15 while increases in SBA-15 content results in higher specific surface area (524–237 m{sup 2}/g). The diffraction intensity of 101 plane of anatase polymorph was seen increasing with increase in TiO{sub 2} ratio. All the photocatalysts were having a mesoporous nature and follow the Langmuir IV isotherm, SBA-15 posses the highest pore volume (0.93 cm{sup 3} g{sup −1}) which consistently decreased with TiO{sub 2} content and was lowest (0.50 cm{sup 3} g{sup −1}) in case of 5 wt% of TiO{sub 2} followed by P25 (0.45 cm{sup 3} g{sup −1}) while pore diameter increased after TiO{sub 2} incorporation due to pore strain. The photocatalytic activity of the nanocomposites were analysed for the photodegradation of alizarin dye and pentachlorophenol under UV light irradiation. The reaction kinetics suggested the highest efficiency (98 % for alizarin and 94 % for PCP) of 5 wt% TiO{sub 2} compared to other photocatalysts, these nanocomposites were reused for several cycles, which is most important for heterogeneous photocatalytic degradation reaction.Graphical abstractThis study demonstrates the synthesis of silica embedded TiO{sub 2} nanocomposites by microwave assisted technique and their catalytic influence on degradation of organic dyes and pollutants. Higher loading of titania (SBA-15/TiO{sub 2}, 1:5) results better catalytic performance than commercial nano TiO{sub 2} (P25).

Exploiting the interactions between the ruthenium Hoveyda–Grubbs catalyst and Al-modified mesoporous silica: the case of SBA15 vs. KCC-1

KAUST Repository

Werghi, Baraa; Pump, Eva; Tretiakov, Mykyta; Abou-Hamad, Edy; Gurinov, Andrei; Doggali, Pradeep; Anjum, Dalaver H.; Cavallo, Luigi; Bendjeriou-Sedjerari, Anissa; Basset, Jean-Marie

2018-01-01

Immobilization of the 2 generation Hoveyda-Grubbs catalyst HG-II onto well-ordered 2D hexagonal (SBA15) and 3D fibrous (KCC-1) mesostructured silica, which contained tetra-coordinated Al, has been investigated through the Surface Organometallic Chemistry (SOMC) methodology. The main interest of this study lies in the peculiarity of the silica supports, which display a well-defined tetrahedral aluminum hydride site displaying a strong Lewis acid character, [(Si-O-Si)(Si-O-)Al-H]. The resulting supported Hoveyda-Grubbs catalysts have been fully characterized by advanced solid state characterization techniques (FT-IR, H and C solid state NMR, DNP-SENS, EF-TEM...). Together with DFT calculations, the immobilization of HG-II does not occur through the formation of a covalent bond between the complex and the Al-modified mesoporous silica as expected, but through an Al⋯Cl-[Ru]-coordination. It is not surprising that in functionalized olefin metathesis of diethyldiallyl malonate, DEDAM (liquid phase), leaching of the catalyst is observed which is not the case in non-functionalized olefin metathesis of propene (gas phase). Besides, the results obtained in propene metathesis with HG-II immobilized either on SBA15 (d = 6 nm) or KCC-1 (d = 4 or 8 nm) highlight the importance of the accessibility of the catalytic site. Therefore, we demonstrate that KCC-1 is a promising and suitable 3D mesoporous support to overcome the diffusion of reactants into the porous network of heterogeneous catalysts.

Exploiting the interactions between the ruthenium Hoveyda–Grubbs catalyst and Al-modified mesoporous silica: the case of SBA15 vs. KCC-1

KAUST Repository

Werghi, Baraa

2018-03-05

Immobilization of the 2 generation Hoveyda-Grubbs catalyst HG-II onto well-ordered 2D hexagonal (SBA15) and 3D fibrous (KCC-1) mesostructured silica, which contained tetra-coordinated Al, has been investigated through the Surface Organometallic Chemistry (SOMC) methodology. The main interest of this study lies in the peculiarity of the silica supports, which display a well-defined tetrahedral aluminum hydride site displaying a strong Lewis acid character, [(Si-O-Si)(Si-O-)Al-H]. The resulting supported Hoveyda-Grubbs catalysts have been fully characterized by advanced solid state characterization techniques (FT-IR, H and C solid state NMR, DNP-SENS, EF-TEM...). Together with DFT calculations, the immobilization of HG-II does not occur through the formation of a covalent bond between the complex and the Al-modified mesoporous silica as expected, but through an Al⋯Cl-[Ru]-coordination. It is not surprising that in functionalized olefin metathesis of diethyldiallyl malonate, DEDAM (liquid phase), leaching of the catalyst is observed which is not the case in non-functionalized olefin metathesis of propene (gas phase). Besides, the results obtained in propene metathesis with HG-II immobilized either on SBA15 (d = 6 nm) or KCC-1 (d = 4 or 8 nm) highlight the importance of the accessibility of the catalytic site. Therefore, we demonstrate that KCC-1 is a promising and suitable 3D mesoporous support to overcome the diffusion of reactants into the porous network of heterogeneous catalysts.

Metal-loaded SBA-16-like silica – Correlation between basicity and affinity towards hydrogen

International Nuclear Information System (INIS)

Ouargli-Saker, R.; Bouazizi, N.; Boukoussa, B.; Barrimo, Diana; Paola-Nunes-Beltrao, Ana; Azzouz, A.

2017-01-01

Highlights: • Metal dispersion in longitudinal channels confers adsorption properties to SBA-16. • Both Fe"0-NPs and Cu"0-NPs seem to be responsible of this effect. • Effect of the repetitive adsorption-desorption cycles on CO_2 and water sorption. • Hydrogen storage on the functionalized materials. - Abstract: Nanoparticles of Cu"o (CuNPs) and Fe"o (FeNPs) were dispersed in SBA-16-like silica, resulting metal-loaded materials (Cu-SBA-16 and Fe-SBA-16) with improved affinity towards hydrogen. Electron microscopy and X-ray diffraction showed that MNP dispersion occurs mainly inside SBA-16 channels. MNP incorporation was found to confer affinity to the silica surface, since higher CO_2 retention capacity (CRC) was registered Cu/SBA-16 and Fe/SBA-16. This was accompanied by a significant improvement of the affinity towards hydrogen, as supported by hydrogen adsorption tests. This was explained in terms of strong hydrogen interaction with MNP and lattice oxygen atoms. The results reported herein open new prospects for SBA-16 as potential adsorbents for hydrogen storage.

Metal-loaded SBA-16-like silica – Correlation between basicity and affinity towards hydrogen

Energy Technology Data Exchange (ETDEWEB)

Ouargli-Saker, R. [Department of Materials Engineering, University of Science and Technology, El M’naouer, BP 1505, Oran (Algeria); Nanoqam, Department of Chemistry, University of Quebec at Montreal, H3C3P8 (Canada); Bouazizi, N. [Nanoqam, Department of Chemistry, University of Quebec at Montreal, H3C3P8 (Canada); Unité de recherche, Electrochimie, Matériaux et Environnement, Faculté des Sciences de Gabès, Université de Gabès, Cité Erriadh, 6072 Gabès (Tunisia); Boukoussa, B. [Department of Materials Engineering, University of Science and Technology, El M’naouer, BP 1505, Oran (Algeria); Lqamb, Laboratório de Química Analítica Ambiental, Faculdade de Química, Pontifícia Universidade Católica do Rio Grande do Sul (Brazil); Barrimo, Diana [Nanoqam, Department of Chemistry, University of Quebec at Montreal, H3C3P8 (Canada); Paola-Nunes-Beltrao, Ana [Nanoqam, Department of Chemistry, University of Quebec at Montreal, H3C3P8 (Canada); Laboratory of Materials Chemistry L.C.M, University of Oran1 Ahmed Ben Bella, BP 1524, El-Mnaouer, 31000 Oran (Algeria); Azzouz, A., E-mail: azzouz.a@uqam.ca [Nanoqam, Department of Chemistry, University of Quebec at Montreal, H3C3P8 (Canada)

2017-07-31

Highlights: • Metal dispersion in longitudinal channels confers adsorption properties to SBA-16. • Both Fe{sup 0}-NPs and Cu{sup 0}-NPs seem to be responsible of this effect. • Effect of the repetitive adsorption-desorption cycles on CO{sub 2} and water sorption. • Hydrogen storage on the functionalized materials. - Abstract: Nanoparticles of Cu{sup o} (CuNPs) and Fe{sup o} (FeNPs) were dispersed in SBA-16-like silica, resulting metal-loaded materials (Cu-SBA-16 and Fe-SBA-16) with improved affinity towards hydrogen. Electron microscopy and X-ray diffraction showed that MNP dispersion occurs mainly inside SBA-16 channels. MNP incorporation was found to confer affinity to the silica surface, since higher CO{sub 2} retention capacity (CRC) was registered Cu/SBA-16 and Fe/SBA-16. This was accompanied by a significant improvement of the affinity towards hydrogen, as supported by hydrogen adsorption tests. This was explained in terms of strong hydrogen interaction with MNP and lattice oxygen atoms. The results reported herein open new prospects for SBA-16 as potential adsorbents for hydrogen storage.

Effects of carbon coating and pore corrugation on capillary condensation of nitrogen in SBA-15 mesoporous silica.

Science.gov (United States)

Morishige, Kunimitsu

2013-09-24

To examine the origin of an ink-bottle-like structure in SBA-15 formed by carbon coating and the effects of pore corrugation on capillary condensation and evaporation of a vapor in the cylindrical pores, we measured the adsorption isotherms of nitrogen at 77 K on 10 kinds of SBA-15 samples before and after a carbon coating process by the exposure to acetylene at 1073 K, as well as desorption scanning curves and subloops on the untreated samples. These SBA-15 samples were synthesized under the different conditions of initial SiO2/P123 ratio and hydrothermal treatment. SBA-15 with relatively large microporosity tends to form easily constrictions inside the main channels by the carbon coating. This strongly suggests that the rough pore walls of SBA-15 may induce the incomplete wetting of carbon layers on the pore walls to form the constrictions inside the cylindrical pores. A comparison of two subloops implies that the pores of SBA-15 synthesized with a SiO2/P123 ratio of 75 consist of an assembly of connecting domains of different diameters; that is, the pores are highly corrugated. For SBA-15 synthesized with a SiO2/P123 ratio of 60, the amplitude of the pore corrugation is significantly decreased by the prolonged hydrothermal treatment at 373 K. On the other hand, for SBA-15 synthesized with a SiO2/P123 ratio of 45, the amplitude of the corrugation is negligibly small, although the cylindrical pores are interconnected through narrow necks with each other. It is found that the smaller the amplitude of the pore corrugation, the smaller the width of the hysteresis loop.

Pore-expanded SBA-15 sulfonic acid silicas for biodiesel synthesis.

Science.gov (United States)

Dacquin, J P; Lee, A F; Pirez, C; Wilson, K

2012-01-07

Here we present the first application of pore-expanded SBA-15 in heterogeneous catalysis. Pore expansion over the range 6-14 nm confers a striking activity enhancement towards fatty acid methyl ester (FAME) synthesis from triglycerides (TAG), and free fatty acid (FFA), attributed to improved mass transport and acid site accessibility. This journal is © The Royal Society of Chemistry 2012

A dansyl group modified SBA-15 INHIBIT logic gate with [Hg2+ and Cl-] or [Hg2+ and Br-] as inputs

Science.gov (United States)

Wang, Xiaoyu; Yang, Honglei

2013-07-01

We developed a SBA-15-based INHIBIT logic gate (DA-SBA-15) which was prepared by covalent immobilization of a dansylamide derivative into the channels of the mesoporous silica material (SBA-15) via (3-aminopropyl)triethoxysilane (APTES) groups. A series of characteristic results proved that the fluorescent ligand was successfully grafted into the mesopores of SBA-15. The fluorescent characterization revealed excellent selectivity of DA-SBA-15 to the Hg2+ ion. Moreover, DA-SBA-15 can be considered as a selective fluorescent probe for Cl- and Br-. The fluorescent changes of DA-SBA-15 upon the addition of ions (Hg2+, Cl- and Br-) were utilized as an INH logic gate at the molecular level, using [Hg2+ and Cl-] or [Hg2+ and Br-] as chemical inputs and the fluorescence intensity signal as output.

Growth and physico-chemical properties of interconnected carbon nanotubes in FeSBA-15 mesoporous molecular sieves

Directory of Open Access Journals (Sweden)

Ulka Suryavanshi

2016-03-01

Full Text Available Carbon nanotubes (CNTs with well-defined hollow interiors, and different morphologies have been grown inside the nanochannels of iron substituted SBA-15 (Santa Barbara Amorphous with different iron contents and well-ordered large mesopores by chemical vapour deposition method. This novel method requires only 3 min for the formation of high quality multiwalled CNTs inside the SBA-15. The physico-chemical characteristics of the prepared CNT/Fe-SBA-15 nanocomposite have been analysed with powder X-ray diffraction (XRD, scanning electron microscopy (SEM, Raman spectroscopy and thermogravimetric analysis (TGA. XRD, Raman spectroscopy and TGA results confirm that the formed CNTs in SBA-15 nanochannels are highly pure and graphitic in nature, which can be altered by tuning the Fe content in the support matrix. SEM images show the interconnected network of SBA-15/CNT where CNT bridges the neighbouring SBA-15 nanoparticles. Interestingly, spring like CNTs and multi-terminal junctions such as Y and H junctions were also observed. The morphology of the CNTs inside the nanochannels of the SBA-15 support can also be controlled by the simple adjustment of the iron content in the SBA-15 framework. It has also been found that the content of Fe in the silica framework of SBA-15 plays a significant role in the formation of the CNTs and the amount of deposited CNTs in the nanochannels of SBA-15 increased with increasing the concentration of iron in framework. Among the materials studied, the FeSBA-15 with the nSi/nFe ratio of 2 showed the highest catalytic activity towards the formation of high quality CNTs.

Mesoporous templated silicas: stability, pore size engineering and catalytic activation

International Nuclear Information System (INIS)

Vansant, Etienne

2003-01-01

The Laboratory of Adsorption and Catalysis has focused its research activities on the synthesis and activation of new porous materials. In the past few years, we have succeeded in developing easy and reproducible pathways to synthesize a huge variety of mesoporous crystalline materials. Points of interest in the synthesis of Mesoporous Templated Silicas are (i) stabilization of the structure, to withstand hydrothermal, thermal and mechanical pressure, (ii) pore size engineering to systematically control the pore size, pore volume and the ratio micro/mesopores and (iii) ease and reproducibility of the synthesis procedure, applying green principles, such as template recuperation. By carefully adapting the synthesis conditions and composition of the synthesis gel, using surfactants (long chain quaternary ammonium ions) and co-templates (long chain amines, alcohols or alkanes), the pore size of the obtained materials can be controlled from 1.5 to 7.0 nm, retaining the very narrow pore size distribution. Alternatively, materials with combined micro- and mesoporosity can be synthesized, using neutral surfactants (triblock copolymers). Hereby, the optimization of the SBA-15 and SBA-16 synthesis is being done in order to create mesoporous materials with microporous walls. The second research line is the controlled activation of MTS materials, by grafting or incorporation of catalytic active centers. We have developed for this purpose the Molecular Designed Dispersion method, which uses metal diketonate complexes as precursors. It is shown that in all cases the dispersion of the metal oxides on the surface is much better compared to the conventional grafting techniques. We have studied and published activation with V, Ti, Mo, Fe, Al and Cr species on different MTS materials. The structure and location of the active metal ion is the subject of an extensive spectroscopic investigation, using FT-IR, FT-Raman, UV-Vis DR coupled with selective chemisorption experiments and

Controlling reaction pathways for alcohol dehydration and dehydrogenation over FeSBA-15 catalysts

NARCIS (Netherlands)

Guan, Y.; Li, Y.; Santen, van R.A.; Hensen, E.J.M.; Li, Can

2007-01-01

The iron location in FeSBA-15 strongly influences the selectivity to dehydrogenation and dehydration in ethanol conversion. At low iron loading, Fe is present as isolated species in the amorphous silica phase. At higher loading additional aggregated forms of iron oxide exist. Isolated species in the

Mesostructured Au/C materials obtained by replication of functionalized SBA-15 silica containing highly dispersed gold nanoparticles

KAUST Repository

Kerdi, Fatmé ; Caps, Valerie; Tuel, Alain

2011-01-01

was the same for both series and apparently did not depend on the nature of the silica template. Both Au/SiO2 templates and their corresponding Au/CMK-3 materials have been characterized by X-ray diffraction, nitrogen adsorption/desorption, chemical analysis

Synthesis and characterization of nano structures of Silica SBA-16 containing Gadolinium-159 as potential nanoparticulated system for cancer therapy; Sintese e caracterizacao de nanoestruturas de Silica SBA-16 contendo Gadolinio-159 como potencial sistema nanoparticulado para o tratamento do cancer

Energy Technology Data Exchange (ETDEWEB)

Oliveira, Andre Felipe de

2013-07-01

Cancer is a leading cause of death worldwide, and malignant neoplasms of the lung, stomach, liver, colon and breast in greater numbers. And recently observed in the literature a large number of reviews where new materials, especially nanoparticle, has been studied as drug carriers and radioisotopes applied to cancer treatment. How mesoporous materials based on silica, thanks to its huge surface area and biocompatibility, have been studied intensively providing broad applications in various areas, the use of nanostructured silica SBA-16 might be a carrier specific radioisotope accumulate in the cells malignant. Thus the aim of this study is to develop in vitro studies using SBA-16 can selectively concentrate in malignant cells therapeutic amounts of the radioisotope Gadolinium-159 escorting them to death. This work was performed orderly synthesis of mesoporous silica, SBA-16 and incorporating the complex Gd-DTPA-BMA, as well as chemical and structural characterization. The techniques used to analyze the occurrence of the incorporation of the gadolinium complex in the silica matrix were elemental analysis (CHN), atomic emission spectroscopy (ICP-AES), infrared spectroscopy (FTIR), nitrogen adsorption (BET), small-angle X-ray scattering (SAXS) and thermogravimetric analysis (TG). To analyze the morphology of pure silica used the scanning electron microscopy (SEM) and transmission electron microscopy (TEM). By photon correlation spectroscopy (PCS) it was possible to obtain a measure of mean particle size, the polydispersity index (PDI) of the silica SBA-16, and the zeta potential by laser Doppler anemometry (LDA). The results of incorporation analyzed by ICP-AES indicated that the material SBA-16 had a higher rate of incorporation of gadolinium (93%). The release kinetics in simulated body fluid, showed considerable stability and low release (1%). The mesoporous silica SBA-16 showed cell viability in direct contact with cell culture. Samples with gadolinium

Silica coated ionic liquid templated mesoporous silica nanoparticles ...

African Journals Online (AJOL)

A series of long chain pyridinium based ionic liquids 1-tetradecylpyridinium bromide, 1-hexadecylpyridinium bromide and 1-1-octadecylpyridinium bromide were used as templates to prepare silica coated mesoporous silica nanoparticles via condensation method under basic condition. The effects of alkyl chain length on ...

Selective synthesis of vitamin K3 over mesoporous NbSBA-15 catalysts synthesized by an efficient hydrothermal method.

Science.gov (United States)

Selvaraj, M; Park, D-W; Kim, I; Kawi, S; Ha, C S

2012-08-28

Well hexagonally ordered NbSBA-15 catalysts synthesized by an efficient hydrothermal method were used, for the first time, for the selective synthesis of vitamin K(3) by liquid-phase oxidation of 2-methyl-1-naphthol (2MN1-OH) under various reaction conditions. The recyclable NbSBA-15 catalysts were also reused to find their catalytic activities. To investigate the leaching of non-framework niobium species on the surface of silica networks, the results of original and recyclable NbSBA-15 catalysts were correlated and compared. To find an optimum condition for the selective synthesis of vitamin K(3), the washed NbSBA-15(2.2pH) was extensively used in this reaction with various reaction parameters such as temperature, time and ratios of reactant (2M1N-OH to H(2)O(2)), and the obtained results were also demonstrated. Additionally, the liquid-phase oxidation of 2M1N-OH was carried out with different solvents to find the best solvent with a good catalytic activity. Based on the all catalytic studies, the vitamin K(3) selectivity (97.3%) is higher in NbSBA-15(2.2pH) than that of other NbSBA-15 catalysts, and the NbSBA-15(2.2pH) is found to be a highly active and eco-friendly heterogeneous catalyst for the selective synthesis of vitamin K(3).

Production of Renewable Hydrogen from Glycerol Steam Reforming over Bimetallic Ni-(Cu,Co,Cr Catalysts Supported on SBA-15 Silica

Directory of Open Access Journals (Sweden)

Alicia Carrero

2017-02-01

Full Text Available Glycerol steam reforming (GSR is a promising alternative to obtain renewable hydrogen and help the economics of the biodiesel industry. Nickel-based catalysts are typically used in reforming reactions. However, the choice of the catalyst greatly influences the process, so the development of bimetallic catalysts is a research topic of relevant interest. In this work, the effect of adding Cu, Co, and Cr to the formulation of Ni/SBA-15 catalysts for hydrogen production by GSR has been studied, looking for an enhancement of its catalytic performance. Bimetallic Ni-M/SBA-15 (M: Co, Cu, Cr samples were prepared by incipient wetness co-impregnation to reach 15 wt % of Ni and 4 wt % of the second metal. Catalysts were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES, N2-physisorption, X-ray powder diffraction (XRD, hydrogen temperature programmed reduction (H2-TPR, transmission electron microscopy (TEM, scanning electron microscopy (SEM, and thermogravimetric analyses (TGA, and tested in GSR at 600 °C and atmospheric pressure. The addition of Cu, Co, and Cr to the Ni/SBA-15 catalyst helped to form smaller crystallites of the Ni phase, this effect being more pronounced in the case of the Ni-Cr/SBA-15 sample. This catalyst also showed a reduction profile shifted towards higher temperatures, indicating stronger metal-support interaction. As a consequence, the Ni-Cr/SBA-15 catalyst exhibited the best performance in GSR in terms of glycerol conversion and hydrogen production. Additionally, Ni-Cr/SBA-15 achieved a drastic reduction in coke formation compared to the Ni/SBA-15 material.

Stability and Catalytic Kinetics of Horseradish Peroxidase Confined in Nanoporous SBA-15

DEFF Research Database (Denmark)

Ikemoto, Hediki; Chi, Qijin; Ulstrup, Jens

2010-01-01

We have synthesized nanoporous silica, SBA-15 in the 1 m size range with the pore diameter of 7.6 nm. The redox enzyme horseradish peroxidase (HRP) was entrapped in the pores to form nanostructured hybrid materials. The catalytic activity of free and immobilized enzyme was first compared at room...... likely due to different hydrogen bonding of water and increased hydration strength of the protein inside the nanopores....

Functionalized SBA-15 materials for bilirubin adsorption

Science.gov (United States)

Tang, Tao; Zhao, Yanling; Xu, Yao; Wu, Dong; Xu, Jun; Deng, Feng

2011-05-01

To investigate the driving force for bilirubin adsorption on mesoporous materials, a comparative study was carried out between pure siliceous SBA-15 and three functionalized SBA-15 mesoporous materials: CH 3-SBA-15 (MS), NH 2-SBA-15 (AS), and CH 3/NH 2-SBA-15 (AMS) that were synthesized by one-pot method. The obtained materials exhibited large surface areas (553-810 m 2/g) and pore size (6.6-7.1 nm) demonstrated by XRD and N 2-ad/desorption analysis. The SEM images showed that the materials had similar fiberlike morphology. The functionalization extent was calculated according to 29Si MAS NMR spectra and it was close to the designed value (10%). The synthesized mesoporous materials were used as bilirubin adsorbents and showed higher bilirubin adsorption capacities than the commercial active carbon. The adsorption capacities of amine functionalized samples AMS and AS were larger than those of pure siliceous SBA-15 and MS, indicating that electrostatic interaction was the dominant driving force for bilirubin adsorption on mesoporous materials. Increasing the ionic strength of bilirubin solution by adding NaCl would decrease the bilirubin adsorption capacity of mesoporous material, which further demonstrated that the electrostatic interaction was the dominant driving force for bilirubin adsorption. In addition, the hydrophobic interaction provided by methyl groups could promote the bilirubin adsorption.

Effect of amine functionalization of spherical MCM-41 and SBA-15 on controlled drug release

International Nuclear Information System (INIS)

Szegedi, A.; Popova, M.; Goshev, I.; Mihaly, J.

2011-01-01

MCM-41 and SBA-15 silica materials with spherical morphology and different particle sizes were synthesized and modified by post-synthesis method with 3-aminopropyltriethoxysilane (APTES). A comparative study of the adsorption and release of a model drug, ibuprofen, were carried out. The modified and drug loaded mesoporous materials were characterized by XRD, TEM, N 2 physisorption, thermal analysis, elemental analysis and FT-IR spectroscopy. Surface modification with amino groups resulted in high degree of ibuprofen loading and slow rate of release for MCM-41, whereas it was the opposite for SBA-15. The adsorbed drug content and the delivery rate can be predetermined by the choice of mesoporous material with the appropriate structural characteristics and surface functionality. -- Graphical Abstract: Ibuprofen delivery from the parent and amino-modified spherical MCM-41 materials with 100 nm (small) and 500 nm (large) particle sizes. Display Omitted Highlights: → Spherical type MCM-41 and SBA-15 with different particle sizes were modified by APTES. → Adsorption and release rate of ibuprofen were compared. → High degree of ibuprofen loading, slow release rate for MCM-41, the opposite for SBA-15. → MCM-41 with 100 nm particles was more stable and showed slower release rate

Carboxylic acid-functionalized SBA-15 nanorods for gemcitabine delivery

International Nuclear Information System (INIS)

Bahrami, Zohreh; Badiei, Alireza; Ziarani, Ghodsi Mohammadi

2015-01-01

The present study deals with the functionalization of mesoporous silica nanoparticles as drug delivery systems. Mono, di, and tri amino-functionalized SBA-15 nanorods were synthesized by post-grafting method using (3-aminopropyl) triethoxysilane, N-(2-aminoethyl-)3- aminopropyltrimethoxysilane, and 3-[2-(2-aminoethylamino) ethylamino] propyl trimethoxysilane, respectively. The carboxylic acid derivatives of the amino-functionalized samples were obtained using succinic anhydride. Tminopropyltrimethoxysilanehe obtained modified materials were investigated as matrixes for the anticancer drug (gemcitabine) delivery. The prepared samples were characterized by SAXS, N 2 adsorption/desorption, SEM, transmission electron microscopy, thermogravimetric analysis, and FTIR and UV spectroscopies. The adsorption and release properties of all samples were studied. It was revealed that the adsorption capacity and release behavior of gemcitabine were highly dependent on the type of the introduced functional groups. The carboxylic acid-modified samples have higher loading content, due to the strong interaction with gemcitabine. The maximum content of deposited drug in the modified SBA-15 nanorods is close to 40 wt%. It was found that the surface functionalization leads toward significant decrease of the drug release rate. The carboxylic acid-functionalized samples have slower release rate in contrast with the amino-functionalized samples

Preparation of Mesoporous SBA-16 Silica-Supported Biscinchona Alkaloid Ligand for the Asymmetric Dihydroxylation of Olefins

Directory of Open Access Journals (Sweden)

Shaheen M. Sarkar

2014-01-01

Full Text Available Optically active cinchona alkaloid was anchored onto mesoporous SBA-16 silica and the as-prepared complex was used as a heterogeneous chiral ligand of osmium tetraoxide for the asymmetric dihydroxylation of olefins. The prepared catalytic system provided 90–93% yield of vicinal diol with 92–99% enantioselectivity. The ordered mesoporous SBA-16 silica was found to be a valuable support for the cinchona alkaloid liganded osmium catalyst system which is frequently used in chemical industries and research laboratories for olefin functionalization.

Synthesis and characterization of nano structures of Silica SBA-16 containing Gadolinium-159 as potential nanoparticulated system for cancer therapy

International Nuclear Information System (INIS)

Oliveira, Andre Felipe de

2013-01-01

Cancer is a leading cause of death worldwide, and malignant neoplasms of the lung, stomach, liver, colon and breast in greater numbers. And recently observed in the literature a large number of reviews where new materials, especially nanoparticle, has been studied as drug carriers and radioisotopes applied to cancer treatment. How mesoporous materials based on silica, thanks to its huge surface area and biocompatibility, have been studied intensively providing broad applications in various areas, the use of nanostructured silica SBA-16 might be a carrier specific radioisotope accumulate in the cells malignant. Thus the aim of this study is to develop in vitro studies using SBA-16 can selectively concentrate in malignant cells therapeutic amounts of the radioisotope Gadolinium-159 escorting them to death. This work was performed orderly synthesis of mesoporous silica, SBA-16 and incorporating the complex Gd-DTPA-BMA, as well as chemical and structural characterization. The techniques used to analyze the occurrence of the incorporation of the gadolinium complex in the silica matrix were elemental analysis (CHN), atomic emission spectroscopy (ICP-AES), infrared spectroscopy (FTIR), nitrogen adsorption (BET), small-angle X-ray scattering (SAXS) and thermogravimetric analysis (TG). To analyze the morphology of pure silica used the scanning electron microscopy (SEM) and transmission electron microscopy (TEM). By photon correlation spectroscopy (PCS) it was possible to obtain a measure of mean particle size, the polydispersity index (PDI) of the silica SBA-16, and the zeta potential by laser Doppler anemometry (LDA). The results of incorporation analyzed by ICP-AES indicated that the material SBA-16 had a higher rate of incorporation of gadolinium (93%). The release kinetics in simulated body fluid, showed considerable stability and low release (1%). The mesoporous silica SBA-16 showed cell viability in direct contact with cell culture. Samples with gadolinium

Silylated Co/SBA-15 catalysts for Fischer-Tropsch synthesis

International Nuclear Information System (INIS)

Jia Lihong; Jia Litao; Li Debao; Hou Bo; Wang Jungang; Sun Yuhan

2011-01-01

A series of silylated Co/SBA-15 catalysts were prepared via the reaction of surface Si-OH of SBA-15 with hexamethyldisilazane (HMDS) under anhydrous, vapor-phase conditions, and then characterized by FT-IR, N 2 physisorption, TG, XRD, and TPR-MS. The results showed that organic modification led to a silylated SBA-15 surface composed of stable hydrophobic Si-(CH 3 ) 3 species even after calcinations and H 2 reduction at 673 K. Furthermore, the hydrophobic surface strongly influenced both metal dispersion and reducibility. Compared with non-silylated Co/SBA, Co/S-SBA (impregnation after silylation) showed a high activity, due to the better cobalt reducibility on the hydrophobic support. However, S-Co/SBA (silylation after impregnation) had the lowest FT activity among all the catalysts, due to the lower cobalt reducibility along with the steric hindrance of grafted -Si(CH 3 ) 3 for the re-adsorption of α-olefins. -- Graphical abstract: The silylation of an SBA-15 before cobalt impregnation enhanced the reducibility of cobalt oxides on an SBA-15-supported cobalt catalyst and consequently increased the catalytic activity for Fischer-Tropsch synthesis. Display Omitted

Tailoring silver nanoparticle construction using dendrimer templated silica networks

International Nuclear Information System (INIS)

Liu Xiaojun; Kakkar, Ashok

2008-01-01

We have examined the role of the internal environment of dendrimer templated silica networks in tailoring the construction of silver nanoparticle assemblies. Silica networks from which 3,5-dihydroxybenzyl alcohol based dendrimer templates have been completely removed, slowly wet with an aqueous solution of silver acetate. The latter then reacts with internal silica silanol groups, leading to chemisorption of silver ions, followed by the growth of silver oxide nanoparticles. Silica network constructed using generation 4 dendrimer contains residual dendrimer template, and mixes with aqueous silver acetate solution easily. Upon chemisorption, silver ions get photolytically reduced to silver metal under a stabilizing dendrimer environment, leading to the formation of silver metal nanoparticles

Preparation of SBA-15-PAMAM as a Nano Adsorbent for Removal of Acid Red 266 from Aqueous Media: Batch Adsorption and Equilibrium Studies

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Maryam Mirzaie

2017-12-01

Full Text Available The purpose of the present study was to increase the adsorption capacity of SBA-15 for acidic dyes. Ordered mesoporous silica SBA-15 was successfully synthesized and functionalized by polyamidoamine (PAMAM dendrimer to develop an efficient anionic dye adsorbent. The prepared materials were characterized by field emission scanning electron microscope (FE-SEM, Fourier transforms infrared spectroscope (FT-IR and N2 adsorption–desorption analysis. The study was concocted in the Science and Research Branch of Islamic Azad University of Tehran, Iran in 2016. The produced adsorbent (SBA-15-Den was applied for the removal of Acid Red 266 (AR266 from aqueous media. The effects of various operational parameters including solution pH, adsorbent dosage, contact time, and temperature on removal of AR266 using SBA-15-Den were investigated in batch adsorption mode. Within the optimum conditions, SBA-15-Den exhibited an excellent adsorptive capability of 1111.11 mg/g. Equilibrium data were best described by Langmuir model (R2 > 0.98 completely.

Phosphoryl functionalized mesoporous silica for uranium adsorption

International Nuclear Information System (INIS)

Xue, Guo; Yurun, Feng; Li, Ma; Dezhi, Gao; Jie, Jing; Jincheng, Yu; Haibin, Sun; Hongyu, Gong; Yujun, Zhang

2017-01-01

Highlights: • Phosphoryl functionalized mesoporous silica (TBP-SBA-15) is synthesized. • The amino and phosphoryl groups are successfully grafted on SBA-15. • TBP-SBA-15 has high and rapid uranium adsorption capacity in broad pH range. • The U(VI) adsorption of TBP-SBA-15 is spontaneous and belongs to chemical adsorption. - Abstract: Phosphoryl functionalized mesoporous silica (TBP-SBA-15) was synthesized by modified mesoporous silica with γ-amino propyl triethoxy silane and tributyl phosphate. The obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray diffraction (SAXRD), thermo-gravimetric/differential thermalanalyzer (TG/DTA), N_2 adsorption–desorption (BET) and Fourier transform infrared spectroscopy (FT-IR) techniques. Results showed that TBP-SBA-15 had large surface areas with ordered channel structure. Moreover, the effects of adsorption time, sorbent dose, solution pH, initial uranium concentration and temperature on the uranium adsorption behaviors were investigated. TBP-SBA-15 showed a high uranium adsorption capacity in a broad range of pH values. The U(VI) adsorption rate of TBP-SBA-15 was fast and nearly achieved completion in 10 min with the sorbent dose of 1 g/L. The U(VI) adsorption of TBP-SBA-15 followed the pseudo-second-order kinetic model and Freundlich isotherm model, indicating that the process was belonged to chemical adsorption. Furthermore, the thermodynamic parameters (ΔG"0, ΔH"0 and ΔS"0) confirmed that the adsorption process was endothermic and spontaneous.

Phosphoryl functionalized mesoporous silica for uranium adsorption

Energy Technology Data Exchange (ETDEWEB)

Xue, Guo; Yurun, Feng; Li, Ma; Dezhi, Gao; Jie, Jing; Jincheng, Yu; Haibin, Sun [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Hongyu, Gong, E-mail: gong_hongyu@163.com [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Yujun, Zhang, E-mail: yujunzhangcn@163.com [Key Laboratory for Liquid-Solid Structural Evolution & Processing of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, Shandong University, Jinan 250061 (China)

2017-04-30

Highlights: • Phosphoryl functionalized mesoporous silica (TBP-SBA-15) is synthesized. • The amino and phosphoryl groups are successfully grafted on SBA-15. • TBP-SBA-15 has high and rapid uranium adsorption capacity in broad pH range. • The U(VI) adsorption of TBP-SBA-15 is spontaneous and belongs to chemical adsorption. - Abstract: Phosphoryl functionalized mesoporous silica (TBP-SBA-15) was synthesized by modified mesoporous silica with γ-amino propyl triethoxy silane and tributyl phosphate. The obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray diffraction (SAXRD), thermo-gravimetric/differential thermalanalyzer (TG/DTA), N{sub 2} adsorption–desorption (BET) and Fourier transform infrared spectroscopy (FT-IR) techniques. Results showed that TBP-SBA-15 had large surface areas with ordered channel structure. Moreover, the effects of adsorption time, sorbent dose, solution pH, initial uranium concentration and temperature on the uranium adsorption behaviors were investigated. TBP-SBA-15 showed a high uranium adsorption capacity in a broad range of pH values. The U(VI) adsorption rate of TBP-SBA-15 was fast and nearly achieved completion in 10 min with the sorbent dose of 1 g/L. The U(VI) adsorption of TBP-SBA-15 followed the pseudo-second-order kinetic model and Freundlich isotherm model, indicating that the process was belonged to chemical adsorption. Furthermore, the thermodynamic parameters (ΔG{sup 0}, ΔH{sup 0} and ΔS{sup 0}) confirmed that the adsorption process was endothermic and spontaneous.

Efficient solid-phase microextraction of triazole pesticides from natural water samples using a Nafion-loaded trimethylsilane-modified mesoporous silica coating of type SBA-15

International Nuclear Information System (INIS)

Abolghasemi, Mir Mahdi; Hassani, Sona; Bamorowat, Mehdi

2016-01-01

A mesoporous silica surface of type SBA-15 was made more hydrophobic by modification with ethoxytrimethylsilane to obtain a hybrid organic–inorganic mesoporous nanocomposite, which then was impregnated with Nafion. The resulting nanocomposite was used as a fiber coating for solid-phase microextraction (SPME). The trimethylsilyl-modified Nafion/SBA-15 nanocomposite with high surface area was characterized by SEM and FTIR. It was immobilized on a stainless steel wire in order to fabricate a fiber for SPME. This fiber was evaluated for its suitability for extracting triazolic agrochemicals from water samples before their quantification through a combination of gas chromatography and mass spectrometry. Experimental conditions for fiber coating, extraction time, stirring rate, ionic strength, pH value, desorption temperature and desorption time were optimized. Under optimum conditions, the repeatability for one fiber (for n = 3) ranges from 4.3 to 5.6 % (relative standard deviation). The detection limits are between 50 and 90 pg⋅mL −1 . The method is simple, fast, low-cost (in terms of equipment), and the fiber used for SPME has high thermal stability and good recovery. (author)

In-situ infrared study of CO{sub 2} adsorption on SBA-15 grafted with {gamma}-(aminopropyl)triethoxysilane

Energy Technology Data Exchange (ETDEWEB)

Alex C.C. Chang; Steven S.C. Chuang; McMahan Gray; Yee Soong [University of Akron, Akron, OH (United States). Chemical Engineering Department

2003-04-01

CO{sub 2} adsorption/desorption on SBA-15 grafted with {gamma}-(aminopropyl)triethoxysilane (APTS) has been studied by infrared spectroscopy coupled with temperature-programmed desorption. SBA-15, a mesoporous silica material with a uniform pore size of 21 nm and a surface area of 200-230 m{sup 2}/g, provides an OH functional group for grafting of {gamma}-(aminopropyl)triethoxysilane. The amine-grafted SBA-15 adsorbed CO{sub 2} as carbonates and bicarbonates with a total capacity of 200-400 {mu}mol/g. The heat of CO{sub 2} desorption was determined to be 3.2-4.5 kJ/mol in the presence of H{sub 2}O and 6.6-11.0 kJ/mol in the absence of H{sub 2}O during temperature-programmed desorption. Repeated CO{sub 2} adsorption/desorption CO{sub 2} cycles shifted the desorption peak temperature downward and decreased the heat of CO{sub 2} adsorption. 22 refs., 9 figs., 3 tabs.

Desidratação de etanol sobre material nanoestruturado do tipo LaSBA-15 Ethanol dehydration over LaSBA-15 nanostrutured material

Directory of Open Access Journals (Sweden)

Geraldo E. Luz Jr

2010-01-01

Full Text Available La-incorporated SBA-15 mesopourous molecular sieves (LaSBA-15 were directly synthesized with aim to convert ethanol to ethylene. The samples were characterized by XRD, XRF, nitrogen sorption and acidity, by thermodesorption of n-buthylamine. The results have indicated that all the samples have showed high ordered mesostructure with a large average pore size, and that the lanthanum incorporation has caused an increase in the acidity of the SBA-15. The LaSBA-15 samples have improved, with low deactivation rate, the conversion of the ethanol to water, ether, acetaldehyde and ethylene. In addition, they have increased the ethylene selectivity.

A novel, efficient and facile method for the template removal from mesoporous materials

KAUST Repository

Chen, Lu

2014-11-12

© 2014, Jilin University, The Editorial Department of Chemical Research in Chinese Universities and Springer-Verlag GmbH. A new catalytic-oxidation method was adopted to remove the templates from SBA-15 and MCM-41 mesoporous materials via Fenton-like techniques under microwave irradiation. The mesoporous silica materials were treated with different Fenton agents based on the template’s property and textural property. The samples were characterized by powder X-ray diffraction(XRD) measurement, N2 adsorption-desorption isotherms, infrared spectroscopy, 29Si MAS NMR and thermo gravimetric analysis(TGA). The results reveal that this is an efficient and facile approach to the thorough template-removal from mesoporous silica materials, as well as to offering products with more stable structures, higher BET surface areas, larger pore volumes and larger quantity of silanol groups.

Controlled and localized delivery of c-myc AS-ODN to cells by 3-aminopropyl-trimethoxylsilane modified SBA-15 mesoporous silica

Science.gov (United States)

Zhang, Juan; Chen, Minmin; Zhao, Xiqiu; Zhang, Min; Mao, Jinxiang; Cao, Xichuan; Zhang, Zhuoqi

2018-01-01

SBA-15 mesoporous silicate was synthesized and functionalized with 3-aminopropyl organic groups through a post-synthesis method. The materials were characterized consecutively by powder X-ray diffraction (XRD), N2 adsorption/desorption analysis and solid-state magic-angle spinning 29Si nuclear magnetic resonance (MAS NMR). Human c-myc anti-sense oligodeoxyneucleotide (AS-ODN) was selected as a model molecule to be loaded onto the surface of bare and functionalized SBA-15 via different loading conditions. It has been found that the amount of AS-ODN incorporated into the porous matrix is strongly dependent on the surface properties, pH of the loading solvent and AS-ODN concentration. The release behaviour of AS-ODN from modified SBA-15 materials was also investigated and depended on conditions chosen. Cellular uptake of the eluted AS-ODN into Hela cells was observed by fluorescent microscopy. The materials showed excellent cytocompatibility. The AS-ODN keeps full transfection and expression activities indicating its structural integrity. The functionalized SBA-15 is an excellent prospect as a biomedical material candidate for the future.

Hydrodeoxygenation of Guaiacol Over Pt/Al-SBA-15 Catalysts.

Science.gov (United States)

Yu, Mi Jin; Park, Sung Hoon; Jeon, Jong-Ki; Ryu, Changkook; Sohn, Jung Min; Kim, Sang Chai; Park, Young-Kwon

2015-01-01

Upgrading of bio-oil through catalytic hydrodeoxygenation (HDO) reaction was investigated for guaiacol as a model compound. A batch reactor was used for the reaction condition of 40 bar and 250 degrees C. The target product was cyclohexane. Pt/Al-SBA-15 with the Si/Al ratios of 20, 40, and 80 and Pt/HZSM-5 were used as the catalyst. The SBA-15 catalysts were characterized by N2 adsorption-desorption, X-ray diffraction analysis, and temperature programmed desorption of ammonia. The order of cyclohexane yield was Pt/Al-SBA-15 (Si/Al = 20) > Pt/Al-SBA-15(40) > Pt/Al-SBA-15 (80), indicating that the quantity of acid sites plays an important role in the HDO reaction. On the other hand, Pt/HZSM-5 led to a very low cyclohexane yield, in spite of its abundant strong acid sites, due to its small pore size.

Synthesis of Hollow Silica by Stober Method with Double Polymers as Templates

International Nuclear Information System (INIS)

Nguyen, Anhthu; Park, Chang Woo; Kim, Sang Hern

2014-01-01

The hollow SiO 2 spheres with uniform size were synthesized by a modified stoeber method under the control of polyelectrolytes (PSS and PAA) as templates. This synthetic route includes the formation of spherical colloid micelle in ethanol solution, hydrolysis of TEOS under control of ammonia, and the removal of polyelectrolyte by washing or calcination. Hollow silica spheres with controllable core diameters between 100 and 270 nm and wall thickness between 15 and 50 nm have been synthesized. The influence of template solution concentration and solvent and dispersant on the formation of silica hollow spheres is studied and reported in detail

In situ synthesis of copper nanoparticles on SBA-16 silica spheres

Directory of Open Access Journals (Sweden)

Asma Tufail Shah

2016-07-01

Full Text Available A chemical method for in situ synthesis of copper nanoparticles on SBA-16 silica spheres under ambient conditions has been reported. The silica support has been introduced into copper precursor solution before chemical reduction. Metal ions diffuse into mesopores (pore diameter 5–7 nm of silica where in situ reduction by hydrazine leads to formation of nanoparticles. These mesopores act as nanoreactor and their walls prevent metal particle’s agglomeration by providing a physical barrier. The obtained copper nanoparticles have been investigated by electron microscopy, X-ray diffraction, UV–Visible spectroscopy, Fourier transform Infra-red spectroscopy and thermogravimetric analyzer. SEM, TEM and UV–Visible spectroscopic images revealed that nanosized particles have been successfully synthesized by this method. Thermogravimetric investigations revealed that copper nanoparticles impregnated on silica were thermally more stable compared to unsupported nanoparticles. Silica not only helps in maintaining the particle size but also makes nanoparticles stable at high temperatures due to its thick pore walls. Macro sized silica support also makes separation/handling of nanoparticles easy and simple.

Propene epoxidation over Au/Ti-SBA-15 catalysts

NARCIS (Netherlands)

Sacaliuc, E.; Beale, A.M.; Weckhuysen, B.M.; Nijhuis, T.A.

2007-01-01

Highly dispersed gold nanoparticles were synthesized within the channels of a mesoporous Ti-SBA-15 support, followed by thorough catalyst characterization and testing in the selective epoxidation of propene to propene oxide. For this purpose, two series of Ti-SBA-15 materials differing in their Ti

Preparation and thermal properties of mesoporous silica/phenolic resin nanocomposites via in situ polymerization

Directory of Open Access Journals (Sweden)

J. Lv

2012-10-01

Full Text Available In order to enhance the adhesion between inorganic particles and polymer matrix, in this paper, the mesoporous silica SBA-15 material was synthesized by the sol-gel method. The surface of SBA-15 was modified using γ-glycidyloxypropyltrimethoxysilane (GOTMS as a coupling agent, and then mesoporous silica/phenolic resin (SBA-15/PF nanocomposites were prepared via in situ polymerization. The structural parameters and physical properties of SBA-15, SBA-15-GOTMS (SBA-15 surface treated using GOTMS as coupling agents and E-SBA-15/PF (SBA-15/PF nanocomposites extracted using ethanol as solvent were characterized by X-ray diffraction (XRD, N2 adsorption-desorption, Fourier transform infrared spectroscopy (FTIR, scanning electron microscopy (SEM, transmission electron microscopy (TEM and thermogravimetric analysis (TGA. The thermal properties of the nanocomposites were studied by differential scanning calorimetry (DSC and thermogravimetric analysis (TGA. The results demonstrated that the GOTMS were successfully grafted onto the surface of SBA-15, and chemical bonds between PF and SBA-15-GOTMS were formed after in situ polymerization. In addition, it is found that the in situ polymerization method has great effects on the textural parameters of SBA-15. The results also showed that the glass transition temperatures and thermal stability of the PF nanocomposites were obviously enhanced as compared with the pure PF at silica contents between 1–3 wt%, due to the uniform dispersion of the modified SBA-15 in the matrix.

Controlled release of phenytoin for epilepsy treatment from titania and silica based materials

International Nuclear Information System (INIS)

Lopez, Tessy; Ortiz, Emma; Meza, Doraliz; Basaldella, Elena; Bokhimi, Xim; Magana, Carlos; Sepulveda, Antonio; Rodriguez, Francisco; Ruiz, Javier

2011-01-01

Research highlights: → Template technique was used to obtain well ordered nanostructured materials: SBA-15 and titania tubes. → Phenytoin (PH), a drug used in epilepsy treatment, was loaded in these materials to used como PH release. → Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. → The load-release PH are faster in nanostructured TiO2 tubes than in mesoporous silica matrix. → There is an inverse effect of the surface area of the structured materials on the amount of released PH. - Abstract: Template technique was used to obtain well ordered nanostructured materials: mesoporous silica and nanostructured titania tubes. This technique permits the synthesis of solids with controlled mesoporosity, where a large variety of molecules that have therapeutic activity can be hosted and further released to specific sites. In this work phenytoin (PH), a drug used in epilepsy treatment, was loaded in ordered mesoporous silica (SBA 15) and nanostructured titania tubes (TiO 2 ). The pure materials and those containing PH were characterized by X-ray diffraction, FTIR spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N 2 adsorption-desorption at 77 K. In order to determine the loading capacity of the antiepileptic drug on these silica- and titania-based materials, the loading and release of PH was investigated using UV-vis spectroscopy. Tubular structures were found for the titania samples, for which the X-ray diffractograms showed to be formed by anatase and rutile phases. On the other hand, an amorphous phase was found in the silica sample. A highly ordered hexagonal structure of 1D cylindrical channels was also observed for this material. Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. The adsorption and desorption of PH are faster in nanostructured TiO 2 tubes than in mesoporous silica matrix.

Selective Preparation of trans-Carveol over Ceria Supported Mesoporous Materials MCM-41 and SBA-15

Directory of Open Access Journals (Sweden)

Nariman F. Salakhutdinov

2013-05-01

Full Text Available Ce-modified mesoporous silica materials MCM-41 and SBA-15, namely 32 wt % Ce–Si–MCM-41, 16 wt % Ce–H–MCM-41 and 20 wt % Ce–Si–SBA-15, were prepared, characterized and studied in the selective preparation of trans-carveol by α-pinene oxide isomerization. The characterizations of these catalysts were performed using scanning electron microscopy, X-ray photoelectron spectroscopy, nitrogen adsorption and FTIR pyridine adsorption. Selective preparation of trans-carveol was carried out in the liquid phase in a batch reactor. The activity and the selectivity of catalyst were observed to be influenced by their acidity, basicity and morphology of the mesoporous materials. The formation of trans-carveol is moreover strongly influenced by the basicity of the used solvent and in order to achieve high yields of this desired alcohol it is necessary to use polar basic solvent.

A flexible, bolaamphiphilic template for mesoporous silicas.

Science.gov (United States)

Yuen, Alexander K L; Heinroth, Falk; Ward, Antony J; Masters, Anthony F; Maschmeyer, Thomas

2013-08-28

A novel symmetrical bolaamphiphile, containing two N-methylimidazolium head-groups bridged by a 32-methylene linker, was synthesized and characterized. A variety of mesoporous silicas was prepared using the bolaamphiphile as a "soft template". The effects of absolute surfactant concentration and synthesis conditions upon the morphologies of these silicas were investigated. For a given surfactant concentration, particle morphology; pore size; and pore ordering were modified through control of the template to silica-precursor ratio and synthesis conditions. Observed morphologies included: lenticular core-shell nanoparticles and decorticated globules, truncated hexagonal plates, and sheets. In all cases the mesopores are aligned along the shortest axis of the nanomaterial. Decorticated materials displayed surface areas of up to 1200 m(2) g(-1) and pore diameters (D(BJH)) of 24-28 Å. Small-angle X-ray diffraction and transmission electron microscopy measurements revealed that the majority of the materials has elliptical pores arranged in rectangular lattices (c2mm). Adoption of this symmetry group is a result of the template aggregate deformation from a regular hexagonal phase of cylindrical rods to a ribbon phase under the synthetic conditions.

Preparation and characterization of catalyst 20% Co/SBA-15

International Nuclear Information System (INIS)

Lima, L.A.; Nogueira, A.C.; Rodrigues, J.J.; Rodrigues, M.G.F.

2012-01-01

The utilization of molecular sieves as supports for cobalt catalysts are promising. SBA-15 is a class of mesoporous silicate with a high thermal stability and high degree of structural order, which confers an important feature for the catalytic process. It was prepared SBA-15 molecular sieve with molar composition: 1.0 TEOS: 0017P123: 5.7 HCl: 193 H2O. The deposition of cobalt on the substrate SBA-15 was performed by wet impregnation, using a solution of 0.1M cobalt nitrate. The materials were characterized by the techniques of X-Ray Diffraction (XRD), chemical analysis by X-Ray Spectrometry by Energy Dispersive (EDX), and nitrogen adsorption (BET). By XRD and BET verified the formation of SBA-15, and after the impregnation there was no change in the structure, with EDX showed that the impregnation method is efficient, the sample showed cobalt content close to the nominal value. (author)

Intermediate-range order in mesoporous silicas investigated by a high-energy X-ray diffraction technique

International Nuclear Information System (INIS)

Wakihara, Toru; Fan, Wei; Ogura, Masaru; Okubo, Tatsuya; Kohara, Shinji; Sankar, Gopinathan

2008-01-01

We perform a high-energy X-ray diffraction study comparing bulk amorphous silica with MCM-41 and SBA-15 that are representative mesoporous silicas prepared in basic and acidic conditions, respectively. It is revealed that mesoporous silicas, especially SBA-15, have less ordered structures and contain larger fractions of three- and four-membered rings than does bulk amorphous silica. (author)

The synthesis of novel hybrid thiol-functionalized nano-structured SBA-15

International Nuclear Information System (INIS)

Hoang, Van Duc; Dang, Tuyet Phuong; Dinh, Quang Khieu; Vu, Anh Tuan; Nguyen, Huu Phu

2010-01-01

Mesoporous thiol-functionalized SBA-15 has been directly synthesized by co-condensation of tetraethyl orthosilicate (TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) with triblock copolymer P123 as-structure-directing agent under hydrothermal conditions. Surfactant removal was performed by Soxhlet ethanol extraction. These materials have been characterized by powder x-ray diffraction (XRD), nitrogen adsorption/desorption (BET model), transmission electron microscopy (TEM), thermal analysis, infrared spectroscopy (IR) and energy-dispersive x-ray spectroscopy (EDX). The main parameters, such as the initial molar ratio of MPTMS to TEOS, the time of adding MPTMS to synthesized gel and the Soxhlet ethanol extraction on the thiol functionalized SBA-15 with high thiol content and highly ordered hexagonal mesostructure, were investigated and evaluated. The adsorption capacity of the thiol-functionalized and non-functionalized SBA-15 materials for Pb 2+ ion from aqueous solution was tested. It was found that the Pb 2+ adsorption capacity of the thiol functionalized SBA-15 is three times higher than that of non-functionalized SBA-15

Controlled drug release from bifunctionalized mesoporous silica

Science.gov (United States)

Xu, Wujun; Gao, Qiang; Xu, Yao; Wu, Dong; Sun, Yuhan; Shen, Wanling; Deng, Feng

2008-10-01

Serial of trimethylsilyl-carboxyl bifunctionalized SBA-15 (TMS/COOH/SBA-15) have been studied as carriers for controlled release of drug famotidine (Famo). To load Famo with large capacity, SBA-15 with high content of carboxyl groups was successfully synthesized by one-pot synthesis under the assistance of KCl. The mesostructure of carboxyl functionalized SBA-15 (COOH/SBA-15) could still be kept even though the content of carboxyl groups was up to 57.2%. Increasing carboxyl content could effectively enhance the loading capacity of Famo. Compared with pure SBA-15, into which Famo could be hardly adsorbed, the largest drug loading capacity of COOH/SBA-15 could achieve 396.9 mg/g. The release of Famo from mesoporous silica was studied in simulated intestine fluid (SIF, pH=7.4). For COOH/SBA-15, the release rate of Famo decreased with narrowing pore size. After grafting TMS groups on the surface of COOH/SBA-15 with hexamethyldisilazane, the release of Famo was greatly delayed with the increasing content of TMS groups.

Iron-functionalized nanoporous silica type SBA-15: Synthesis, characterization and application in alkene epoxidation in presence of hydrogen peroxide

Directory of Open Access Journals (Sweden)

Mahdieh Ghazizadeh

2017-05-01

Full Text Available Fe(IIIsalophen complex on a SBA-15 support functionalized with (3-aminopropyltriethoxysilane as a linker. It has been synthesized and characterized by XRD, adsorption–desorption of nitrogen, SEM, FT-IR and UV–Vis. The formation of metal-salophen complex with the amino groups as connectors to the SBA-15 surface was confirmed. This material was successfully used as a heterogeneous catalyst for the epoxidation of alkenes and the effects of reaction time, different solvents and amount of catalyst on catalytic activity were investigated. This catalyst gave suitable and comparable yield and percentage conversion values. It is also stable and can be recycled and reused in the epoxidation of alkenes.

A mesoporous silica composite scaffold: Cell behaviors, biomineralization and mechanical properties

Science.gov (United States)

Xu, Yong; Gao, Dan; Feng, Pei; Gao, Chengde; Peng, Shuping; Ma, HaoTian; Yang, Sheng; Shuai, Cijun

2017-11-01

Mesoporous structure is beneficial to cellular response due to the large specific surface area and high pore volume. In this study, mesoporous silica (SBA15) was incorporated into poly-L-lactic acid (PLLA) to construct composite scaffold by selective laser sintering. The results showed that SBA15 facilitated cells proliferation, which was mainly attributed to its unique intrinsic mesoporous structure and the released bioactive silicon. Moreover, the hydrolyzate of soluble mesoporous silica can adsorb ions to form nucleation sites that promote biomineralization, leading to improve biological activity of the composite scaffold. In addition, the compressive strength, compressive modulus and Vickers hardness of the scaffold were increased by 47.6%, 35.5% and 29.53% respectively with 1.5 wt.% SBA15. It was found that the particle enhancement of uniform distributed SBA15 accounted for the mechanic reinforcement of the composite scaffold. It indicated that the PLLA-SBA15 composite scaffold had potential applications in bone tissue engineering.

Controlled release of phenytoin for epilepsy treatment from titania and silica based materials

Energy Technology Data Exchange (ETDEWEB)

Lopez, Tessy, E-mail: tessy3@prodigy.net.mx [Universidad Autonoma Metropolitana-Xochimilco. Departamento de Microbiologia. Calzada del Hueso 1100, Col. Villa Quietud, Coyoacan, C.P. 04960, Mexico D.F. Mexico (Mexico); Instituto Nacional de Neurologia y Neurocirugia ' MVS' . Laboratorio de Nanotecnologia. Av. Insurgentes Sur 3877, Col. La Fama, Tlalpan, 14269, Mexico, D.F. Mexico (Mexico); Department of Chemical and Biomolecular Engineering, Tulane University, New Orleans, LA 70118 (United States); Ortiz, Emma [Instituto Nacional de Neurologia y Neurocirugia ' MVS' . Laboratorio de Nanotecnologia. Av. Insurgentes Sur 3877, Col. La Fama, Tlalpan, 14269, Mexico, D.F. Mexico (Mexico); Meza, Doraliz [Universidad Autonoma Metropolitana-Iztapalapa, Departamento de Quimica, Av. San Rafael Atlixco 186, A.P. 55-534, Mexico D.F., C.P. 09340 (Mexico); Basaldella, Elena [CIC-CINDECA - Universidad Nacional de La Plata - Calle 47 No 257 - La Plata (Argentina); Bokhimi, Xim; Magana, Carlos [Instituto de fisica, UNAM. Circuito de la Investigacion s/n. C.U. Mexico D.F. 01000 (Mexico); Sepulveda, Antonio; Rodriguez, Francisco; Ruiz, Javier [Departamento de Quimica Inorganica, Universidad de Alicante. Apartado 99, E-03080 Alicante, Espana Spain (Spain)

2011-04-15

Research highlights: {yields} Template technique was used to obtain well ordered nanostructured materials: SBA-15 and titania tubes. {yields} Phenytoin (PH), a drug used in epilepsy treatment, was loaded in these materials to used como PH release. {yields} Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. {yields} The load-release PH are faster in nanostructured TiO2 tubes than in mesoporous silica matrix. {yields} There is an inverse effect of the surface area of the structured materials on the amount of released PH. - Abstract: Template technique was used to obtain well ordered nanostructured materials: mesoporous silica and nanostructured titania tubes. This technique permits the synthesis of solids with controlled mesoporosity, where a large variety of molecules that have therapeutic activity can be hosted and further released to specific sites. In this work phenytoin (PH), a drug used in epilepsy treatment, was loaded in ordered mesoporous silica (SBA 15) and nanostructured titania tubes (TiO{sub 2}). The pure materials and those containing PH were characterized by X-ray diffraction, FTIR spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N{sub 2} adsorption-desorption at 77 K. In order to determine the loading capacity of the antiepileptic drug on these silica- and titania-based materials, the loading and release of PH was investigated using UV-vis spectroscopy. Tubular structures were found for the titania samples, for which the X-ray diffractograms showed to be formed by anatase and rutile phases. On the other hand, an amorphous phase was found in the silica sample. A highly ordered hexagonal structure of 1D cylindrical channels was also observed for this material. Loaded PH showed a good stability inside the used materials as observed by spectroscopy analysis. The adsorption and desorption of PH are faster in nanostructured TiO{sub 2} tubes than in mesoporous silica

Fischer-Tropsch synthesis in slurry-phase reactors using Co/SBA-15 catalysts

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, J.J.; Lima, L.A.; Lima, W.S.; Rodrigues, M.G.F. [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia Quimica], e-mail: meiry@deq.ufcg.edu.br; Fernandes, F.A.N. [Universidade Federal do Ceara (UFCE), CE (Brazil). Dept. de Engenharia Quimica

2011-07-15

The objective of this work is to describe the production of bifunctional catalysts using the incipient humidity method, producing catalysts with 15 wt.% cobalt supported in SBA-15 molecular sieve, to be applied in the Fischer-Tropsch (FT) reaction. The originality of this work is its focus on the use of a 15 wt.% Co/SBA-15 catalyst in FT synthesis in slurry reactors. The deposition of cobalt over SBA-15 support was accomplished by impregnation with a 0.1-M aqueous solution of cobalt nitrate. The Fischer-Tropsch synthesis was carried out with the catalyst at 240 deg C and 20 atm, under a COH{sub 2} atmosphere (molar ratio= 1), in a slurry reactor for 8 hours. X-ray diffraction measurements showed that the calcined cobalt catalyst did not modify the structure of SBA-15, proving that Co was present under the form of Co{sub 3}O{sub 4} in the catalyst. The addition of cobalt in the SBA-15 decreased the specific superficial area of the molecular sieve. The 15 wt.% Co/SBA-15 catalyst had a 40% CO conversion rate and a high selectivity towards the production of C{sub 5}{sup +} (53.9% after 8 hours). (author)

Preparation of silica stabilized biological templates for the production of metal and layered nanoparticles

Science.gov (United States)

Culver, James N; Royston, Elizabeth; Brown, Adam; Harris, Michael

2013-02-26

The present invention relates to a system and method providing for increased silica growth on a bio-template, wherein the bio-template is pretreated with aniline to produce a uniform silica attractive surface and yielding a significant silica layers of at least 10 nm, and more preferably at least 20 nm in thickness, thereby providing for a high degree of stability to the bio-template.

Fabrication of silica hollow particles using yeast cells as a template

Science.gov (United States)

Liao, Shenglan; Lin, Liqin; Chen, Xiaofang; Liu, Jingru; Zhang, Biao

2018-04-01

Inorganic hollow particles have attracted great interest in recent years. In this study, silica micro spheres were produced. Yeast cells were used as a biological template. The silica shell was synthesized by the hydrolysis of tetraethoxysilane (TEOS) in water-alcohol mixtures as solvent using ammonia as a catalyst according to the Stoeber process. Various approaches including X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the products. The results showed that the thermally treated samples were SiO2 hollow microspheres with a diameter varying between 1-5μm.

Preparation and evaluation of aminopropyl-functionalized manganese-loaded SBA-15 for copper removal from aqueous solution.

Science.gov (United States)

Lei, Di; Zheng, Qianwen; Wang, Yili; Wang, Hongjie

2015-02-01

A novel material, aminopropyl-functionalized manganese-loaded SBA-15 (NH2-Mn-SBA-15), was synthesized by bonding 3-aminopropyl trimethoxysilane (APTMS) onto manganese-loaded SBA-15 (Mn-SBA-15) and used as a Cu2+ adsorbent in aqueous solution. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction spectra (XRD), N2 adsorption/desorption isotherms, high resolution field emission scanning electron microscopy (FESEM) and X-ray photoelectron spectroscopy (XPS) were used to characterize the NH2-Mn-SBA-15. The ordered mesoporous structure of SBA-15 was remained after modification. The manganese oxides were mainly loaded on the internal surface of the pore channels while the aminopropyl groups were mainly anchored on the external surface of SBA-15. The adsorption of Cu2+ on NH2-Mn-SBA-15 was fitted well by the Langmuir equation and the maximum adsorption capacity of NH2-Mn-SBA-15 for Cu2+ was over two times higher than that of Mn-SBA-15 under the same conditions. The Elovich equation gave a good fit for the adsorption process of Cu2+ by NH2-Mn-SBA-15 and Mn-SBA-15. Both the loaded manganese oxides and the anchored aminopropyl groups were found to contribute to the uptake of Cu2+. The NH2-Mn-SBA-15 showed high selectivity for copper ions. Consecutive adsorption-desorption experiments showed that the NH2-Mn-SBA-15 could be regenerated by acid treatment without altering its properties. Copyright © 2014. Published by Elsevier B.V.

Microporous silica prepared by organic templating: relationship between the molecular template and pore structure

International Nuclear Information System (INIS)

Brinker, C. Jeffrey; Cao, Guozhong; Kale, Rahul P.; Lopez, Gabriel P.; Lu, Yunfeng; Prabakar, S.

1999-01-01

Microporous silica materials with a controlled pore size and a narrow pore size distribution have been prepared by sol-gel processing using an organic-templating approach. Microporous networks were formed by pyrolytic removal of organic ligands (methacryloxypropyl groups) from organic/inorganic hybrid materials synthesized by copolymerization of 3-methacryloxypropylsilane (MPS) and tetraethoxysilane (TEOS). Molecular simulations and experimental measurements were conducted to examine the relationship between the microstructural characteristics of the porous silica (e.g., pore size, total pore volume, and pore connectivity) and the size and amount of organic template ligands added. Adsorption measurements suggest that the final porosity of the microporous silica is due to both primary pores (those present in the hybrid materials prior to pyrolysis) and secondary pores (those created by pyrolytic removal of organic templates). Primary pores were inaccessible to N(sub 2) at 77 K but accessible to CO(sub 2) at 195 K; secondary pores were accessible to both N(sub 2) (at 77 K) and CO(sub 2) (at 195 K) in adsorption measurements. Primary porosity decreases with the amount of organic ligands added because of the enhanced densification of MPS/TEOS hybrid materials as the mole fraction of trifunctional MPS moieties increases. pore volumes measured by nitrogen adsorption experiments at 77 K suggest that the secondary (template-derived) porosity exhibits a percolation behavior as the template concentration is increased. Gas permeation experiments indicate that the secondary pores are approximately 5(angstrom) in diameter, consistent with predictions based on molecular simulations

Aminopropyl-modified mesoporous silica SBA-15 as recovery agents of Cu(II)-sulfate solutions: Adsorption efficiency, functional stability and reusability aspects

International Nuclear Information System (INIS)

Lombardo, M.V.; Videla, M.; Calvo, A.; Requejo, F.G.; Soler-Illia, G.J.A.A.

2012-01-01

Highlights: ► We produce mesoporous amino-silica as Cu(II) adsorbent (1.15–1.75 mmol Cu(II) g −1 ). ► Elemental analysis and XPS demonstrate that amino groups concentrate at the material surface. ► The integrity of the adsorbent through the adsorption, desorption and recycling processes is assessed. ► These materials can be regenerated by exposure to acidic media. ► A careful thermal processing of the material is central to better durability during reprocessing. - Abstract: Hybrid mesoporous materials are potentially useful for metal ion scavenging and retrieval because of their high surface areas, controlled accessibility and tailored functionalization. Some aspects that are linked to the performance of HMM include pore accessibility, stability of the organic functions and reusability. Knowledge of these aspects is critical in the design of adsorption–desorption protocols. In this work we produce and characterize propylamino-substituted large pore silica (SBA-15-N), which is submitted to Cu(II) adsorption from copper sulfate solutions, followed by desorption in acid media and material regeneration. We find that the hybrid material is an efficient adsorbent (1.15–1.75 mmol Cu(II) g −1 ), although a fraction of the organic groups is lost during the adsorption process. An X-ray photoelectron spectroscopy (XPS) study demonstrates that the contents of amino groups are higher in the material surface, leading to different behaviors in Cu(II) complexation along the material. These materials can be regenerated by exposure to acidic media. Thermal processing of the hybrid materials leads to better durability in aqueous solutions during reprocessing, due to enhanced polycondensation of the inorganic framework. Thermally treated samples, once regenerated, are efficient adsorbents in a second step of Cu(II) adsorption. We discuss the materials processing factors involved in the improved adsorption of Cu(II), its quantitative release and reusability of the

Interactions of NO{sub 2} at ambient temperature with cerium-zirconium mixed oxides supported on SBA-15

Energy Technology Data Exchange (ETDEWEB)

Levasseur, Benoit; Ebrahim, Amani M. [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States); Burress, Jacob [NIST Center for Neutron Research, National Institute of Standards and Technology 100 Bureau Drive, Gaithersburg, MD 20899 (United States); Bandosz, Teresa J., E-mail: tbandosz@ccny.cuny.edu [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States)

2011-12-15

Highlights: Black-Right-Pointing-Pointer Ce{sub 1-y}Zr{sub y}O{sub 2-x} mixed oxides were highly dispersed in mesoporous silica SBA-15. Black-Right-Pointing-Pointer A strong increase in the NO{sub 2} adsorption capacity was observed on composites. Black-Right-Pointing-Pointer The insertion of Zr{sup 4+} in ceria fluorite structure promotes the reduction of Ce{sup 4+} into Ce{sup 3+}. Black-Right-Pointing-Pointer Ce{sup 3+} and -OH groups were found to be the main active centers for NO{sub x} retention. Black-Right-Pointing-Pointer The structure remains quite stable after exposure to NO{sub 2} in ambient conditions. - Abstract: New silica-based composites were obtained using a slow precipitation of mixed oxide Ce{sub 1-x}Zr{sub x}O{sub 2} on the surface of mesoporous silica, SBA-15. The samples were tested as NO{sub 2} adsorbents in dynamic conditions at room temperature. The surface of the initial and exhausted materials was characterized using N{sub 2} sorption, XRD, TEM, potentiometric titration, and thermal analysis before and after exposure to NO{sub 2}. In comparison with unsupported Ce{sub 1-x}Zr{sub x}O{sub 2} mixed oxides, a significant increase in the NO{sub 2} adsorption capacity was observed. This is due to the high dispersion of active oxide phase on the surface of SBA-15. A linear trend was found between the NO{sub 2} adsorption capacity and the amount of Zr(OH){sub 4} added to the structure. Introduction of Zr{sup 4+} cations to ceria contributes to an increase in the amount of Ce{sup 3+}, which is the active center for the NO{sub 2} adsorption, and to an increase in the density of -OH groups. These groups are found to be involved in the retention of both NO{sub 2} and NO on the surface. After exposure to NO{sub 2}, an acidification of the surface caused by the oxidation of the cerium as well as the formation of nitrite and nitrates took place. The structure of the composites appears not to be affected by reactive adsorption of NO{sub 2}.

Effect of ceria and zirconia promotors on Ni/SBA-15 catalysts for coking and sintering resistant steam reforming of propylene glycol in microreactors

NARCIS (Netherlands)

Shanmugam, V.; Zapf, R.; Neuberg, S.; Hessel, V.; Kolb, G.

2017-01-01

Highly dispersed and size controlled Ni nanoparticles in CeO2, ZrO2 and CeO2-ZrO2 promoted mesoporous SBA-15 silica were achieved with the aid of treatment by ultrasound. The catalysts were characterized systematically to investigate their morphological structure and surface properties. It was found

The Effect of Nitrogen Surface Ligands on Propane Metathesis: Design and Characterizations of N-modified SBA15-Supported Schrock-type Tungsten Alkylidyne

KAUST Repository

Eid, Ahmed A.

2014-04-01

Catalysis, which is primarily a molecular phenomenon, is an important field of chemistry because it requires the chemical conversion of molecules into other molecules. It also has an effect on many fields, including, but not limited to, industry, environment and life Science[1]. Surface Organometallic Chemistry is an effective methodology for Catalysis as it imports the concept and mechanism of organometallic chemistry, to surface science and heterogeneous catalysis. So, it bridges the gap between homogenous and heterogeneous catalysis[1]. The aim of the present research work is to study the effect of Nitrogen surface ligands on the activity of Alkane, Propane in particular, metathesis. Our approach is based on the preparation of selectively well-defined group (VI) transition metal complexes supported onto mesoporous materials, SBA15 and bearing amido and/or imido ligands. We choose nitrogen ligands because, according to the literature, they showed in some cases better catalytic properties in homogenous catalysis in comparison with their oxygen counterparts[2]. The first section covers the modification of a highly dehydroxylated SBA15 surface using a controlled ammonia treatment. These will result in the preparation of two kind of Nitrogen surface ligands: -\\tOne with vicinal silylamine/silanol, (≡SiNH2)(≡SiOH), noted [N,O]SBA15 and, -\\tAnother\\tone\\twith\\tvicinal\\tbis-silylamine moieties (≡SiNH2)2, noted [N,N]SBA15[3]. The second section covers the reaction of Schrock type Tungsten Carbyne [W(≡C- tBu)(CH2-tBu)3] with those N-surface ligands and their characterizations by FT-IR, multiple quantum solid state NMR (1H, 13C), elemental analysis and gas phase analysis. The third section covers the generation of the active site, tungsten hydride species. Their performance toward propane metathesis reaction using the dynamic reactor technique PID compared toward previous well-known catalysts supported on silica oxide or mesoporous materials[4]. A fairly good

Grafted chromium 13-membered dioxo-macrocyclic complex into aminopropyl-based nanoporous SBA-15

Energy Technology Data Exchange (ETDEWEB)

Tarlani, Aliakbar, E-mail: Tarlani@ccerci.ac.ir [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of); Joharian, Monika; Narimani, Khashayar [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of); Muzart, Jacques [Institut de Chimie Moléculaire de Reims, CNRS-Université de Reims Champagne-Ardenne, BP 1039, 51687 Reims Cedex 2 (France); Fallah, Mahtab [Inorganic Nanostructures and Catalysts Research Laboratory, Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Boulevard, km 17, Karaj Highway, Tehran 14968-13151 (Iran, Islamic Republic of)

2013-07-15

In a new approach, chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 after four step reactions by using coordinating ability of anchored amino functionalized SBA-15. After the termination of each step, the obtained product was characterized by FT-IR, low-angle X-ray diffraction (LA-XRD), N{sub 2} adsorption–desorption isotherms (Brunauer–Emmett–Teller (BET)–Barret–Joyner–Halenda (BJH)) and thermogravimetric analysis (TGA), and used as catalyst for the efficient and regioselective alcoholysis of styrene oxide to 2-alkoxy-1-phenylethanol product at ambient temperature. - Graphical abstract: Chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 using coordinating ability of anchored amino functionalized SBA-15. Preparation of the catalyst is depicted in Scheme 1. - Highlights: • Dioxo tetraazachromium macrocyclic complex grafted into the SBA-15-NH{sub 2} channels. • The bond is created by coordinating ability of anchored amino functionalized SBA-15. • The prepared nanocatalyst has superior activity in the alcoholysis of styrene oxide. • The catalyst is reusable at ambient temperature for the mentioned reaction.

High surface area TiO2/SBA-15 nanocomposites: Synthesis, microstructure and adsorption-enhanced photocatalysis

Science.gov (United States)

Wei, J. Q.; Chen, X. J.; Wang, P. F.; Han, Y. B.; Xu, J. C.; Hong, B.; Jin, H. X.; Jin, D. F.; Peng, X. L.; Li, J.; Yang, Y. T.; Ge, H. L.; Wang, X. Q.

2018-06-01

Mesoporous SBA-15 was used to anchor TiO2 nanoparticles into the mesopores to form high surface area TiO2/SBA-15 nanocomposites, and then the influence of mesoporous-structure on the photocatalytic performance was investigated. TiO2/SBA-15 nanocomposites possessed the high specific surface area and appropriate pore size, indicating the excellent adsorption performance. TiO2/SBA-15 nanocomposites exhibited the higher photocatalytic activity to degrade dyes (methylene blue: MB) than TiO2 (removing SBA-15), which should attributed to the excellent adsorption performance of the nanocomposites. MB was absorbed to form the higher concentration near TiO2/SBA-15 photocatalysts, and the photocatalytic degradation for MB was improved.

Ascorbyl Tetraisopalmitate Inclusion into Υ-Cyclodextrin and Mesoporous SBA-15: Preparation, Characterization and In Vitro Release Study

Directory of Open Access Journals (Sweden)

Maria Bastianini

2017-07-01

Full Text Available Ascorbic acid or vitamin C is a strong antioxidant widely used in cosmetic and food fields. This vitamin is very unstable and rapidly undergoes degradation. In order to solve this problem and to obtain a stable ascorbic acid, Nikkol Group has developed ascorbyltetraisopalmitate (VC-IP. This raw material is an oil phase, already well-known and employed in the cosmetic market. The objective of this study is to obtain VC-IP in micro-powder form, in order to produce a new raw material that is easily dispersible in oil and water phases and useful for make-up and color cosmetic applications. Various types of drug carriers were studied and considered in order to support VC-IP and obtain the conversion in powder. Υ-cyclodextrin and mesoporous silica SBA-15 were chosen as the best candidates. A white powder of supported VC-IP was obtained with each carrier (VC-IP@cyclodextrin, VC-IP@SBA-15. The systems underwent physicochemical characterization and in vitro release tests were carried out. Based on the conducted study, it can be concluded that by supporting VC-IP on Υ-cyclodextrin and SBA-15, it is feasible to obtain a new raw material in powder form. The two carriers possess different release profiles, adding the possibility to finely tune the release of the active component in smart formulations.

Textural and morphological studies of transition metal doped SBA ...

Indian Academy of Sciences (India)

J. Chem. Sci. Vol. 127, No. 5, May 2015, pp. 909–919. c Indian Academy of Sciences. ... The difference in hydrolysis rates of metal and silica precursors have led to textural ... tures of mesoporous SBA-15.13 General shape-selective.

A well-defined mesoporous amine silica surface via a selective treatment of SBA-15 with ammonia

KAUST Repository

Bendjeriou-Sedjerari, Anissa; Pelletier, Jeremie; Abou-Hamad, Edy; Emsley, Lyndon; Basset, Jean-Marie

2012-01-01

2D double-quantum 1H- 1H NMR unambiguously shows that the "isolated" Si-OH surface silanols of dehydroxylated SBA-15 are converted upon treatment with ammonia into single silylamine surface site Si-NH 2. The "gem" di-silanols (Si(OH) 2) remain intact. Treatment using HMDS produces (Si(OSiMe 3) 2) but leaves Si-NH 2 untouched. The resulting surface is hydrophobic and stable. © The Royal Society of Chemistry 2012.

Synthesis of ordered mesoporous uranium dioxide by a nanocasting route

Energy Technology Data Exchange (ETDEWEB)

Zhao, Ran; Wang Lin; Shi, Wei-Qun [Chinese Academy of Sciences, Beijing (China). Laboratory of Nuclear Energy Chemistry and Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety; Chai, Zhi-Fang [Chinese Academy of Sciences, Beijing (China). Laboratory of Nuclear Energy Chemistry and Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences and Collaborative Innovation Center

2016-11-01

Ordered mesoporous UO{sub 2} with 3-D structure (for UO{sub 2}-KIT-6) and nanowire bundles (for UO{sub 2}-SBA-15) was synthesized for the first time by a nanocasting route using different ordered mesoporous silica (KIT-6 and SBA-15, respectively) as templates and uranyl nitrate hexahydrate as the metal precursor. The uranyl nitrate was impregnated into the mesopore of the silica template and was converted to U{sub 3}O{sub 8} after the first step. The synthesis of ordered UO{sub 2} mesostructure was achieved by reducing the mesoporous U{sub 3}O{sub 8} with silica composites under 5% H{sub 2}/Ar atmosphere at 700 C, followed by a template removal process. The as-prepared UO{sub 2}-KIT-6 had a particle size of several millimeters, and was constructed with uncoupled subframework mesostructure and crystalline walls, while UO{sub 2}-SBA-15 possessed a rope-like morphology and consisted of nanowire arrays. The surface area and pore volume of ordered UO{sub 2} mesostructure are 47.2 m{sup 2} g{sup -1} and 0.23 cm{sup 3} g{sup -1} for the UO{sub 2}-KIT-6, and 54.4 m{sup 2} g{sup -1} and 0.28 cm{sup 3} g{sup -1} for the UO{sub 2}-SBA-15, respectively.

Dehydrogenation of Isobutane with Carbon Dioxide over SBA-15-Supported Vanadium Oxide Catalysts

Directory of Open Access Journals (Sweden)

Chunling Wei

2016-10-01

Full Text Available A series of vanadia catalysts supported on SBA-15 (V/SBA with a vanadia (V content ranging from 1% to 11% were prepared by an incipient wetness method. Their catalytic behavior in the dehydrogenation of isobutane to isobutene with CO2 was examined. The catalysts were characterized by N2 adsorption, X-ray diffraction (XRD, scanning electron microscopy (SEM, Raman spectroscopy, and temperature-programmed reduction (TPR. It was found that these catalysts were effective for the dehydrogenation reaction, and the catalytic activity is correlated with the amount of dispersed vanadium species on the SBA-15 support. The 7% V/SBA catalyst shows the highest activity, which gives 40.8% isobutane conversion and 84.8% isobutene selectivity. The SBA-15-supported vanadia exhibits higher isobutane conversion and isobutene selectivity than the MCM-41-supported one.

Insights into the Hydrothermal Stability of Triamine-Functionalized SBA-15 Silica for CO2 Adsorption.

Science.gov (United States)

Jahandar Lashaki, Masoud; Ziaei-Azad, Hessam; Sayari, Abdelhamid

2017-10-23

The hydrothermal stability of triamine-grafted, large-pore SBA-15 CO 2 adsorbents was studied by using steam stripping. Following two 3 h cycles of steam regeneration, lower CO 2 uptakes, lower CO 2 /N ratios, and slower adsorption kinetics were observed relative to fresh samples, particularly at the lowest adsorption temperature (25 °C). CO 2 adsorption measurements for a selected sample exposed to 48 h of steam stripping depicted that after the initial loss during the first exposure to steam (3-6 h), the adsorptive properties stabilized. For higher adsorption temperatures (i.e., 50 and 75 °C), however, all adsorptive properties remained almost unchanged after steaming, indicating the significance of diffusional limitations. Thermogravimetric analysis and FTIR spectroscopy on grafted samples before and after steam stripping showed no amine leaching and no change in the chemical nature of the amine groups, respectively. Also, a six-cycle CO 2 adsorption/desorption experiment under dry conditions showed no thermal degradation. However, N 2 adsorption measurement at 77 K showed significant reductions in the BET surface area of the grafted samples following steaming. Based on the pore size distribution of calcined, grafted samples before and after steaming, it is proposed that exposure to steam restructured the grafted materials, causing mass transfer resistance. It is inferred that triamine-grafted, large-pore SBA-15 adsorbents are potential candidates for CO 2 capture at relatively high temperatures (50-75 °C; for example, flue gas) combined with steam regeneration. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Aminopropyl-modified mesoporous silica SBA-15 as recovery agents of Cu(II)-sulfate solutions: Adsorption efficiency, functional stability and reusability aspects

Energy Technology Data Exchange (ETDEWEB)

Lombardo, M.V. [Gerencia Quimica, Centro Atomico Constituyentes, CNEA, Av. General Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina); Videla, M. [Rhein Chemie Argentina, Luis Maria Drago 1555 - (B1852LGS) Burzaco, Buenos Aires (Argentina); Calvo, A.; Requejo, F.G. [INIFTA-CONICET, Universidad Nacional de La Plata, CC 16 Sucursal 4 (1900), La Plata (Argentina); Soler-Illia, G.J.A.A., E-mail: gsoler@cnea.gov.ar [Gerencia Quimica, Centro Atomico Constituyentes, CNEA, Av. General Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina); DQIAyQF, FCEN, Universidad de Buenos Aires, Ciudad Universitaria, Pab. II (C1428EHA), Buenos Aires (Argentina)

2012-07-15

Highlights: Black-Right-Pointing-Pointer We produce mesoporous amino-silica as Cu(II) adsorbent (1.15-1.75 mmol Cu(II) g{sup -1}). Black-Right-Pointing-Pointer Elemental analysis and XPS demonstrate that amino groups concentrate at the material surface. Black-Right-Pointing-Pointer The integrity of the adsorbent through the adsorption, desorption and recycling processes is assessed. Black-Right-Pointing-Pointer These materials can be regenerated by exposure to acidic media. Black-Right-Pointing-Pointer A careful thermal processing of the material is central to better durability during reprocessing. - Abstract: Hybrid mesoporous materials are potentially useful for metal ion scavenging and retrieval because of their high surface areas, controlled accessibility and tailored functionalization. Some aspects that are linked to the performance of HMM include pore accessibility, stability of the organic functions and reusability. Knowledge of these aspects is critical in the design of adsorption-desorption protocols. In this work we produce and characterize propylamino-substituted large pore silica (SBA-15-N), which is submitted to Cu(II) adsorption from copper sulfate solutions, followed by desorption in acid media and material regeneration. We find that the hybrid material is an efficient adsorbent (1.15-1.75 mmol Cu(II) g{sup -1}), although a fraction of the organic groups is lost during the adsorption process. An X-ray photoelectron spectroscopy (XPS) study demonstrates that the contents of amino groups are higher in the material surface, leading to different behaviors in Cu(II) complexation along the material. These materials can be regenerated by exposure to acidic media. Thermal processing of the hybrid materials leads to better durability in aqueous solutions during reprocessing, due to enhanced polycondensation of the inorganic framework. Thermally treated samples, once regenerated, are efficient adsorbents in a second step of Cu(II) adsorption. We discuss the

A Pd/SBA-15 composite: synthesis, characterization and protein biosensing

Energy Technology Data Exchange (ETDEWEB)

Liu Yuge; Zhang Jingjing; Hou Wenhua; Zhu Junjie [Key Laboratory of Mesoscopic Chemistry and Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China)], E-mail: whou@nju.edu.cn, E-mail: jjzhu@nju.edu.cn

2008-04-02

In this paper, palladium (Pd) nanoparticles have been successfully encapsulated into the channels of modified SBA-15 in situ via a facile, ethylene glycol (EG)-assisted sonochemical method. The products were confirmed by x-ray diffraction, transmission electron microscopy (TEM) and nitrogen adsorption analysis. The Pd/SBA-15 composite was used for the realization of direct electron transfer of hemoglobin (Hb). Electrochemical results showed that the Pd nanoparticles in the channels of SBA-15 could enhance the direct electron transfer between Hb and the electrode surface. The composite modified electrode displayed excellent electrochemical behavior. The sensor fabricated by the composite showed an excellent response to the reduction of hydrogen peroxide (H{sub 2}O{sub 2}), and the linear range for the determination of H{sub 2}O{sub 2} was from 1.8 to 119.3 {mu}M with a detection limit of 0.8 {mu}M.

Photocatalytic activity of Ce-modified SBA-15 for the degradation of ...

Indian Academy of Sciences (India)

transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and N2 adsorption/desorption analysis. ... water.7,8,18 Existence of different sites of cerium ions and ... hydrocarbons.21 In this study, Ce-SBA-15 and Ce-Al-SBA-.

Selective Preparation of Furfural from Xylose over Sulfonic Acid Functionalized Mesoporous Sba-15 Materials

Directory of Open Access Journals (Sweden)

Panpan Li

2011-04-01

Full Text Available Sulfonic acid functionalized mesoporous SBA-15 materials were prepared using the co-condensation and grafting methods, respectively, and their catalytic performance in the dehydration of xylose to furfural was examined. SBA-15-SO3H(C prepared by the co-condensation method showed 92–95% xylose conversion and 74% furfural selectivity, and 68–70% furfural yield under the given reaction conditions. The deactivation and regeneration of the SBA-15-SO3H(C catalyst for the dehydration of xylose was also investigated. The results indicate that the used and regeneration catalysts retained the SBA-15 mesoporous structure, and the S content of SBA-15-SO3H(C almost did not change. The deactivation of the catalysts is proposed to be associated with the accumulation of byproducts, which is caused by the loss reaction of furfural. After regeneration by H2O2, the catalytic activity of the catalyst almost recovered.

Efficient epoxidation over cyanocobalamine containing SBA-15 organic-inorganic nanohybrids

Energy Technology Data Exchange (ETDEWEB)

Karimi, Z. [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mahjoub, A.R., E-mail: mahjouba@modares.ac.ir [Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

2010-05-01

SBA-15 mesoporous silica is synthesized using triblock copolymer P123 surfactant and chemically modified by aminopropyl, thiol, ammonium and sulfonic acid functional groups. Functionalization is performed via post synthesize method using 3-aminopropyltriethoxysilane (APTES) or 3-mercatopropyl trimethoxysilane (MPTMS) precursor. The as synthesized mesoporous systems are applied for immobilization of cyanocobalamine. Functionalization effectively improves sorption properties of the supports, while different functional groups exert different effects. The organic-inorganic mesoporous materials are characterized via X-ray diffraction (XRD), nitrogen adsorption and desorption, transmission electron microscopy (TEM), FT-IR and inductively coupled plasma-optical emission (ICP). The newly synthesized systems exhibit high catalytic activity for heterogeneous epoxidation of cyclooctene in presence of hydrogen peroxide. Reaction conditions are optimized, effect of functional groups on performance of the catalysts is taken into consideration and reusability of the designed heterogeneous systems is studied. Systems with chemically modified supports are shown to be more efficient and stable catalysts however; chemical nature of functional groups plays a crucial role.

Highly stable and regenerable Mn-based/SBA-15 sorbents for desulfurization of hot coal gas

International Nuclear Information System (INIS)

Zhang, F.M.; Liu, B.S.; Zhang, Y.; Guo, Y.H.; Wan, Z.Y.; Subhan, Fazle

2012-01-01

Highlights: ► A series of mesoporous Cu x Mn y O z /SBA-15 sorbents were fabricated for hot coal gas desulfurization. ► 1Cu9Mn/SBA-15 sorbent with high breakthrough sulfur capacity is high stable and regenerable. ► Utilization of SBA-15 constrained the sintering and pulverization of sorbents. - Abstract: A series of mesoporous xCuyMn/SBA-15 sorbents with different Cu/Mn atomic ratios were prepared by wet impregnation method and their desulfurization performance in hot coal gas was investigated in a fixed-bed quartz reactor in the range of 700–850 °C. The successive nine desulfurization–regeneration cycles at 800 °C revealed that 1Cu9Mn/SBA-15 presented high performance with durable regeneration ability due to the high dispersion of Mn 2 O 3 particles incorporated with a certain amount of copper oxides. The breakthrough sulfur capacity of 1Cu9Mn/SBA-15 observed 800 °C is 13.8 g S/100 g sorbents, which is remarkably higher than these of 40 wt%LaFeO 3 /SBA-15 (4.8 g S/100 g sorbents) and 50 wt%LaFe 2 O x /MCM-41 (5.58 g S/100 g sorbents) used only at 500–550 °C. This suggested that the loading of Mn 2 O 3 active species with high thermal stability to SBA-15 support significantly increased sulfur capacity at relatively higher sulfidation temperature. The fresh and used xCuyMn/SBA-15 sorbents were characterized by means of BET, XRD, XPS, XAES, TG/DSC and HRTEM techniques, confirmed that the structure of the sorbents remained intact before and after hot coal gas desulfurization.

Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

International Nuclear Information System (INIS)

Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

2015-01-01

Graphical abstract: Ligand-modified signal-site SBA-15 supported zirconium catalysts were synthesized by SOMC method and characterized by a variety of techniques. The zirconium surface complexes show high catalytic efficiency for cyanosilylation of benzaldehyde. - Highlights: • Some Zr active species have been anchored on the surface of SBA-15 by SOMC technique. • The structures of the Zr species have been characterized by a variety of techniques. • The anchored Zr species are single-sited surface complexes. • The Zr surface complexes are catalytic active for cyanosilylation of benzaldehyde. - Abstract: A successive anchoring of Zr(NMe 2 ) 4 , cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15 -500 ) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15 -500 supported zirconium complexes were characterized by in situ FT-IR, 13 C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands

Amine-modified ordered mesoporous silica: Effect of pore size on carbon dioxide capture

Energy Technology Data Exchange (ETDEWEB)

V. Zelenak; M. Badanicova; D. Halamova; J. Cejka; A. Zukal; N. Murafa; G. Goerigk [P.J. Safarik University, Kosice (Slovak Republic)

2008-10-15

Three mesoporous silica materials with different pore sizes and pore connectivity were prepared and functionalized with aminopropyl (AP) ligands by post-synthesis treatment. The materials were characterized by small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and nitrogen adsorption/desorption experiments. The carbon dioxide sorption on modified mesoporous molecular sieves was investigated by using of microbalances at 25{sup o}C, and the influence of pore size and pore architecture on CO{sub 2} sorption was discussed. The large pore silica, SBA-15, showed the largest carbon dioxide sorption capacity (1.5 mmol/g), relating to highest amine surface density in this material. On the other hand, three-dimensional accessibility of amine sites inside the pores of SBA-12 silica resulted in a faster response to CO{sub 2} uptake in comparison with MCM-41 and SBA-15 molecular sieves

Catalytic Activity and Photophysical Properties of Biomolecules Immobilized on Mesoporous Silica

DEFF Research Database (Denmark)

Ikemoto, Hideki

Mesoporous silicas, based on Santa Barbara Amorphous-15 (SBA-15), with different morphology, structure, pore size and functional groups have been synthesized. Two metalloenzymes and a photosynthetic membrane protein were immobilized on or confined in the pores of the mesoporous silicas to prepare...

Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnOx/SBA-15

International Nuclear Information System (INIS)

Sun, Qiangqiang; Wang, Yu; Li, Laisheng; Bing, Jishuai; Wang, Yingxin; Yan, Huihua

2015-01-01

Highlights: • Clofibric acid (CA) is efficiently mineralized by O 3 /MnO x /SBA-15. • Adsorption of CA and its intermediates on MnO x /SBA-15 is proved unimportant. • Initiation of hydroxyl radicals (·OH) is enhanced in O 3 /MnO x /SBA-15. • Uniformly distributed MnO x accounts for the high activity of MnO x /SBA-15. • Degradation routes of CA in ozonation alone and catalytic ozonation are proposed. - Abstract: Comparative experiments were conducted to investigate the catalytic ability of MnO x /SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O 3 /MnO x /SBA-15). Adsorption of CA and its intermediates by MnO x /SBA-15 was proved unimportant in O 3 /MnO x /SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO 3 ) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO x /SBA-15 facilitated the generation of hydroxyl radicals (·OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO x on SBA-15 were believed to be the main active component in MnO x /SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more ·OH

Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

Energy Technology Data Exchange (ETDEWEB)

Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang, E-mail: gfzhang@snnu.edu.cn; Gao, Ziwei, E-mail: zwgao@snnu.edu.cn

2015-01-15

Graphical abstract: Ligand-modified signal-site SBA-15 supported zirconium catalysts were synthesized by SOMC method and characterized by a variety of techniques. The zirconium surface complexes show high catalytic efficiency for cyanosilylation of benzaldehyde. - Highlights: • Some Zr active species have been anchored on the surface of SBA-15 by SOMC technique. • The structures of the Zr species have been characterized by a variety of techniques. • The anchored Zr species are single-sited surface complexes. • The Zr surface complexes are catalytic active for cyanosilylation of benzaldehyde. - Abstract: A successive anchoring of Zr(NMe{sub 2}){sub 4}, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1′-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15{sub -500}) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15{sub -500} supported zirconium complexes were characterized by in situ FT-IR, {sup 13}C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands.

Silica-Silver Nanocomposites as Regenerable Sorbents for Hg0 Removal from Flue Gases.

Science.gov (United States)

Cao, Tiantian; Li, Zhen; Xiong, Yong; Yang, Yue; Xu, Shengming; Bisson, Teresa; Gupta, Rajender; Xu, Zhenghe

2017-10-17

Silica-silver nanocomposites (Ag-SBA-15) are a novel class of multifunctional materials with potential applications as sorbents, catalysts, sensors, and disinfectants. In this work, an innovative yet simple and robust method of depositing silver nanoparticles on a mesoporous silica (SBA-15) was developed. The synthesized Ag-SBA-15 was found to achieve a complete capture of Hg 0 at temperatures up to 200 °C. Silver nanoparticles on the SBA-15 were shown to be the critical active sites for the capture of Hg 0 by the Ag-Hg 0 amalgamation mechanism. An Hg 0 capture capacity as high as 13.2 mg·g -1 was achieved by Ag(10)-SBA-15, which is much higher than that achievable by existing Ag-based sorbents and comparable with that achieved by commercial activated carbon. Even after exposure to more complex simulated flue gas flow for 1 h, the Ag(10)-SBA-15 could still achieve an Hg 0 removal efficiency as high as 91.6% with a Hg 0 capture capacity of 457.3 μg·g -1 . More importantly, the spent sorbent could be effectively regenerated and reused without noticeable performance degradation over five cycles. The excellent Hg 0 removal efficiency combined with a simple synthesis procedure, strong tolerance to complex flue gas environment, great thermal stability, and outstanding regeneration capability make the Ag-SBA-15 a promising sorbent for practical applications to Hg 0 capture from coal-fired flue gases.

Improved antimicrobial property and controlled drug release kinetics of silver sulfadiazine loaded ordered mesoporous silica

Directory of Open Access Journals (Sweden)

Suman Jangra

2016-09-01

Full Text Available The present study deals with the loading of silver sulfadiazine into ordered mesoporous silica material by post-impregnation method and its effect on the in vitro release kinetics and antimicrobial property of the drug. The formulated SBA-15 silica material with rope-like morphology and SBA-15-silver sulfadiazine (SBA-AgSD were characterized by UV–visible spectrophotometer, small and wide-angle powder X-ray diffraction (PXRD, field emission scanning electron microscope (FESEM and high resolution transmission electron microscope (HRTEM. Thermo-gravimetric analysis of SBA-AgSD revealed a high loading amount of 52.87%. Nitrogen adsorption–desorption analysis confirmed the drug entrapment into host material by revealing a reduced surface area (214 m2/g and pore diameter (6.7 nm of the SBA-AgSD. The controlled release of silver sulfadiazine drug from the mesoporous silica to simulated gastric, intestinal and body fluids was evaluated. The Korsmeyer–Peppas model fits the drug release data with the non-Fickian diffusion model and zero order kinetics of SBA-AgSD. The antibacterial performance of the SBA-AgSD was evaluated with respect to Staphylococcus aureus, Bacillus subtilis and Pseudomonas aeruginosa. The controlled drug delivery of the SBA-AgSD revealed improved antibacterial activity, thus endorsing its applicability in effective wound dressing.

Characterization of crystalline silica nanorods synthesized via a solvothermal route using polyvinylbutyral as a template

International Nuclear Information System (INIS)

Chen, Lin-Jer; Liao, Jiunn-Der; Chuang, Yu-Ju; Fu, Yaw-Shyan

2011-01-01

The preparation of crystalline silica nanorods is presented. Crystalline silica nanorods were synthesized via a simple solvothermal route using polyvinylbutyral (PVB) as a template in an autoclave with ethylenediamine as a solvent at 180 °C for 25 h. Silica nanorods with diameters in the range of 50–80 nm were obtained. The solvothermal route with a PVB template played affected the crystallization process and the growth of the silica nanorods. The as-synthesized products were characterized using X-ray diffraction, energy dispersive spectrometry, scanning electron microscopy, and transmission electron microscopy.

Single-site SBA-15 supported zirconium catalysts. Synthesis, characterization and toward cyanosilylation reaction

Science.gov (United States)

Xu, Wei; Yu, Bo; Zhang, Ying; Chen, Xi; Zhang, Guofang; Gao, Ziwei

2015-01-01

A successive anchoring of Zr(NMe2)4, cyclopentadiene and a O-donor ligand, 1-hydroxyethylbenzene (PEA), 1,1‧-bi-2-naphthol (Binol) or 2,3-dihydroxybutanedioic acid diethyl ester (Tartrate), on dehydroxylated SBA-15 pretreated at 500 °C for 16 h (SBA-15-500) was conducted by SOMC strategy in moderate conditions. The dehydoxylation of SBA-15 was monitored by in situ Fourier transform infrared spectroscopy (in situ FT-IR). The ligand-modified SBA-15-500 supported zirconium complexes were characterized by in situ FT-IR, 13C CP MAS-NMR, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MAS) and elemental analysis in detail, verifying that the surface zirconium species are single-sited. The catalytic activity of these complexes was evaluated by cyanosilylation of benzaldehyde. The results showed that the catalytic activity is dependent strongly on the structure of surface species and the configuration of the ligands.

Evaluation of bi-functionalized mesoporous silicas as reversed phase/cation-exchange mixed-mode sorbents for multi-residue solid phase extraction of veterinary drug residues in meat samples.

Science.gov (United States)

Casado, Natalia; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

2017-04-01

A SBA-15 type mesoporous silica was synthesized and bi-functionalized with octadecylsilane (C18) or octylsilane (C8), and sulfonic acid (SO 3 - ) groups in order to obtain materials with reversed-phase/strong cation-exchange mixed-mode retention mechanism. The resulting hybrid materials (SBA-15-C18-SO 3 - and SBA-15-C8-SO 3 - ) were comprehensively characterized. They showed high surface area, high pore volume and controlled porous size. Elemental analysis of the materials revealed differences in the amount of C18 and C8. SBA-15-C18-SO 3 - contained 0.19mmol/g of C18, while SBA-15-C8-SO 3 - presented 0.54mmol/g of C8. The SO 3 - groups anchored to the silica surface of the pore walls were 0.20 and 0.09mmol/g, respectively. The bi-functionalized materials were evaluated as SPE sorbents for the multi-residue extraction of 26 veterinary drug residues in meat samples using ultra-high-performance liquid chromatography coupled to mass spectrometry detector (UHPLC-MS/MS). Different sorbent amounts (100 and 200mg) and organic solvents were tested to optimize the extraction procedure. Both silicas showed big extraction potential and were successful in the extraction of the target analytes. The mixed-mode retention mechanism was confirmed by comparing both silicas with SBA-15 mesoporous silica mono-functionalized with C18 and C8. Best results were achieved with 200mg of SBA-15-C18-SO 3 - obtaining recoveries higher than 70% for the majority of analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

Facile fabrication of mesoporous Fe-Ti-SBA15 silica with enhanced visible-light-driven simultaneous photocatalytic degradation and reduction reactions

Science.gov (United States)

Chang, Fei; Jiao, Mingzhi; Xu, Quan; Deng, Baoqing; Hu, Xuefeng

2018-03-01

A series of mesoporous iron-titanium-containing silica Fe-TiO2-SBA15 (FTS) were constructed via a facile one-pot hydrothermal route and subsequently characterized by X-ray diffraction patterns, UV-vis diffuse reflection spectroscopy, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption-desorption, X-ray photoelectron spectroscopy, and X-ray energy dispersion spectroscopy. By analyses, these samples possessed ordered two-dimensional hexagonal mesoporous structures, mainly involving mixed dual-phases of anatase and rutile TiO2, like commercial titania P25. The UV-vis diffuse reflection spectra demonstrated the presence of Fe species that was further confirmed by the X-ray photoelectron spectra and X-ray energy dispersion spectrum. The existence of Fe species in form of Fe3+ cations played an important role on the phase composition and electronic structure of these samples. With structural and morphological merits, these samples exhibited relatively high photocatalytic efficiency toward the degradation of dye methylene blue (MB) and reduction of Cr(VI) under visible-light irradiation, comparing with P25. In addition, among all candidates, the sample with a Fe/Si molar ratio of 0.03 showed the highest catalytic performance under optimal conditions, especially in the coexistence of both MB and Cr(VI), revealing an obviously synergistic effect when the consumption of both contaminants occurred. Finally, a primary catalytic mechanism was speculated on basis of active species capture experiments.

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

Energy Technology Data Exchange (ETDEWEB)

Yang, Jae Hwan [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of); Park, Hwan Seo; Ahn, Do-Hee [Nuclear Fuel Cycle Process Development Division, Korea Atomic Energy Research Institute, 989-111 Daeduk-daero, Yuseong-gu, Daejeon, 305-353 (Korea, Republic of); Yim, Man-Sung, E-mail: msyim@kaist.ac.kr [Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of)

2016-11-15

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi{sub 2}O{sub 3} (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi{sub 2}O{sub 3} and the glass composition. It was confirmed that BiI{sub 3}, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi{sub 5}O{sub 7}I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10{sup −3}–10{sup −2} g/m{sup 2} day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of {sup 129}I. - Highlights: • Glass composite waste forms were developed to stabilize iodine confined in Bi-embedded SBA-15. • BiI{sub 3} within Bi-embedded SBA-15 was transformed to BiOI and Bi{sub 5}O{sub 7}I during sintering process. • Iodine volatility was significantly affected by glass composition and Bi{sub 2}O{sub 3} additive. • Iodine leaching rates were 10{sup −3}–10{sup −2} g/m{sup 2} day due to the stable iodine phases encapsulated by glassy networks. • Glass composite waste form of Bi-embedded SBA-15 is expected to be a candidate material for stable storage of {sup 129}I.

Soft template synthesis of yolk/silica shell particles.

Science.gov (United States)

Wu, Xue-Jun; Xu, Dongsheng

2010-04-06

Yolk/shell particles possess a unique structure that is composed of hollow shells that encapsulate other particles but with an interstitial space between them. These structures are different from core/shell particles in that the core particles are freely movable in the shell. Yolk/shell particles combine the properties of each component, and can find potential applications in catalysis, lithium ion batteries, and biosensors. In this Research News article, a soft-template-assisted method for the preparation of yolk/silica shell particles is presented. The demonstrated method is simple and general, and can produce hollow silica spheres incorporated with different particles independent of their diameters, geometry, and composition. Furthermore, yolk/mesoporous silica shell particles and multishelled particles are also prepared through optimization of the experimental conditions. Finally, potential applications of these particles are discussed.

Modifying the Hierarchical Porosity of SBA-15 via Mild-Detemplation Followed by Secondary Treatments

NARCIS (Netherlands)

Zhang, Zheng; Melian-Cabrera, Ignacio

2014-01-01

Fenton-chemistry-based detemplation combined with secondary treatments offers options to tune the hierarchical porosity of SBA-15. This approach has been studied on a series of SBA-15 mesophases and has been compared to the conventional calcination. The as-synthesized and detemplated materials were

Microspectroscopic analysis of green fluorescent proteins infiltrated into mesoporous silica nanochannels

NARCIS (Netherlands)

Ma, Yujie; Rajendran, Prayanka; Blum, Christian; Cesa, Yanina; Gartmann, Nando; Brühwiler, Dominik; Subramaniam, Vinod

2011-01-01

The infiltration of enhanced green fluorescent protein (EGFP) into nanochannels of different diameters in mesoporous silica particles was studied in detail by fluorescence microspectroscopy at room temperature. Silica particles from the MCM-41, ASNCs and SBA-15 families possessing nanometer-sized

Utilization of rice husk ash as silica source for the synthesis of mesoporous silicas and their application to CO2 adsorption through TREN/TEPA grafting

International Nuclear Information System (INIS)

Bhagiyalakshmi, Margandan; Yun, Lee Ji; Anuradha, Ramani; Jang, Hyun Tae

2010-01-01

Mesoporous MCM-41, MCM-48 and SBA-15 were synthesized using Rice husk ash (RHA) as the silica source and their defective Si-OH sites were functionalized by 3-cholropropyltrimethoxysilane (CPTMS) which was subsequently grafted with amine compounds, Tris(2-aminoethyl)amine (TREN) and Tetraethylenepentamine (TEPA). X-ray powder diffraction (XRD) and BET results of the parent mesoporous silica suggested their closeness of structural properties to those obtained from conventional silica sources. CO 2 adsorption of branched amine TREN and straight chain amine TEPA at 25, 50 and 75 deg. C was obtained by Thermogravimetric Analyser (TGA) at atmospheric pressure. TREN grafted mesoporous silica showed 7% of CO 2 adsorption while TEPA grafted mesoporous silicas showed less CO 2 adsorption, which is due to the presence of isolated amine groups in TREN. TREN grafted mesoporous silicas were also observed to be selective towards CO 2 , thermally stable and recyclable. The order of CO 2 adsorption with respect to amount of amine grafting was observed to be MCM-48/TREN > MCM-41/TREN > SBA-15/TREN.

Surface functionalization of SBA-15 by the solvent-free method

International Nuclear Information System (INIS)

Wang Yimeng; Zheng Yingwu; Zhu Jianhua

2004-01-01

A solvent-free technique was employed for fast modification of mesoporous materials. Copper, chromium and iron oxide species could be highly dispersed in SBA-15 by manually grinding the corresponding precursor salts and the host, followed by calcinations for the first time. This method is more effective to spontaneously disperse oxide species onto SBA-15 than impregnation, probably forming monolayer or submonolayer dispersion of salts or oxides. Besides, Cr(VI) species dominate in the mixing sample while Cr(III) species dominate in the impregnation one. In the temperature programmed surface reaction of nitrosamines, the sample prepared by solvent-free method showed a higher catalytic activity than the impregnation one

Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnOx/SBA-15.

Science.gov (United States)

Sun, Qiangqiang; Wang, Yu; Li, Laisheng; Bing, Jishuai; Wang, Yingxin; Yan, Huihua

2015-04-09

Comparative experiments were conducted to investigate the catalytic ability of MnO(x)/SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O3/MnO(x)/SBA-15). Adsorption of CA and its intermediates by MnO(x)/SBA-15 was proved unimportant in O3/MnO(x)/SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO3) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO(x)/SBA-15 facilitated the generation of hydroxyl radicals (OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO(x) on SBA-15 were believed to be the main active component in MnO(x)/SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more OH. Copyright © 2014 Elsevier B.V. All rights reserved.

Ordered nanoporous silica as carriers for improved delivery of water insoluble drugs: a comparative study between three dimensional and two dimensional macroporous silica

Directory of Open Access Journals (Sweden)

Wang Y

2013-10-01

Full Text Available Ying Wang, Qinfu Zhao, Yanchen Hu, Lizhang Sun, Ling Bai, Tongying Jiang, Siling WangDepartment of Pharmaceutics, Shenyang Pharmaceutical University, Liaoning Province, People’s Republic of ChinaAbstract: The goal of the present study was to compare the drug release properties and stability of the nanoporous silica with different pore architectures as a matrix for improved delivery of poorly soluble drugs. For this purpose, three dimensional ordered macroporous (3DOM silica with 3D continuous and interconnected macropores of different sizes (200 nm and 500 nm and classic mesoporous silica (ie, Mobil Composition of Matter [MCM]-41 and Santa Barbara Amorphous [SBA]-15 with well-ordered two dimensional (2D cylindrical mesopores were successfully fabricated and then loaded with the model drug indomethacin (IMC via the solvent deposition method. Scanning electron microscopy (SEM, N2 adsorption, differential scanning calorimetry (DSC, and X-ray diffraction (XRD were applied to systematically characterize all IMC-loaded nanoporous silica formulations, evidencing the successful inclusion of IMC into nanopores, the reduced crystallinity, and finally accelerated dissolution of IMC. It was worth mentioning that, in comparison to 2D mesoporous silica, 3DOM silica displayed a more rapid release profile, which may be ascribed to the 3D interconnected pore networks and the highly accessible surface areas. The results obtained from the stability test indicated that the amorphous state of IMC entrapped in the 2D mesoporous silica (SBA-15 and MCM-41 has a better physical stability than in that of 3DOM silica. Moreover, the dissolution rate and stability of IMC loaded in 3DOM silica was closely related to the pore size of macroporous silica. The colorimetric 3-(4,5-Dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide (MTT and Cell Counting Kit (CCK-8 assays in combination with direct morphology observations demonstrated the good biocompatibility of nanoporous

Template preparation of twisted nanoparticles of mesoporous silica

Institute of Scientific and Technical Information of China (English)

Kui Niu; Zhongbin Ni; Chengwu Fu; Tatsuo Kaneko; Mingqing Chen

2011-01-01

Optical isomers of N-lauroyl-L-(or-D-) alanine sodium salt {C12-L-(or-D-)AlaS} surfactants were used for the preparation of mesoporous silica nanoparticles with a twisted hexagonal rod-like morphology. Thermogravimetric analysis (TGA) was used to determine the temperature for template removal. Circular dichroism (CD) spectra of the surfactant solution with various compositions illustrated the formation and supramolecular assembly of protein-like molecular architecture leading to formation of twisted nanoparticles. Scanning electron microscopy (SEM),high-resolution transmission electron microscopy (HRTEM)and X-ray powder diffraction (XRD) patterns of these as-synthesized mesoporous silica confirmed that the twisted morphology of these nanoparticles was closely related to the supramolecular-assembled complex of amino acid surfactants.

Mechanism for enhanced degradation of clofibric acid in aqueous by catalytic ozonation over MnO{sub x}/SBA-15

Energy Technology Data Exchange (ETDEWEB)

Sun, Qiangqiang; Wang, Yu [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China); Li, Laisheng, E-mail: llsh@scnu.edu.cn [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China); Bing, Jishuai [Key Laboratory of Aquatic Science and Technology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); Wang, Yingxin; Yan, Huihua [School of Chemistry & Environment, South China Normal University, Guangzhou 510006 (China)

2015-04-09

Highlights: • Clofibric acid (CA) is efficiently mineralized by O{sub 3}/MnO{sub x}/SBA-15. • Adsorption of CA and its intermediates on MnO{sub x}/SBA-15 is proved unimportant. • Initiation of hydroxyl radicals (·OH) is enhanced in O{sub 3}/MnO{sub x}/SBA-15. • Uniformly distributed MnO{sub x} accounts for the high activity of MnO{sub x}/SBA-15. • Degradation routes of CA in ozonation alone and catalytic ozonation are proposed. - Abstract: Comparative experiments were conducted to investigate the catalytic ability of MnO{sub x}/SBA-15 for the ozonation of clofibric acid (CA) and its reaction mechanism. Compared with ozonation alone, the degradation of CA was barely enhanced, while the removal of TOC was significantly improved by catalytic ozonation (O{sub 3}/MnO{sub x}/SBA-15). Adsorption of CA and its intermediates by MnO{sub x}/SBA-15 was proved unimportant in O{sub 3}/MnO{sub x}/SBA-15 due to the insignificant adsorption of CA and little TOC variation after ceasing ozone in stopped-flow experiment. The more remarkably inhibition effect of sodium bisulfite (NaHSO{sub 3}) on the removal of TOC in catalytic ozonation than in ozonation alone elucidated that MnO{sub x}/SBA-15 facilitated the generation of hydroxyl radicals (·OH), which was further verified by electron spin-resonance spectroscopy (ESR). Highly dispersed MnO{sub x} on SBA-15 were believed to be the main active component in MnO{sub x}/SBA-15. Some intermediates were indentified and different degradation routes of CA were proposed in both ozonation alone and catalytic ozonation. The amounts of small molecular carboxylic acids (i.e., formic acid (FA), acetic acid (AA) and oxalic acid (OA)) generated in catalytic ozonation were lower than in ozonation alone, resulting from the generation of more ·OH.

Thiol-Functionalized Mesoporous Silica for Effective Trap of Mercury in Rats

Directory of Open Access Journals (Sweden)

Wei Zhao

2016-01-01

Full Text Available The chance of exposure to heavy metal for human being rises severely today due to the increasing water contamination and air pollution. Here, we prepared a series of thiol-functionalized mesoporous silica as oral formulation for the prevention and treatment of heavy metal poisoning. The successful incorporation of thiol was verified by the FTIR spectra. SBA15-SH-10 was used for the study as it is of uniform mesopores and fine water dispersibility. In simulated gastrointestinal fluid, the thiol-functionalized mesoporous silica can selectively capture heavy metal, showing a very high affinity for inorganic mercury (II. The blood and urine mercury levels of rats fed with a diet containing Hg (II and material were significantly lower than those of rats fed with the metal-rich diet only. On the contrary, the mercury content in fecal excretion of the treatment group increased more than twice as much as that of the control group. This result indicated that SBA15-SH-10 could effectively remove mercury (II in vivo and the mercury loaded on SBA15-SH-10 would be excreted out. Hence, SBA15-SH-10 has potential application in preventing and treating heavy metal poisoning via digestive system.

Cr(VI) adsorption on functionalized amorphous and mesoporous silica from aqueous and non-aqueous media

International Nuclear Information System (INIS)

Perez-Quintanilla, Damian; Hierro, Isabel del; Fajardo, Mariano; Sierra, Isabel

2007-01-01

A mesoporous silica (SBA-15) and amorphous silica (SG) have been chemically modified with 2-mercaptopyridine using the homogeneous route. This synthetic route involved the reaction of 2-mercaptopyridine with 3-chloropropyltriethoxysilane prior to immobilization on the support. The resulting material has been characterized by powder X-ray diffraction, nitrogen gas sorption, FT-IR and MAS NMR spectroscopy, thermogravimetry and elemental analysis. The solid was employed as a Cr(VI) adsorbent from aqueous and non-aqueous solutions at room temperature. The effect of several variables (stirring time, pH, metal concentration and solvent polarity) has been studied using the batch technique. The results indicate that under the optimum conditions, the maximum adsorption value for Cr(VI) was 1.83 ± 0.03 mmol/g for MP-SBA-15, whereas the adsorption capacity of the MP-SG was 0.86 ± 0.02 mmol/g. On the basis of these results, it can be concluded that it is possible to modify chemically SBA-15 and SG with 2-mercaptopyridine and to use the resulting modified silicas as effective adsorbents for Cr(VI)

Mesoporous silica as carrier of antioxidant for food packaging materials

Science.gov (United States)

Buonocore, Giovanna Giuliana; Gargiulo, Nicola; Verdolotti, Letizia; Liguori, Barbara; Lavorgna, Marino; Caputo, Domenico

2014-05-01

Mesoporous silicas have been long recognized as very promising materials for the preparation of drug delivery systems. In this work SBA-15 mesoporous silica has been functionalized with amino-silane to be used as carrier of antioxidant compound in the preparation of active food packaging materials exhibiting tailored release properties. Active films have been prepared by loading the antioxidant tocopherol, the purely siliceous SBA-15 and the aminofunctionalized SBA-15 loaded with tocopherol into LDPE matrix trough a two-step process (mixing+extrusion). The aim of the present work is the study of the effect of the pore size and of the chemical functionality of the internal walls of the mesophase on the migration of tocopherol from active LDPE polymer films. Moreover, it has been proved that the addition of the active compound do not worsen the properties of the film such as optical characteristic and water vapor permeability, thus leading to the development of a material which could be favorably used mainly, but not exclusively, in the sector of food packaging.

Microstructure and Magnetic Properties of Highly Ordered SBA-15 Nanocomposites Modified with Fe2O3 and Co3O4 Nanoparticles

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P. F. Wang

2012-01-01

Full Text Available Owing to the unique order mesopores, mesoporous SBA-15 could be used as the carrier of the magnetic nanoparticles. The magnetic nanoparticles in the frame and the mesopores lead to the exchange-coupling interaction or other interactions, which could improve the magnetic properties of SBA-15 nanocomposites. Mesoporous Fe/SBA-15 had been prepared via in situ anchoring Fe2O3 into the frame and the micropores of SBA-15 using the sol-gel and hydrothermal processes. Co3O4 nanoparticles had been impregnated into the mesopores of Fe/SBA-15 to form mesoporous Fe/SBA-15-Co3O4 nanocomposites. XRD, HRTEM, VSM, and N2 physisorption isotherms were used to characterize the mesostructure and magnetic properties of the SBA-15 nanocomposites, and all results indicated that the Fe2O3 nanoparticles presented into the frame and micropores, while the Co3O4 nanoparticles existed inside the mesopores of Fe/SBA-15. Furthermore, the magnetic properties of SBA-15 could be conveniently adjusted by the Fe2O3 and Co3O4 magnetic nanoparticles. Fe/SBA-15 exhibited ferromagnetic properties, while the impregnation of Co3O4 nanoparticles greatly improved the coercivity with a value of 1424.6 Oe, which was much higher than that of Fe/SBA-15.

Sulfated zirconia modified SBA-15 catalysts for cellobiose hydrolysis

NARCIS (Netherlands)

Degirmenci, V.; Uner, D.; Cinlar, B.; Shanks, B.H.; Yilmaz, A.; Santen, van R.A.; Hensen, E.J.M.

2011-01-01

Zirconia modified SBA-15 becomes a very active catalyst for the selective hydrolysis of cellobiose to glucose after sulfation. Spectroscopic investigations indicate the presence of Brønsted acid sites with similar properties to those present in conventional sulfated zirconia. Indications are found

Facile functionalized of SBA-15 via a biomimetic coating and its application in efficient removal of uranium ions from aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Gao, Jun-Kai [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China); School of Energy and Environmental Engineering, Hebei University of Technology, Tianjin 300401 (China); Hou, Li-An; Zhang, Guang-Hui [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China); Gu, Ping, E-mail: guping@tju.edu.cn [School of Environmental Science and Engineering, Tianjin University, Tianjin 300072 (China)

2015-04-09

Highlights: • Dopamine-functionalized SBA-15 (DMS) was developed via a biomimetic coating. • The modification approach was simple, facile and cost-effective. • The DMS was firstly used to remove U(VI) from aqueous solution. • Large adsorption capacity and rapid separation were obtained. - Abstract: A novel dopamine-functionalized mesoporous silica (DMS), synthesized by grafting dopamine onto a mesoporous molecular sieve (SBA-15), was developed as a sorbent to extract U(VI) from aqueous solution. The method used to modify SBA-15 was simple, facile and cost-effective. The DMS was characterized by SEM, TEM, XRD and BET, showing that the material had an ordered mesoporous structure and a large surface area. The effect of contact time, pH, ionic strength, temperature, and solid–liquid ratio on the sorption process was investigated. It was demonstrated that the adsorption of U(VI) by DMS was fast and that it can be described by the pseudo-second order-equation where the equilibrium time was 20 min. Additionally, the adsorption isotherm data were fitted well by the Langmuir model with the maximum adsorption capacity of DMS of 196 mg/g at pH 6.0. Furthermore, the influence of the K{sup +} and Na{sup +} concentrations and solid-to-liquid ratio on the sorption was very weak, and the values of the thermodynamic parameters revealed that the sorption process was exothermic and spontaneous. All the results suggested that the DMS could be used as an excellent adsorbent to remove U(VI) from aqueous solution.

Microwave radiation hydrothermal synthesis and characterization of micro- and mesoporous composite molecular sieve Y/SBA-15

Directory of Open Access Journals (Sweden)

Wenyuan Wu

2017-05-01

Full Text Available A microwave radiation hydrothermal method to control synthesis of micro- and mesoporous Y/SBA-15 composite molecular sieves was reported. The synthesized SBA-15 and Y/SBA-15 were characterized by scanning electron microscopy (SEM and N2 adsorption–desorption. The three kinds of different concentrations of hydrochloric acid (0.75 M, 2 M and 3.25 M were used to investigate the effect on Y/SBA-15. The analysis results of the composite products indicated that the optimization synthesis condition employed zeolite type Y and TEOS as silicon sources under 0.75 M hydrochloric acid by the microwave radiation hydrothermal synthesis method. The N2 adsorption–desorption test results of micro–mesoporous composite molecular sieve type Y/SBA-15 in mesoporous extent indicated that SBET is 355.529 m2/g, D‾BET is 4.050 nm, and mesoporous aperture focuses on the distribution region of 5.3 nm. It was found that the received composite product has an appropriate proportion of smaller size, larger size pore structure and the thicker pore wall. In addition, its internal channels have a high degree of order and smooth flow in long-range channels.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

OpenAIRE

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-01-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hol...

Direct esterification of olive-pomace oil using mesoporous silica supported sulfonic acids

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F. Alrouh

2017-02-01

Full Text Available Mesoporous silica MCM-41 and SBA-15 containing propyl sulfonic acid groups were synthesized according to the literature and were characterized by X-ray diffraction, N2 adsorption and the H+ exchange capacities of the sulfonic acid groups were titrated. The esterification reaction of glycerol with olive-pomace oil has been carried out by using prepared functionalized mesoporous silica (MCM-41 and SBA-15 as catalysts. It has been monitored by GC two fatty acids (palmitic and oleic acids as reactants in olive-pomace oil and their related monoacylglycerols (Glycerol monopalmitate GMP and monooleate GMO as reaction product. The catalytic activities of the functionalized mesoporous silica were compared with commercial catalysts, these included homogeneous catalysts (p-toluenesulfonic acid and heterogeneous catalysts (Amberlyst-15. The total yield of monoacylglycerols (GMO + GMP was nearly 40%. Remarkably, we found that MCM-41-SO3H was recycled at least 3 times without any loss of activity.

Monodisperse metal nanoparticle catalysts on silica mesoporous supports: synthesis, characterizations, and catalytic reactions

Energy Technology Data Exchange (ETDEWEB)

Somorjai, G.A.

2009-09-14

The design of high performance catalyst achieving near 100% product selectivity at maximum activity is one of the most important goals in the modern catalytic science research. To this end, the preparation of model catalysts whose catalytic performances can be predicted in a systematic and rational manner is of significant importance, which thereby allows understanding of the molecular ingredients affecting the catalytic performances. We have designed novel 3-dimensional (3D) high surface area model catalysts by the integration of colloidal metal nanoparticles and mesoporous silica supports. Monodisperse colloidal metal NPs with controllable size and shape were synthesized using dendrimers, polymers, or surfactants as the surface stabilizers. The size of Pt, and Rh nanoparticles can be varied from sub 1 nm to 15 nm, while the shape of Pt can be controlled to cube, cuboctahedron, and octahedron. The 3D model catalysts were generated by the incorporation of metal nanoparticles into the pores of mesoporous silica supports via two methods: capillary inclusion (CI) and nanoparticle encapsulation (NE). The former method relies on the sonication-induced inclusion of metal nanoparticles into the pores of mesoporous silica, whereas the latter is performed by the encapsulation of metal nanoparticles during the hydrothermal synthesis of mesoporous silica. The 3D model catalysts were comprehensively characterized by a variety of physical and chemical methods. These catalysts were found to show structure sensitivity in hydrocarbon conversion reactions. The Pt NPs supported on mesoporous SBA-15 silica (Pt/SBA-15) displayed significant particle size sensitivity in ethane hydrogenolysis over the size range of 1-7 nm. The Pt/SBA-15 catalysts also exhibited particle size dependent product selectivity in cyclohexene hydrogenation, crotonaldehyde hydrogenation, and pyrrole hydrogenation. The Rh loaded SBA-15 silica catalyst showed structure sensitivity in CO oxidation reaction. In

Influence of the preparation method on the morphology of templated NiCo{sub 2}O{sub 4} spinel

Energy Technology Data Exchange (ETDEWEB)

Cabo, Moises; Pellicer, Eva, E-mail: eva.pellicer.icn@uab.cat; Rossinyol, Emma; Solsona, Pau [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain); Castell, Onofre [Universitat Autonoma de Barcelona, Servei de Microscopia, Facultat de Ciencies (Spain); Surinach, Santiago; Baro, Maria Dolors [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain)

2011-09-15

The synthesis of NiCo{sub 2}O{sub 4} spinel by several nanocasting strategies (i.e., multi-step nanocasting, one-step nanocasting and soft-templating), in which nickel and cobalt nitrates are used as precursors and Pluronic P123 as surfactant, is explored. First, in the multi-step nanocasting, the effect of the impregnation method (evaporation, solid-liquid and two-solvent) of the SBA-15 silica template on the morphology of NiCo{sub 2}O{sub 4} replica is investigated. The evaporation method seems to be the best choice to obtain mesoporous NiCo{sub 2}O{sub 4} powder which, after calcination at 375 Degree-Sign C and subsequent template removal, displays the highest surface area (93.1 m{sup 2}/g). We have also checked the feasibility of the one-step nanoscating approach for the synthesis of ordered NiCo{sub 2}O{sub 4} arrays, though this methodology entails severe difficulties, mainly related to the different decomposition temperature of the nitrate precursors and the P123 surfactant. Finally, randomly oriented, aggregated NiCo{sub 2}O{sub 4} nanoparticles are obtained by means of P123 surfactant-assisted soft-templating approach.

Evidence for metalsupport interactions in Au modified TiO_{x}/SBA-15 materials prepared by photodeposition

OpenAIRE

Mei, Bastian; Wiktor, Christian; Turner, Stuart; Pougin, Anna; Tendeloo, Van, Gustaaf; Fischer, Roland A.; Muhler, Martin; Strunk, Jennifer

2013-01-01

Abstract: Gold nanoparticles have been efficiently photodeposited onto titanate-loaded SBA-15 (Ti(x)/SBA-15) with different titania coordination. Transmission electron microscopy shows that relatively large Au nanoparticles are photodeposited on the outer surface of the Ti(x)/SBA-15 materials and that TiOx tends to form agglomerates in close proximity to the Au nanoparticles, often forming coreshell Au/TiOx structures. This behavior resembles typical processes observed due to strong-metal sup...

Substantially Stabilized Superacid Incorporated SBA-15 with Calcium Bridging for Selective Esterification of Glycerol

Science.gov (United States)

Hoo, P. Y.; Abdullah, A. Z.; Shuit, S. H.; Teoh, Y. P.; Ng, Q. H.; Kunasundari, B.

2018-03-01

The exploitation of the super acidity of heteropolyacids incorporated heterogeneous catalysts was only feasible if the heterogeneity of these catalysts was assured. To maintain the catalyst heterogeneity in polar medium, a novel two-step modification method was proposed to synthesize the highly active, yet stable heterogeneous catalyst, catered for selective esterification of monoglyceride. The surficial, structural and acidity properties of the modified catalysts were investigated via crucial characterization methods (N2 BET, HRTEM, and FTIR). The collective evidences verified the predicted formation of calcium oxides (CaO) on the mesopores surfaces of the SBA-15 support after the first modification, and the successful subsequent 12-tungstophosphoric acid (HPW) functionalization. The superior stability of the synthesized catalysts (10wt%-HPW/CaSBA-15) was demonstrated (negligible change in both conversion – 75% and yield – 70%), without the need for catalyst regeneration. Such result was attributed to the strong interaction between HPW and SBA-15 via calcium bridging. Being alkaline in nature, calcium oxides in the inner pores readily reacted with highly acidic HPW introduced in the subsequent wetness incipient step, forming insoluble HPW acid sites on inner pore walls of SBA-15 via the calcium bridging. This modification deemed promising and other alkaline metals should be explored in the future.

Polymeric carbon nitride/mesoporous silica composites as catalyst support for Au and Pt nanoparticles.

Science.gov (United States)

Xiao, Ping; Zhao, Yanxi; Wang, Tao; Zhan, Yingying; Wang, Huihu; Li, Jinlin; Thomas, Arne; Zhu, Junjiang

2014-03-03

Small and homogeneously dispersed Au and Pt nanoparticles (NPs) were prepared on polymeric carbon nitride (CNx )/mesoporous silica (SBA-15) composites, which were synthesized by thermal polycondensation of dicyandiamide-impregnated preformed SBA-15. By changing the condensation temperature, the degree of condensation and the loading of CNx can be controlled to give adjustable particle sizes of the Pt and Au NPs subsequently formed on the composites. In contrast to the pure SBA-15 support, coating of SBA-15 with polymeric CNx resulted in much smaller and better-dispersed metal NPs. Furthermore, under catalytic conditions the CNx coating helps to stabilize the metal NPs. However, metal NPs on CNx /SBA-15 can show very different catalytic behaviors in, for example, the CO oxidation reaction. Whereas the Pt NPs already show full CO conversion at 160 °C, the catalytic activity of Au NPs seems to be inhibited by the CNx support. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of nano grade hollow silica sphere via a soft template method.

Science.gov (United States)

Tsai, Ming-Shyong; Li, Miao Ju; Yen, Fu-Hsu

2008-06-01

The nano grade hollow silica sphere (HSS) was synthesized by a novel soft template method. We found that the precipitate of aluminate had a porous structure that could be the soft template for HSS. After mixing the colloidal silica with the aluminate precipitate, the bubble trapped in this porous structure could form the nano grade HSS. The aluminate precipitate was removed by adjusting the pH of the slurry to approximately 1. The outside diameter, the specific surface, and the mean pore size diameter of the forming HSS were 60-90 nm, 571 m2/g, and 3 nm, respectively. The formed HSS was collected by modifying the surface with Si(OCH3)3CHCH2 (VTMO) and then filtrating the precipitated gel in the n-butanol and ethanol solvent system.

Efficient low-temperature soot combustion by bimetallic Ag-Cu/SBA-15 catalysts.

Science.gov (United States)

Wen, Zhaojun; Duan, Xinping; Hu, Menglin; Cao, Yanning; Ye, Linmin; Jiang, Lilong; Yuan, Youzhu

2018-02-01

In this study, the effects of copper (Cu) additive on the catalytic performance of Ag/SBA-15 in complete soot combustion were investigated. The soot combustion performance of bimetallic Ag-Cu/SBA-15 catalysts was higher than that of monometallic Ag and Cu catalysts. The optimum catalytic performance was acquired with the 5Ag 1 -Cu 0.1 /SBA-15 catalyst, on which the soot combustion starts at T ig =225°C with a T 50 =285°C. The temperature for 50% of soot combustion was lower than that of conventional Ag-based catalysts to more than 50°C (Aneggi et al., 2009). Physicochemical characterizations of the catalysts indicated that addition of Cu into Ag could form smaller bimetallic Ag-Cu nanolloy particles, downsizing the mean particle size from 3.7nm in monometallic catalyst to 2.6nm in bimetallic Ag-Cu catalyst. Further experiments revealed that Ag and Cu species elicited synergistic effects, subsequently increasing the content of surface active oxygen species. As a result, the structure modifications of Ag by the addition of Cu strongly intensified the catalytic performance. Copyright © 2017. Published by Elsevier B.V.

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

Science.gov (United States)

Yang, Jae Hwan; Park, Hwan Seo; Ahn, Do-Hee; Yim, Man-Sung

2016-11-01

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi2O3 (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi2O3 and the glass composition. It was confirmed that BiI3, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi5O7I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10-3-10-2 g/m2 day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of 129I.

H2 formation by electron irradiation of SBA-15 materials and the effect of Cu(II) grafting

International Nuclear Information System (INIS)

Brodie-Linder, N.; Le Caer, S.; Shahdo Alam, M.; Renault, J.P.; Alba-Simionesco, Ch.

2010-01-01

Measurement of H 2 production from electron irradiation (10 MeV) on SBA-15 materials has shown that adsorbed water is attacked preferentially. Silanol groups are only attacked when they are in the majority with respect to adsorbed water, however they are much less efficient at producing H 2 . The comparison between water content before and after electron irradiation and the corresponding H 2 production indicates that water desorption is the main route to adsorbed water loss for SBA-15 materials. On the other hand, surface silanol groups are more susceptible to attack,leading to H 2 production when SBA-15 samples have undergone extensive thermal treatment. Electron irradiation of SBA-15-Cu materials has shown that the presence of Cu(II) on the surface reduces and inhibits the production of H 2 . This inhibiting power affects adsorbed water bonded to grafted copper but not surface silanol groups. (authors)

The retained templates as "helpers" for the spherical meso-silica in adsorption of heavy metals and impacts of solution chemistry.

Science.gov (United States)

Liang, Zhijie; Shi, Wenxin; Zhao, Zhiwei; Sun, Tianyi; Cui, Fuyi

2017-06-15

The spherical mesoporous silica (meso-silica) MCM-41 and those with different dosage of the retained templates were prepared and characterized. Particularly, effects of the retained template and its dosage on the adsorption of typical heavy metals (Cu 2+ and Cd 2+ ) in the synthesized materials were investigated. The results indicated that the retained templates acted as "helpers" for the adsorption of Cu 2+ and Cd 2+ in the spherical meso-silica MCM-41, and the maximum adsorption capacities (Q max ) increased with the increase of the retained template dosage. The interaction between the metal ions and the cationic heads of the templates contributed to the enhancement effect due to the anions (Cl - and OH - ) electronically adsorbed on the interface of the template micelles. Additionally, the presented results indicated that the adsorption of Cu 2+ and Cd 2+ depended on pH and high ion strength of the solution but not on the coexisted humic acid. Copyright © 2017 Elsevier Inc. All rights reserved.

Comparative Study of Molecular Basket Sorbents Consisting of Polyallylamine and Polyethylenimine Functionalized SBA-15 for CO2 Capture from Flue Gas.

Science.gov (United States)

Wang, Dongxiang; Wang, Xiaoxing; Song, Chunshan

2017-11-17

Polyallylamine (PAA)-based molecular basket sorbents (MBS) have been studied for CO 2 capture in comparison with polyethylenimine (PEI)-based MBS. The characterizations including N 2 physisorption, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and thermogravimetric analysis (TGA) showed that PAA (M n =15 000) is more rigid and has more steric hindrance inside SBA-15 pores than PEI owing mainly to its different polymer structure. The effects of temperature and PAA loading on the CO 2 sorption capacity of PAA-based MBS have been examined by TGA by using 100 % CO 2 gas stream and compared with PEI/SBA-15. It was found that the capacity of the PAA/SBA-15 sorbent increased with increasing temperature. The optimum capacity of 88 mg CO2  g sorb -1 was obtained at 140 °C for PAA(50)/SBA-15 whereas the optimum sorption temperature was 75 and 90 °C for PEI-I(50)/SBA-15 (PEI-I, M n =423) and PEI-II(50)/SBA-15 (PEI-II, M n =25 000), respectively. The capacity initially increased with the increase of PAA loading and then dropped at high amine contents, owing to the increased diffusion barrier. The highest CO 2 capacity of 109 mg CO2  g sorb -1 was obtained at a PAA loading of 65 wt %, whereas the PAA(50)/SBA-15 sorbent gave the best amine efficiency of 0.23 mol CO2  mol N -1 . The effect of moisture was examined in a fixed-bed flow system with simulated flue gas containing 15 % CO 2 and 4.5 % O 2 in N 2 . It was found that the presence of moisture significantly enhanced CO 2 sorption over PAA(50)/SBA-15 and greatly improved its cyclic stability and regenerability. Compared with PEI/SBA-15, PAA/SBA-15 possesses a better thermal stability and higher resistance to oxidative degradation. However, the CO 2 sorption rate over the PAA(50)/SBA-15 sorbent was much slower. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Production of Ethylene through Ethanol Dehydration on SBA-15 Catalysts Synthesized by Sol-gel and One-step Hydrothermal Methods.

Science.gov (United States)

Autthanit, Chaowat; Jongsomjit, Bunjerd

2018-02-01

The present work deals with the catalytic performance of SBA-15 supported catalysts in the gas phase catalytic dehydration of ethanol in the temperature range of 200 to 400°C. The SBA-15 support was incorporated on a zirconium (Zr) and bimetal of zirconium and lanthanum (Zr-La) prepared by sol-gel (SG) and hydrothermal (HT) methods. The catalysts were characterized by means of N 2 physisorption, SEM/EDX, and NH 3 -TPD. The experimental results demonstrated that the Zr-La/SBA-15-HT exhibited the highest catalytic activity. Ethanol conversion and ethylene selectivity were found to increase with increased reaction temperature. The best catalytic results were achieved for Zr-La/SBA-15-HT indicating values of ethanol conversion and ethylene yield of ca. 84% and 80%, respectively at 400°C. The most important parameter influencing their catalytic properties appears to be the interaction between metal and support depending on different methods. The metal dispersion inside the siliceous matrix of SBA-15 has a direct influence on their surface acidity. Meanwhile, the performance of these SBA-15 supported catalysts in ethanol dehydration is also related with the alteration of surface acidity caused by the introduction of Zr and Zr-La.

Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

International Nuclear Information System (INIS)

Erko, M; Paris, O; Wallacher, D; Findenegg, G H

2012-01-01

The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

Mesoporous silica particles modified with graphitic carbon: interaction with human red blood cells and plasma proteins

Energy Technology Data Exchange (ETDEWEB)

Martinez, Diego Stefani Teodoro; Franqui, Lidiane Silva; Bettini, Jefferson; Strauss, Mathias, E-mail: diego.martinez@lnnano.cnpem.br [Centro Nacional de Pesquisa em Energia e Materiais (CNPEM), Campinas, SP (Brazil); Damasceno, Joao Paulo Vita; Mazali, Italo Odone [Universidade Estadual de Campinas (UNICAMP), SP (Brazil)

2016-07-01

Full text: In this work the interaction of the mesoporous silica particles (SBA-15, ∼700 nm) modified with graphitic carbon (SBA-15/C) on human red blood cells (hemolysis) and plasma proteins (protein corona formation) is studied. XPS and CHN analysis showed that the carbon content on the SBA-15/C samples varied from 2 to 10% and was tuned by the functionalization step. The formed carbon structures where associated to graphitic nanodomains coating the pores surface as verified by Raman spectroscopy and {sup 13}C NMR. Advanced TEM/EELS analysis showed that the carbon structures are distributed along the SBA-15 mesopores. SAXS and textural analyses were used to confirm that the porous structure of the silica support is kept after the modification procedure and to calculate the number of graphitic carbon stacked layers coating the mesopores. After incubation of SBA-15 with human red blood cells (RBCs), it was observed a dose-dependent hemolytic effect, probably, due to binding of the material silanol-rich surface to the phosphatidylcholine molecules from the RBC membrane. The graphitic carbon modifications have mitigated this effect, indicating that the graphitic carbon coating protected the silanol groups of the particle surface hindering the hemolysis. Considering the protein corona formation, selective biomolecular interaction of proteins was observed for the different materials using gel electrophoresis (SDS-PAGE) analysis. Besides, graphitic carbon modification decreased the amount of proteins on the corona. Together, the in vitro hemolysis and protein corona assays are promising biological models to understand the influence of silica surface functionalization on their bionano-interactions. Finally, our work contributes to the development of fundamental research on such nanomaterials chemistry in the emerging field of nanobioscience and nanotoxicology. (author)

Applying Mesoporous Silica SBA-15 in Electrochemical Detection of DNA Hybridization

Czech Academy of Sciences Publication Activity Database

Josypčuk, Oksana; Fojta, Miroslav; Daňhel, Aleš; Josypčuk, Bohdan

2016-01-01

Roč. 28, č. 8 (2016), s. 1860-1864 ISSN 1040-0397 R&D Projects: GA ČR GAP206/11/1638 Institutional support: RVO:68081707 ; RVO:61388955 Keywords : voltammetry * sensor DNA hybridization * mesoporous silica Subject RIV: CG - Electrochemistry Impact factor: 2.851, year: 2016

Catalytic silica particles via template-directed molecular imprinting

Energy Technology Data Exchange (ETDEWEB)

Markowitz, M.A.; Kust, P.R.; Deng, G.; Schoen, P.E.; Dordick, J.S.; Clark, D.S.; Gaber, B.P.

2000-02-22

The surfaces of silica particle were molecularly imprinted with an {alpha}-chymotrypsin transition-state analogue (TSA) by utilizing the technique of template-directed synthesis of mineralized materials. The resulting catalytic particles hydrolyzed amides in an enantioselective manner. A mixture of a nonionic surfactant and the acylated chymotrysin TSA, with the TSA acting as the headgroup at the surfactant-water interface, was used to form a microemulsion for silica particle formation. Incorporation of amine-, dihydroimidazole-, and carboxylate-terminated trialkoxysilanes into the particles during imprinting resulted in enhancement of the rates of amide hydrolysis. Acylated imprint molecules formed more effective imprints in the presence of the functionalized silanes than nonacylated imprint molecules. Particles surface-imprinted with the chymotrypsin TSA were selective for the trypsin substrate, and particles surface-imprinted with the L-isomer of the enzyme TSA were enantioselective for the D-isomer of the substrate.

Grafting of alumina on SBA-15: Effect of surface roughness

Czech Academy of Sciences Publication Activity Database

Zukal, Arnošt; Šiklová, Helena; Čejka, Jiří

2008-01-01

Roč. 24, č. 17 (2008), s. 9837-9842 ISSN 0743-7463 R&D Projects: GA AV ČR KAN100400701 Institutional research plan: CEZ:AV0Z40400503 Keywords : alumina-grafted materials * SBA-15 * Nitrogen adsorption Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.097, year: 2008

The enhancement of photoresponse of an ordered inorganic-organic hybrid architecture by increasing interfacial contacts

International Nuclear Information System (INIS)

Zhang Bin; Chen Xudong; Ma Shaohua; Yang Jin; Zhang Mingqiu; Chen Yujie

2010-01-01

A modified ZnO quantum dot/polythiophene (ZnO/PTh) inorganic-organic hybrid architecture was fabricated by using ordered mesoporous silica (SBA-15) as the retaining template. First, a two-step strategy was developed to synthesize an ordered organic conducting polymer composite (PTh/SBA-15). Then, ZnO quantum dots were in situ formed on the pore walls of the ordered PTh/SBA-15 composite. Photoresponse of the inorganic-organic hybrid was studied with respect to its incident photon to collected electron conversion efficiency (IPCE) and morphology. The presence of SBA-15 proved to be critical for controlling the interfacial morphology and hence enlarging the interfacial area of the inorganic-organic heterojunction. The proposed approach may act as a key method to open up potential applications in photovoltaic devices.

The enhancement of photoresponse of an ordered inorganic-organic hybrid architecture by increasing interfacial contacts.

Science.gov (United States)

Zhang, Bin; Chen, Xudong; Ma, Shaohua; Chen, Yujie; Yang, Jin; Zhang, Mingqiu

2010-02-10

A modified ZnO quantum dot/polythiophene (ZnO/PTh) inorganic-organic hybrid architecture was fabricated by using ordered mesoporous silica (SBA-15) as the retaining template. First, a two-step strategy was developed to synthesize an ordered organic conducting polymer composite (PTh/SBA-15). Then, ZnO quantum dots were in situ formed on the pore walls of the ordered PTh/SBA-15 composite. Photoresponse of the inorganic-organic hybrid was studied with respect to its incident photon to collected electron conversion efficiency (IPCE) and morphology. The presence of SBA-15 proved to be critical for controlling the interfacial morphology and hence enlarging the interfacial area of the inorganic-organic heterojunction. The proposed approach may act as a key method to open up potential applications in photovoltaic devices.

Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

KAUST Repository

Bendjeriou-Sedjerari, Anissa

2016-08-11

Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

Facile functionalized of SBA-15 via a biomimetic coating and its application in efficient removal of uranium ions from aqueous solution.

Science.gov (United States)

Gao, Jun-Kai; Hou, Li-An; Zhang, Guang-Hui; Gu, Ping

2015-04-09

A novel dopamine-functionalized mesoporous silica (DMS), synthesized by grafting dopamine onto a mesoporous molecular sieve (SBA-15), was developed as a sorbent to extract U(VI) from aqueous solution. The method used to modify SBA-15 was simple, facile and cost-effective. The DMS was characterized by SEM, TEM, XRD and BET, showing that the material had an ordered mesoporous structure and a large surface area. The effect of contact time, pH, ionic strength, temperature, and solid-liquid ratio on the sorption process was investigated. It was demonstrated that the adsorption of U(VI) by DMS was fast and that it can be described by the pseudo-second order-equation where the equilibrium time was 20 min. Additionally, the adsorption isotherm data were fitted well by the Langmuir model with the maximum adsorption capacity of DMS of 196 mg/g at pH 6.0. Furthermore, the influence of the K(+) and Na(+) concentrations and solid-to-liquid ratio on the sorption was very weak, and the values of the thermodynamic parameters revealed that the sorption process was exothermic and spontaneous. All the results suggested that the DMS could be used as an excellent adsorbent to remove U(VI) from aqueous solution. Copyright © 2014 Elsevier B.V. All rights reserved.

Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

KAUST Repository

Bendjeriou-Sedjerari, Anissa; Sofack-Kreutzer, Julien; Minenkov, Yury; Abou-Hamad, Edy; Hamzaoui, Bilel; Werghi, Baraa; Anjum, Dalaver H.; Cavallo, Luigi; Huang, Kuo-Wei; Basset, Jean-Marie

2016-01-01

Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

Iron oxide inside SBA-15 modified with amino groups as reusable adsorbent for highly efficient removal of glyphosate from water

Science.gov (United States)

Fiorilli, Sonia; Rivoira, Luca; Calì, Giada; Appendini, Marta; Bruzzoniti, Maria Concetta; Coïsson, Marco; Onida, Barbara

2017-07-01

Iron oxide clusters were incorporated into amino-functionalized SBA-15 in order to obtain a magnetically recoverable adsorbent. The physical-chemical properties of the material were characterized by FE-SEM, STEM, XRD, TGA, XPS, FT-IR and acid-base titration analysis. Iron oxide nanoparticles were uniformly dispersed into the pore of mesoporous silica and that the adsorbent is characterized high specific surface area (177 m2/g) and accessible porosity. The sorbent was successfully tested for the removal of glyphosate in real water matrices. Despite the significant content of inorganic ions, a quantitative removal of the contaminant was found. The complete regeneration of the sorbent after the adsorption process through diluted NaOH solution was also proved.

A highly sensitive electrochemical sensor for the determination of methanol based on PdNPs@SBA-15-PrEn modified electrode.

Science.gov (United States)

Karimi, Ziba; Shamsipur, Mojtaba; Tabrizi, Mahmoud Amouzadeh; Rostamnia, Sadegh

2018-05-01

In this study, a novel electrochemical sensor for the determination of methanol based on palladium nanoparticles supported on Santa barbara amorphous-15- PrNHEtNH 2 (PdNPs@SBA-15-PrEn) as nanocatalysis platform is presented. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electrochemical methods are employed to characterize the PdNPs@SBA-15-PrEn nanocomposite. The Nafion-Pd@SBA-15-PrEn modified glassy carbon electrode (Nafion-PdNPs@SBA-15-PrEn/GCE) displayed the high electrochemical activity and excellent catalytic characteristic for electro-oxidation of methanol in an alkaline solution. The electro-oxidation performance of the proposed sensor was investigated using cyclic voltammetry (CV) and amperometry. The sensor exhibits a good sensitivity of 0.0905 Amol -1 Lcm -2 , linear range of 20-1000 μM and the corresponding detection limit of 12 μM (3σ). The results demonstrate that the Nafion-PdNPs@SBA-15-PrEn/GCE has potential as an efficient and integrated sensor for methanol detection. Copyright © 2018 Elsevier Inc. All rights reserved.

Silicon oxynitrides of KCC-1, SBA-15 and MCM-41 for CO 2 capture with excellent stability and regenerability

KAUST Repository

Patil, Umesh

2012-01-01

We report the use of silicon oxynitrides as novel adsorbents for CO 2 capture. Three series of functionalized materials based on KCC-1, SBA-15 and MCM-41 with Si-NH 2 groups were prepared using a simple one-step process via thermal ammonolysis using ammonia gas, and they demonstrated excellent CO 2 capture capabilities. These materials overcome several limitations of conventional amine-grafted mesoporous silica. They offer good CO 2 capture capacity, faster adsorption-desorption kinetics, efficient regeneration and reuse, more crucially excellent thermal and mechanical stability even in oxidative environments, and a clean and green synthesis route, which allows the overall CO 2 capture process to be practical and sustainable. This journal is © The Royal Society of Chemistry 2012.

Mesoporous Silica-Supported Sulfonyldiamine Ligand for Microwave-Assisted Transfer Hydrogenation

Directory of Open Access Journals (Sweden)

Shaheen M. Sarkar

2015-01-01

Full Text Available N-Sulfonyl-1,2-diamine ligands, derived from 1,2-diaminocyclohexane and 1,2-diaminopropane, were immobilized onto mesoporous SBA-15 silica. The SBA-15-supported sulfonyldiamine-Ru complex was prepared in situ under microwave heating at 60 W for 3 min. The prepared sulfonyldiamine-Ru complex was used as an efficient catalyst for the transfer hydrogenation of ketones to the corresponding secondary alcohols. The heterogeneous complex showed extremely high catalytic activity with 99% conversion rate under microwave heating condition. The complexes were regenerated by simple filtration and reused two times without significant loss of activity.

A novel, efficient and facile method for the template removal from mesoporous materials

KAUST Repository

Chen, Lu; Jiang, Shang; Wang, Runwei; Zhang, Zongtao; Qiu, Shilun

2014-01-01

© 2014, Jilin University, The Editorial Department of Chemical Research in Chinese Universities and Springer-Verlag GmbH. A new catalytic-oxidation method was adopted to remove the templates from SBA-15 and MCM-41 mesoporous materials via Fenton

Dual soft-template system based on colloidal chemistry for the synthesis of hollow mesoporous silica nanoparticles.

Science.gov (United States)

Li, Yunqi; Bastakoti, Bishnu Prasad; Imura, Masataka; Tang, Jing; Aldalbahi, Ali; Torad, Nagy L; Yamauchi, Yusuke

2015-04-20

A new dual soft-template system comprising the asymmetric triblock copolymer poly(styrene-b-2-vinyl pyridine-b-ethylene oxide) (PS-b-P2VP-b-PEO) and the cationic surfactant cetyltrimethylammonium bromide (CTAB) is used to synthesize hollow mesoporous silica (HMS) nanoparticles with a center void of around 17 nm. The stable PS-b-P2VP-b-PEO polymeric micelle serves as a template to form the hollow interior, while the CTAB surfactant serves as a template to form mesopores in the shells. The P2VP blocks on the polymeric micelles can interact with positively charged CTA(+) ions via negatively charged hydrolyzed silica species. Thus, dual soft-templates clearly have different roles for the preparation of the HMS nanoparticles. Interestingly, the thicknesses of the mesoporous shell are tunable by varying the amounts of TEOS and CTAB. This study provides new insight on the preparation of mesoporous materials based on colloidal chemistry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Templated Control of Au nanospheres in Silica Nanowires

Energy Technology Data Exchange (ETDEWEB)

Tringe, J W; Vanamu, G; Zaidi, S H

2007-03-15

The formation of regularly-spaced metal nanostructures in selectively-placed insulating nanowires is an important step toward realization of a wide range of nano-scale electronic and opto-electronic devices. Here we report templated synthesis of Au nanospheres embedded in silica nanowires, with nanospheres consistently spaced with a period equal to three times their diameter. Under appropriate conditions, nanowires form exclusively on Si nanostructures because of enhanced local oxidation and reduced melting temperatures relative to templates with larger dimensions. We explain the spacing of the nanospheres with a general model based on a vapor-liquid-solid mechanism, in which an Au/Si alloy dendrite remains liquid in the nanotube until a critical Si concentration is achieved locally by silicon oxide-generated nanowire growth. Additional Si oxidation then locally reduces the surface energy of the Au-rich alloy by creating a new surface with minimum area inside of the nanotube. The isolated liquid domain subsequently evolves to become an Au nanosphere, and the process is repeated.

A novel visible light-driven Ag3PO4/SBA-15 nanocomposite: Preparation and application in the photo-degradation of pollutants

International Nuclear Information System (INIS)

Chai, Yuanyuan; Wang, Li; Ren, Jia; Dai, Wei-Lin

2015-01-01

Graphical abstract: - Highlights: • Highly efficient visible-light-driven Ag 3 PO 4 /SBA-15 nanocomposite. • Application in the photo-degradation of RhB. • Synthesis from a facile and simple colloidal method. • 20%-Ag 3 PO 4 /SBA-15 shows 8 times faster degradation rate than Ag 3 PO 4 . • Super stability and recycling ability. - Abstract: A novel visible light-driven environmental-benign Ag 3 PO 4 /SBA-15 nanocomposite photo-catalyst was synthesized for the photo-degradation of pollutants. The exploration on adsorption and photo-catalysis of dye or organic pollution for the nanocomposite was carried out. The adsorption capability for Ag 3 PO 4 /SBA-15 nanocomposite increases by 3 times compared with that of the Ag 3 PO 4 particles. The photo-catalytic activity of nanocomposite is higher than pristine Ag 3 PO 4 nanoparticle for the degradation of RhB or MO under visible light irradiation (λ > 420 nm). The effect of Ag 3 PO 4 loading on the catalytic performance was also studied. The results show that the optimum degradation is achieved over 20% Ag 3 PO 4 /SBA-15. Compared to pure Ag 3 PO 4 nanoparticle, the most efficient catalyst showed 8 times higher photo-catalytic activity for the degradation of RhB. The Ag 3 PO 4 /SBA-15 catalysts were systematically characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–Vis diffuse reflectance spectroscopy (DRS), and N 2 -adsorption–desorption isotherms (BET). A possible mechanism scheme regarding photo-degradation enhancement induced by dye enrichments has been proposed on the Ag 3 PO 4 /SBA-15 nanocomposite. Additionally, the SBA-15 support can enhance the efficiency of separation of catalyst from the reaction mixture, implying that the Ag 3 PO 4 loading on the SBA-15 catalyst will not result in the extra environment and health problems and reduce the cost of wastewater treatment

Immobilization of HRP in Mesoporous Silica and Its Application for the Construction of Polyaniline Modified Hydrogen Peroxide Biosensor

Directory of Open Access Journals (Sweden)

Chien-Chung Chen

2009-06-01

Full Text Available Polyaniline (PANI, an attractive conductive polymer, has been successfully applied in fabricating various types of enzyme-based biosensors. In this study, we have employed mesoporous silica SBA-15 to stably entrap horseradish peroxidase (HRP, and then deposited the loaded SBA-15 on the PANI modified platinum electrode to construct a GA/SBA-15(HRP/PANI/Pt biosensor. The mesoporous structures and morphologies of SBA-15 with or without HRP were characterized. Enzymatic protein assays were employed to evaluate HRP immobilization efficiency. Our results demonstrated that the constructed biosensor displayed a fine linear correlation between cathodic response and H2O2 concentration in the range of 0.02 to 18.5 mM, with enhanced sensitivity. In particular, the current approach provided the PANI modified biosensor with improved stability for multiple measurements.

Catalytic Synthesis of n-Butyl Oleate by Cerium Complex Doped Y/SBA-15 Composite Molecular Sieve

Science.gov (United States)

Shi, Chunwei; Bian, Xue; Wu, Yongfu; Cong, Yufeng; Pei, Mingyuan

2018-01-01

Cerium ion was successfully incorporated into Y/SBA-15 micro-mesoporous molecular sieves via the hydrothermal synthesis method to give a series of composite materials. The prepared materials were thoroughly characterized using Fourier transform infrared spectroscopy (FT-IR), X-ray fluorescence spectroscopy (XRF), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and differential thermo gravimetric analysis (TG-DTG). The results showed that the prepared composite materials retained the highly ordered mesoporous two-dimensional hexagonal structure of SBA-15 and the octagonal structure of Y. The catalyst Ce-Y/SBA-15 was prepared and characterized, then the esterification of n-butanol and oleic acid was studied with bismuth phosphotungstate as a catalyst. Using this model reaction, the effects of Ce-HY/SBA-15, molar ratio of alcohol to oleic acid, amount of catalysts, reaction time and reaction temperature were investigated. The experimental results show that the optimal reaction conditions were: 1.8:1 molar ratio of alcohol to acid, 5 % catalyst amount (based on weight of oleic acid), 4 h reaction time and reflux conditions. Under these conditions, the yield of esterification was 90.6 %. The results suggest that the addition of Ce can effectively improve the catalytic properties of composite molecular sieves.

Innovative preparation of Au/C by replication of gold-containing mesoporous silica catalysts

KAUST Repository

Kerdi, Fatmé ; Caps, Valerie; Tuel, Alain

2010-01-01

A new strategy, based on the nanocasting concept, has been used to prepare gold nanoparticles (NPs) highly dispersed in meso-structured carbons. Gold is first introduced in various functionalized mesostructured silicas (MCM-48 and SBA-15

Anchoring Tri(8-QuinolinolatoIron Onto Sba-15 for Partial Oxidation of Benzyl Alcohol Using Water as the Solvent

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Yang Xiaoyuan

2014-09-01

Full Text Available Tri(8-quinolinolatoiron complex immobilized onto SBA-15 catalyst has been synthesized through a stepwise procedure. The characterization results indicated that the BET surface area, total pore volume and average pore width decrease after stepwise modification of SBA-15, while the structure keeps intact. Catalytic tests showed that FeQ3-SBA-15 catalyzes the oxidation reaction well with 34.8% conversion of benzyl alcohol and 74.7% selectivity to benzaldehyde when water is used as the solvent after 1 h reaction. In addition, homogeneous catalyst tri(8-quinolinolatoiron exhibits very bad catalytic behavior using water as the solvent.

Insight into the adsorption of tetracycline onto amino and amino-Fe3+ gunctionalized mesoporous silica: Effect of functionalized groups.

Science.gov (United States)

Zhang, Ziyang; Li, Haiyan; Liu, Huijuan

2018-03-01

In order to study the influences of functionalized groups onto the adsorption of tetracycline, we prepared a series of amino and amino-Fe 3+ complex mesoporous silica adsorbents with diverse content of amino and Fe 3+ groups (named N,N-SBA15 and Fe-N,N-SBA15). The resulting mesoporous silica adsorbents were fully characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR) and N 2 adsorption/desorption isotherms. Furthermore, the effects of functionalized groups on the removal of TC were investigated. The results showed that the periodic ordered structure of SBA-15 was maintained after modification of amino/Fe 3+ groups. The functionalized amino groups decreased the adsorption capacity while the coordinated Fe 3+ increased the adsorption capacity. The adsorption kinetics of TC fitted pseudo-second-order model well and the equilibrium was achieved quickly. The adsorption isotherms fitted the Langmuir model well and with the Fe 3+ content increased from 3.93% to 8.26%, the Q max of the adsorbents increased from 102 to 188mmol/kg. The solution pH affected the adsorption of TC onto amino complex adsorbents slightly while influenced the adsorption onto Fe-amine complex adsorbents greatly. The adsorption of TC on SBA15 and N,N-SBA15 may be related to the formation of outer-sphere surface complexes, while the adsorption of TC onto Fe-N,N-SBA15 was mainly attributed to the inner-sphere surface complexes. This study could offer potential materials that have excellent adsorption behavior for environmental remediation and suggested useful information for the preparing other adsorbents in environmental applications. Copyright © 2017. Published by Elsevier B.V.

Assessment of the adjuvant activity of mesoporous silica nanoparticles in recombinant Mycoplasma hyopneumoniae antigen vaccines

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Veridiana Gomes Virginio

2017-01-01

Full Text Available The adjuvant potential of two mesoporous silica nanoparticles (MSNs, SBa-15 and SBa-16, was assessed in combination with a recombinant HSP70 surface polypeptide domain from Mycoplasma hyopneumoniae, the etiological agent of porcine enzootic pneumonia (PEP. The recombinant antigen (HSP70212-600, previously shown as immunogenic in formulation with classic adjuvants, was used to immunize BALB/c mice in combination with SBa-15 or SBa-16 MSNs, and the effects obtained with these formulations were compared to those obtained with alum, the adjuvant traditionally used in anti-PEP bacterins. The HSP70212-600 + SBa-15 vaccine elicited a strong humoral immune response, with high serum total IgG levels, comparable to those obtained using HSP70212-600 + alum. The HSP70212-600 + SBa-16 vaccine elicited a moderate humoral immune response, with lower levels of total IgG. The cellular immune response was assessed by the detection of IFN-γ, IL-4 and IL-10 in splenocyte culture supernatants. The HSP70212-600 + SBa-15 vaccine increased IFN-γ, IL-4 and IL-10 levels, while no stimulation was detected with the HSP70212-600 + SBa-16 vaccine. The HSP70212-600 + SBa-15 vaccine induced a mixed Th1/Th2-type response, with an additional IL-10 mediated anti-inflammatory effect, both of relevance for an anti-PEP vaccine. Alum adjuvant controls stimulated an unspecific cellular immune response, with similar levels of cytokines detected in mice immunized either with HSP70212-600 + alum or with the adjuvant alone. The better humoral and cellular immune responses elicited in mice indicated that SBa-15 has adjuvant potential, and can be considered as an alternative to the use of alum in veterinary vaccines. The use of SBa-15 with HSP70212-600 is also promising as a potential anti-PEP subunit vaccine formulation.

Highly active and durable Ca-doped Ce-SBA-15 catalyst for biodiesel production

International Nuclear Information System (INIS)

Thitsartarn, Warintorn; Maneerung, Thawatchai; Kawi, Sibudjing

2015-01-01

In this work, Ca-doped Ce-incorporated SBA-15 (Ca/CeS) catalyst was successfully synthesized by using direct synthesis of Ce-incorporated SBA-15 followed by impregnation of CaO (calcium oxide). The maximum Si/Ce molar ratio that Ce atoms can be incorporated successfully into the mesoporous framework was found to be 5 (CeS-5). After the impregnation of 30 wt. % Ca, the obtained 30Ca/CeS-5 catalysts showed the superior catalytic performance for transesterification reaction of palm oil with methanol and also the higher catalytic activity as compared to other supported catalysts, i.e. CaO/CeO 2 and CaO–CeO 2 /SBA-15. This can be attributed to the well-dispersion of CaO on the CeS-5 support surface. Furthermore, it was found that the leaching of Si, Ce and Ca from the catalyst into biodiesel produced was negligible (i.e. <1 ppm after 7 cycles), indicating the strong interaction between CaO and CeS-5 support. As a result, the 30Ca/CeS-5 catalyst can be reused at least 15 cycles with insignificant decrease in catalytic activity, offering the efficient CaO-based catalyst for biodiesel production. - Highlights: • Mesoporous Ca-based catalyst was successfully developed for biodiesel production. • Catalyst exhibited high activity towards transesterification (FAME yield > 98%). • Catalyst can be effectively re-used at least 15 cycles. • Extremely low catalyst contaminant (<1 ppm) was presented

Control the Morphologies and the Pore Architectures of Meso porous Silicas through a Dual-Templating Approach

International Nuclear Information System (INIS)

Wang, H.; Chen, H.; Xu, Z.; Wang, S.; Li, B.; Li, Y.

2012-01-01

Meso porous silica nanospheres were prepared using a chiral cationic low-molecular-weight amphiphile and organic solvents such as toluene, cyclohexane, and tetrachlorocarbon through a dual-templating approach. X-ray diffraction, nitrogen sorption, field emission scanning electron microscopy, and transmission electron microscopy techniques have been used to characterize the meso porous silicas. The volume ratio of toluene to water plays an important role in controlling the morphologies and the pore architectures of the meso porous silicas. It was also found that meso porous silica nano flakes can be prepared by adding tetrahydrofuran to the reaction mixtures.

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Vapor phase hydrogenation of levulinic acid using formic acid as a hydrogen source has been conducted over ordered mesoporous Cu/Fe2O3 catalysts prepared by hard template method using mesoporous silica, SBA-15. X-ray diffraction result reveals the absence of copper peaks because of either highly dispersed state, ...

Visible Light-Induced Metal Free Surface Initiated Atom Transfer Radical Polymerization of Methyl Methacrylate on SBA-15

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Liang Ma

2017-02-01

Full Text Available Surface-initiated atom transfer radical polymerization (SI-ATRP is one of the most versatile techniques to modify the surface properties of materials. Recent developed metal-free SI-ATRP makes such techniques more widely applicable. Herein photo-induced metal-free SI-ATRP of methacrylates, such as methyl methacrylate, N-isopropanyl acrylamide, and N,N-dimethylaminoethyl methacrylate, on the surface of SBA-15 was reported to fabricate organic-inorganic hybrid materials. A SBA-15-based polymeric composite with an adjustable graft ratio was obtained. The structure evolution during the SI-ATRP modification of SBA-15 was monitored and verified by FT-IR, XPS, TGA, BET, and TEM. The obtained polymeric composite showed enhanced adsorption ability for the model compound toluene in aqueous conditions. This procedure provides a low-cost, readily available, and easy modification method to synthesize polymeric composites without the contamination of metal.

Mesoporous silica materials modified with alumina polycations as catalysts for the synthesis of dimethyl ether from methanol

Energy Technology Data Exchange (ETDEWEB)

Macina, Daniel; Piwowarska, Zofia; Tarach, Karolina; Góra-Marek, Kinga [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland); Ryczkowski, Janusz [Maria Curie Skłodowska University, Faculty of Chemistry, Maria Curie-Skłodowska 2, 20-031 Lublin (Poland); Chmielarz, Lucjan, E-mail: chmielar@chemia.uj.edu.pl [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland)

2016-02-15

Highlights: • Deposition of alumina ologoctaions on mesoporous silicas modified with surface −SO{sub 3}H groups. • Alumina aggregates generated acid properties in the silica supports. • Alumina modified SBA-15 and MCF were active and selective catalysts in DME synthesis. - Abstract: Mesoporous silica materials (SBA-15 and MCF) were used as catalytic supports for the deposition of aggregated alumina species using the method consisting of the following steps: (i) anchoring 3-(mercaptopropyl)trimethoxysilane (MPTMS) on the silica surface followed by (ii) oxidation of −SH to−SO{sub 3}H groups and then (iii) deposition of aluminum Keggin oligocations by ion-exchange method and (iv) calcination. The obtained samples were tested as catalysts for synthesis of dimethyl ether from methanol. The modified silicas were characterized with respect to the ordering of their porous structure (XRD), textural properties (BET), chemical composition (EDS, CHNS), structure ({sup 27}Al NMR, FTIR) and location of alumina species (EDX-TEM), surface acidity (NH{sub 3}-TPD, Py-FTIR) and thermal stability (TGA). The obtained materials were found to be active and selective catalysts for methanol dehydration to dimethyl ether (DME) in the MTD process (methanol-to-dimethyl ether).

VOx species supported on Al2O3-SBA-15 prepared by the grafting of alumina onto SBA-15: structure and activity in the oxidative dehydrogenation of ethane

Czech Academy of Sciences Publication Activity Database

Botková, Š.; Čapek, L.; Setnička, M.; Bulánek, R.; Čičmanec, P.; Kalužová, A.; Pastva, Jakub; Zukal, Arnošt

2016-01-01

Roč. 119, č. 1 (2016), s. 319-333 ISSN 1878-5190 R&D Projects: GA ČR GAP106/10/0196 Institutional support: RVO:61388955 Keywords : Ethane * UV-Vis * VOx species * Al2O3-SBA-15 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.264, year: 2016

Studying the loading effect of acidic type antioxidant on amorphous silica nanoparticle carriers

Science.gov (United States)

Ravinayagam, Vijaya; Rabindran Jermy, B.

2017-06-01

The study investigates the suitable nanosilica carriers to transport acidic type cargo molecules for potential targeted drug delivery application. Using phenolic acidic type antioxidant gallic acid (GA) as model compound, the present study investigates the loading effect of GA (0.3-15.9 mmol GA g-1 support) on textural characteristics of amorphous silica nanoparticles such as Q10 silica (1D), structured two-dimensional Si-MCM-41 (2D), and three-dimensional Si-SBA-16 (3D). The variation in the nature of textures after GA loading was analyzed using X-ray diffraction, N2 adsorption, FT-IR, scanning electron microscopy with energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy. Among the nanocarriers, high adsorption of GA was found in the following order: Si-SBA-16 (3D)˜Si-KIT-6 (3D) > Si-MCM-41 (2D) > ultralarge pore FDU-12 (ULPFDU-12; 3D) > Q10 (1D)˜mesostructured cellular silica foam (MSU-F). 3D-type silicas Si-SBA-16 and KIT-6 were shown to maintain structural integrity at acidic condition (pH ˜3) and accommodate GA in non-crystalline form. In the case of ULPFDU-12 and MSU-F cellular foam, only crystalline deposition of GA occurs with a significant variation in the surface area and pore volume. [Figure not available: see fulltext.

A Dual-Functional [SBA-15/Fe3O4/P(N-iPAAm] Hybrid System as a Potential Nanoplatform for Biomedical Application

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Andreza de Sousa

2014-01-01

Full Text Available The synthesis strategy of a multifunctional system of [SBA-15/Fe3O4/P(N-iPAAm] hybrids of interest for bioapplications was explored. Magnetite nanoparticles coated by mesoporous silica were prepared by an alternative chemical route using neutral surfactant and without the application of any functionalization method. Monomer adsorption followed by in situ polymerization initiated by a radical was the adopted procedure to incorporate the hydrogel into the pore channels of silica nanocomposite. Characterization of the materials was carried out by using X-ray diffraction (XRD, Fourier-transform infrared spectroscopy (FTIR, N2 adsorption, transmission electron microscopy (TEM, and Temperature programmed reduction studies (TPR. Their application as drug delivery system using atenolol as a model drug to assess the influence of the application of low frequency alternating magnetic fields on drug release was evaluated. The structural characteristics of the magnetic hybrid nanocomposite, including the effect of the swelling behavior on heating by the application of an alternating magnetic field, are presented and discussed.

Catalytic Steam Reforming of Toluene as a Model Compound of Biomass Gasification Tar Using Ni-CeO2/SBA-15 Catalysts

Directory of Open Access Journals (Sweden)

Erik Dahlquist

2013-07-01

Full Text Available Nickel supported on SBA-15 doped with CeO2 catalysts (Ni-CeO2/SBA-15 was prepared, and used for steam reforming of toluene which was selected as a model compound of biomass gasification tar. A fixed-bed lab-scale set was designed and employed to evaluate the catalytic performances of the Ni-CeO2/SBA-15 catalysts. Experiments were performed to reveal the effects of several factors on the toluene conversion and product gas composition, including the reaction temperature, steam/carbon (S/C ratio, and CeO2 loading content. Moreover, the catalysts were subjected to analysis of their carbon contents after the steam reforming experiments, as well as to test the catalytic stability over a long experimental period. The results indicated that the Ni-CeO2/SBA-15 catalysts exhibited promising capabilities on the toluene conversion, anti-coke deposition and catalytic stability. The toluene conversion reached as high as 98.9% at steam reforming temperature of 850 °C and S/C ratio of 3 using the Ni-CeO2(3wt%/SBA-15 catalyst. Negligible coke formation was detected on the used catalyst. The gaseous products mainly consisted of H2 and CO, together with a little CO2 and CH4.

A novel visible light-driven Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite: Preparation and application in the photo-degradation of pollutants

Energy Technology Data Exchange (ETDEWEB)

Chai, Yuanyuan; Wang, Li; Ren, Jia; Dai, Wei-Lin, E-mail: wldai@fudan.edu.cn

2015-01-01

Graphical abstract: - Highlights: • Highly efficient visible-light-driven Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite. • Application in the photo-degradation of RhB. • Synthesis from a facile and simple colloidal method. • 20%-Ag{sub 3}PO{sub 4}/SBA-15 shows 8 times faster degradation rate than Ag{sub 3}PO{sub 4}. • Super stability and recycling ability. - Abstract: A novel visible light-driven environmental-benign Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite photo-catalyst was synthesized for the photo-degradation of pollutants. The exploration on adsorption and photo-catalysis of dye or organic pollution for the nanocomposite was carried out. The adsorption capability for Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite increases by 3 times compared with that of the Ag{sub 3}PO{sub 4} particles. The photo-catalytic activity of nanocomposite is higher than pristine Ag{sub 3}PO{sub 4} nanoparticle for the degradation of RhB or MO under visible light irradiation (λ > 420 nm). The effect of Ag{sub 3}PO{sub 4} loading on the catalytic performance was also studied. The results show that the optimum degradation is achieved over 20% Ag{sub 3}PO{sub 4}/SBA-15. Compared to pure Ag{sub 3}PO{sub 4} nanoparticle, the most efficient catalyst showed 8 times higher photo-catalytic activity for the degradation of RhB. The Ag{sub 3}PO{sub 4}/SBA-15 catalysts were systematically characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–Vis diffuse reflectance spectroscopy (DRS), and N{sub 2}-adsorption–desorption isotherms (BET). A possible mechanism scheme regarding photo-degradation enhancement induced by dye enrichments has been proposed on the Ag{sub 3}PO{sub 4}/SBA-15 nanocomposite. Additionally, the SBA-15 support can enhance the efficiency of separation of catalyst from the reaction mixture, implying that the Ag{sub 3}PO{sub 4} loading on the SBA-15 catalyst will not result in the extra environment and health

Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

Science.gov (United States)

Albayati, Talib M.; Doyle, Aidan M.

2015-02-01

Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption-desorption porosimetry (Brunauer-Emmett-Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96-99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction.

Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

Energy Technology Data Exchange (ETDEWEB)

Albayati, Talib M., E-mail: talib-albyati@yahoo.com [University of Technology, Department of Chemical Engineering (Iraq); Doyle, Aidan M., E-mail: a.m.doyle@mmu.ac.uk [Manchester Metropolitan University, Division of Chemistry and Environmental Science (United Kingdom)

2015-02-15

Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption–desorption porosimetry (Brunauer–Emmett–Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96–99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction.

Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

International Nuclear Information System (INIS)

Albayati, Talib M.; Doyle, Aidan M.

2015-01-01

Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption–desorption porosimetry (Brunauer–Emmett–Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96–99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction

Surface PEGylation of mesoporous silica materials via surface-initiated chain transfer free radical polymerization: Characterization and controlled drug release.

Science.gov (United States)

Huang, Long; Liu, Meiying; Mao, Liucheng; Huang, Qiang; Huang, Hongye; Wan, Qing; Tian, Jianwen; Wen, Yuanqing; Zhang, Xiaoyong; Wei, Yen

2017-12-01

As a new type of mesoporous silica materials with large pore diameter (pore size between 2 and 50nm) and high specific surface areas, SBA-15 has been widely explored for different applications especially in the biomedical fields. The surface modification of SBA-15 with functional polymers has demonstrated to be an effective way for improving its properties and performance. In this work, we reported the preparation of PEGylated SBA-15 polymer composites through surface-initiated chain transfer free radical polymerization for the first time. The thiol group was first introduced on SBA-15 via co-condensation with γ-mercaptopropyltrimethoxysilane (MPTS), that were utilized to initiate the chain transfer free radical polymerization using poly(ethylene glycol) methyl ether methacrylate (PEGMA) and itaconic acid (IA) as the monomers. The successful modification of SBA-15 with poly(PEGMA-co-IA) copolymers was evidenced by a series of characterization techniques, including 1 H NMR, FT-IR, TGA and XPS. The final SBA-15-SH- poly(PEGMA-co-IA) composites display well water dispersity and high loading capability towards cisplatin (CDDP) owing to the introduction of hydrophilic PEGMA and carboxyl groups. Furthermore, the CDDP could be released from SBA-15-SH-poly(PEGMA-co-IA)-CDDP complexes in a pH dependent behavior, suggesting the potential controlled drug delivery of SBA-15-SH-poly(PEGMA-co-IA). More importantly, the strategy should be also useful for fabrication of many other functional materials for biomedical applications owing to the advantages of SBA-15 and well monomer adoptability of chain transfer free radical polymerization. Copyright © 2017 Elsevier B.V. All rights reserved.

Covalent immobilization of lipase onto chitosan-mesoporous silica hybrid nanomaterials by carboxyl functionalized ionic liquids as the coupling agent.

Science.gov (United States)

Xiang, Xinran; Suo, Hongbo; Xu, Chao; Hu, Yi

2018-05-01

Chitosan-mesoporous silica SBA-15 hybrid nanomaterials (CTS-SBA-15) were synthesized by means of carboxyl functionalized ionic liquids as the coupling agent. The as-prepared CTS-SBA-15 support was characterized by TEM, FTIR, TG and nitrogen adsorption-desorption techniques. Porcine pancreas lipase (PPL) was then bound to the hybrid nanomaterials by using the cross-linking reagent glutaraldehyde (GA). Further, the parameters like cross-linking concentration, time and ratio of supports to enzyme were optimized. The property of immobilized lipase were tested in detail by enzyme activity assays. The results indicated that the hybrid nanomaterials could form three-dimensional (3D) structure with homogeneous mesoporous structures and immobilized PPL revealed excellent enzymatic performance. Copyright © 2018 Elsevier B.V. All rights reserved.

Micelle-template synthesis of hollow silica spheres for improving water vapor permeability of waterborne polyurethane membrane

Science.gov (United States)

Bao, Yan; Wang, Tong; Kang, Qiaoling; Shi, Chunhua; Ma, Jianzhong

2017-04-01

Hollow silica spheres (HSS) with special interior spaces, high specific surface area and excellent adsorption and permeability performance were synthesized via micelle-template method using cetyl trimethyl ammonium bromide (CTAB) micelles as soft template and tetraethoxysilane (TEOS) as silica precursor. SEM, TEM, FT-IR, XRD, DLS and BET-BJH were carried out to characterize the morphology and structure of as-obtained samples. The results demonstrated that the samples were amorphous with a hollow structure and huge specific surface area. The growth of HSS was an inward-growth mechanism along template. Notably, we have provided a new and interesting fundamental principle for HSS materials by precisely controlling the ethanol-to-water volume ratio. In addition, the as-obtained HSS were mixed with waterborne polyurethane (WPU) to prepare WPU/HSS composite membrane. Various characterizations (SEM, TEM, FT-IR and TGA) revealed the morphology, polydispersity and adherence between HSS and WPU. Performance tests showed that the introduction of HSS can improve the water vapor permeability of composite membrane, promoting its water resistance and mechanical performance at the same time.

Modeling of boldine alkaloid adsorption onto pure and propyl-sulfonic acid-modified mesoporous silicas. A comparative study

Energy Technology Data Exchange (ETDEWEB)

Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland); Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Berdychowo 4, 60-965 Poznań (Poland)

2016-12-01

The present study deals with the adsorption of boldine onto pure and propyl-sulfonic acid-functionalized SBA-15, SBA-16 and mesocellular foam (MCF) materials. Siliceous adsorbents were characterized by nitrogen sorption analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier-transform infrared (FT-IR) spectroscopy and thermogravimetric analysis. The equilibrium adsorption data were analyzed using the Langmuir, Freundlich, Redlich-Peterson, and Temkin isotherms. Moreover, the Dubinin-Radushkevich and Dubinin-Astakhov isotherm models based on the Polanyi adsorption potential were employed. The latter was calculated using two alternative formulas including solubility-normalized (S-model) and empirical C-model. In order to find the best-fit isotherm, both linear regression and nonlinear fitting analysis were carried out. The Dubinin-Astakhov (S-model) isotherm revealed the best fit to the experimental points for adsorption of boldine onto pure mesoporous materials using both linear and nonlinear fitting analysis. Meanwhile, the process of boldine sorption onto modified silicas was described the best by the Langmuir and Temkin isotherms using linear regression and nonlinear fitting analysis, respectively. The values of adsorption energy (below 8 kJ/mol) indicate the physical nature of boldine adsorption onto unmodified silicas whereas the ionic interactions seem to be the main force of alkaloid adsorption onto functionalized sorbents (energy of adsorption above 8 kJ/mol). - Graphical abstract: Modeling of boldine adsorption onto unmodified and propyl-sulfonic acid-modified mesoporous adsorbents. - Highlights: • The process of boldine adsorption onto SBA-15, SBA-16 and MCF silicas was examined. • Siliceous adsorbents were functionalized with propyl-sulfonic acid groups. • The equilibrium adsorption data were analyzed using several isotherm models. • Both linear regression and nonlinear fitting analysis were carried out. �

Functionalized mesoporous silicas with crown ether moieties for selective adsorption of lithium ions in artificial sea water.

Science.gov (United States)

Sung, Soo Park; Moorthy, Madhappan Santha; Song, Hyun-Jin; Ha, Chang-Sik

2014-11-01

Lithium ion has been increasingly recognized in a wide range of industrial applications. In this work, we studied on the adsorption of Li+ in the artificial seawater with high selectivity using methyl-crown ether (AC-SBA-15) and aza-crown ether (HMC-SBA-15) moieties-functionalized mesoporous silica materials. First, methyl-crown ether and aza-crown ether moieties-functionalized mesoporous silica materials were synthesized via two-step post-synthesis process using a grafting method. The functionalized materials were employed to the metal ion adsorption from aqueous solution (artificial seawater) containing Li+, Co2+, Cr3+ and Hg2+. The prepared hybrid material showed high selectivity for Li+ ion in the artificial seawater at pH 8.0. The absorbed amount of Li+ was 73 times higher than Cr3+ for aza-crown ether containing AC-SBA-15 as an absorbent. The absorbed amount of Co2+ (4.5 x 10(-5) mol/g), Cr3+ (1.5 x 10(-5) mol/g) and Hg2+ (2.25 x 10(-4) mol/g) were remarkably lower than the case of Li+. On the other hand, the absorbed amount of various metal ions of HMC-SBA-15 with amine groups in alky chains and crown ether moieties were 1.1 x 10(-3) mol/g for Li+, 5.0 x 10(-5) mol/g for Co2+, 2.9 x 10(-4) mol/g for Cr3+, 2.8 x 10(-4) mol/g for Hg2+ mol/g, respectively.

Kinetically-controlled template-free synthesis of hollow silica micro-/nanostructures with unusual morphologies

International Nuclear Information System (INIS)

Zhang, An-Qi; Li, Hui-Jun; Qian, Dong-Jin; Chen, Meng

2014-01-01

We report a kinetically-controlled template-free room-temperature production of hollow silica materials with various novel morphologies, including tubes, crutches, ribbons, bundles and bells. The obtained products, which grew in a well-controlled manner, were monodispersed in shape and size. The role of ammonia, sodium citrate, polyvinylpyrrolidone, chloroauric acid and NaCl in shape control is discussed in detail. The oriented growth of these micro-/nanostructures directed by reverse micelles followed a solution–solution–solid (SSS) mechanism, similar to the classic vapor–liquid–solid mechanism. The evolution processes of silica rods, tubes, crutches, bundles and bells were recorded using transmission electron microscopy to prove the SSS mechanism. (paper)

Controlling pore morphology and properties of nanoporous silica films using the different architecture PS-b-P2VP as a template.

Science.gov (United States)

Yu, Yang-Yen; Chien, Wen-Chen; Chen, Shih-Ting

2010-07-01

Nanoporous silica films were prepared through the templating of amphiphilic block copolymer, poly(styrene-2-vinyl pyridine) (PS-b-P2VP), and monodispersed colloidal silica nanoparticles. The experimental and theoretical studies suggested that the intermolecular hydrogen bonding existes between the colloidal silica nanoparticles and PS-b-P2VP. The effects of the loading ratio and P2VP chain length on the morphology and properties of the prepared nanoporous silica films were investigated. TEM and AFM studies showed that the uniform pore size could be achieved and the pore size increased with increasing porogen loading. The refractive index and dielectric constant of the prepared nanoporous films decreased with an increase in PS-b-P2VP loading. On the other hand, the porosity increased with an increasing PS-b-P2VP loading. This study demonstrated a methodology to control pore morphology and properties of the nanoporous silica films through the templating of PS-b-P2VP.

Study of DDT and its derivatives DDD, DDE adsorption and degradation over Fe-SBA-15 at low temperature

Institute of Scientific and Technical Information of China (English)

Hailin Wang; Hua Tian; Zhengping Hao

2012-01-01

Mesoporous SBA-15 with different Fe2O3 loading were synthesized by an in-situ coating progress for removals of dichlorodiphenyltrichloroethane(DDT)and its derivatives,i.e.,1,1-dichloro-2,2-bis-(p-chlorophenyl)ethane(DDD)and 1,l-dichloro-2,2-bis-(4-chloro -phenyl)ethane(DDE).The results from XRD(X-ray diffractometer),TEM(transmission electron microscopy)indicated that the iron could be well dispersed on SBA-15 within 6 wt.% Fe2O3 loading.Nitrogen adsorption-desorption tests indicated that the synthesized materials were characterized by ordered meso-structure,high surface area and large pore volume.DDTs were removed from aqueous media in 12-hr treatment and high removal efficiency of DDTs was achieved at over 94%.DDTs could be completely degraded at 350℃ under the existence of SBA-15 with 4 wt.% Fe2O3 loading.The final degradation products of DDT were dichlorobenzophenone (DCB)and bis-(4-chloro-phenyl)methane(DDM),suggesting a complete dechlorination from trichloromethyl.

Understanding the effect of postsynthesis ammonium treatment on the catalytic activity of Au/TI-SBA-15 catalysts for the oxidation of propene

NARCIS (Netherlands)

Sacaliuc, E.; Friedrich, H.; Palkovits, R.; Weckhuysen, B.M.; Nijhuis, T.A.

2008-01-01

Postsynthesis ammonium treatment induces a substantial increase in the catalytic activity of Au/Ti-SBA-15 catalysts for the direct vapor-phase epoxidation of propylene using hydrogen and oxygen. The PO formation rate of a calcined Au/Ti-SBA-15 catalyst prepared by this method increased from 4.3 mgPO

Alizarin red S functionalized mesoporous silica modified glassy carbon electrode for electrochemical determination of anthracene

International Nuclear Information System (INIS)

Liu, Shan; Wei, Maochao; Zheng, Xiangli; Xu, Shuai; Xia, Fangquan; Zhou, Changli

2015-01-01

Highlights: • Alizarin red S-SBA15 composite was prepared and characterized. • A novel sensing platform was constructed for anthracene determination. • The proposed sensor exhibited high sensitivity and low detection limit for detecting anthracene. • This method can be applied to the practical detection of anthracene in waste water. - Abstract: In the paper, a novel and sensitive electrochemical sensor based on modification of electroactive alizarin red S functionalized mesoporous silica material SBA15 onto glassy carbon electrode (ARS-SBA15/GCE) was developed. Alizarin red S, called electrochemical probe that can selectively recognize polycyclic aromatic hydrocarbons (PAHs), as tools for the detection of tricyclic aromatic hydrocarbon anthracene. The morphology and interface property of ARS modified SBA15 (ARS-SBA15) were examined by transmission electron microscopy (TEM) and fourier transform infrared spectroscopy (FTIR). Taking advantage of the π-π stacking force between alizarin red S and anthracene, the ARS-SBA15/GCE sensor could detect anthracene quantitatively in a wide range of 1.0 pM–10.0 nM and a low detection limit of 0.5 pM (S/N = 3). Other PAHs, such as naphthalene, phenanthrene, pyrene, and benzo[a]pyrene show little interference on the detection. Consequently, a simple and sensitive electrochemical method was proposed for the determination of anthracene, which can be used to determine anthracene in waste water samples. The electrochemical method provides a general tool that complements the commonly used spectroscopic methods and immune method for the detection of PAHs

Removal of lead(II ions from aqueous solutions using cashew nut shell liquid-templated thiol-silica materials

Directory of Open Access Journals (Sweden)

J. E. G. Mdoe

2014-09-01

Full Text Available A range of thiol-silica composites were prepared using cashew nut shell liquid (CNSL or one of its phenolic constituents, cardanol, as templates. The procedure involved formation of a CNSL or cardanol emulsion in a water-ethanol system into which (3-mercaptopropyl-trimethoxysilane and tetraethyl orthosilicate were simultaneously added at various ratios. The reaction mixture was aged at room temperature for 18 h followed by a Soxhlet extraction of the template and drying. The materials were characterized by diffuse reflectance Fourier transform infrared, nitrogen physisorption, scanning electron microscopy and acid titration. Results indicated that indeed the thiol-silica composites were successfully prepared, with thiol group loadings ranging from 1.6-2.5 mmol/g. The materials were tested for lead(II adsorption, and results showed that they had maximum adsorption capacities up to 66.7 mg/g, depending on the thiol group loading and type of template used in preparing the adsorbent. DOI: http://dx.doi.org/10.4314/bcse.v28i3.5

Generation of Well-Defined Pairs of Silylamine on Highly Dehydroxylated SBA-15: Application to the Surface Organometallic Chemistry of Zirconium

KAUST Repository

Azzi, Joachim

2012-01-01

achieved by an ammonia treatment of a highly dehydroxylated SBA-15 at 1000°C (SBA-151000). This support is known to contain mainly strained reactive siloxane bridges (≡Si-O-Si≡)[1] along with a small amount of isolated plus germinal silanols =Si(OH)2

Aminopropyl-modified mesoporous molecular sieves as efficient adsorbents for removal of auxins

Energy Technology Data Exchange (ETDEWEB)

Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Berdychowo 4, 60-965 Poznań (Poland); Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland)

2015-03-15

Graphical abstract: Adsorption of indole-3-acetic acid (IAA) on aminopropyl-modified mesoporous sieves. - Highlights: • Four types of mesoporous molecular sieves were used as sorbents for removal of auxins. • SBA-15, MCF, PHTS and SBA-16 were grafted with (3-aminopropyl)triethoxysilane. • The adsorption capacity of modified materials was higher as compared to pure silicas. • Surface modification and pore volume play important role in adsorption process. - Abstract: In the present study, mesoporous siliceous materials grafted with 3-aminopropyltriethoxysilane (APTES) were examined as sorbents for removal of chosen plant growth factors (auxins) such as 1-naphthaleneacetic acid (NAA), indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA). Four different types of mesoporous molecular sieves including SBA-15, PHTS, SBA-16 and MCF have been prepared via non-ionic surfactant-assisted soft templating method. Silica molecular sieves were thoroughly characterized by nitrogen adsorption–desorption analysis, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FT-IR). The maximum adsorption capacity (Q{sub max}) for NAA, IAA and IBA was in the range from 51.0 to 140.8 mg/g and from 4.3 to 7.3 mg/g for aminopropyl-modified adsorbents and pure silicas, respectively. The best adsorption performance was observed for IAA entrapment using both APTES-functionalized SBA-15 and MCF matrices (Q{sub max} of 140.8 and 137.0 mg/g, respectively) which can be ascribed to their larger pore volumes and pore diameters. Moreover, these silicas were characterized by the highest adsorption efficiency exceeding 90% at low pollutant concentration. The experimental points for adsorption of plant growth factors onto aminopropyl-modified mesoporous molecular sieves fitted well to the Langmuir equation.

Aminopropyl-modified mesoporous molecular sieves as efficient adsorbents for removal of auxins

International Nuclear Information System (INIS)

Moritz, Michał; Geszke-Moritz, Małgorzata

2015-01-01

Graphical abstract: Adsorption of indole-3-acetic acid (IAA) on aminopropyl-modified mesoporous sieves. - Highlights: • Four types of mesoporous molecular sieves were used as sorbents for removal of auxins. • SBA-15, MCF, PHTS and SBA-16 were grafted with (3-aminopropyl)triethoxysilane. • The adsorption capacity of modified materials was higher as compared to pure silicas. • Surface modification and pore volume play important role in adsorption process. - Abstract: In the present study, mesoporous siliceous materials grafted with 3-aminopropyltriethoxysilane (APTES) were examined as sorbents for removal of chosen plant growth factors (auxins) such as 1-naphthaleneacetic acid (NAA), indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA). Four different types of mesoporous molecular sieves including SBA-15, PHTS, SBA-16 and MCF have been prepared via non-ionic surfactant-assisted soft templating method. Silica molecular sieves were thoroughly characterized by nitrogen adsorption–desorption analysis, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FT-IR). The maximum adsorption capacity (Q max ) for NAA, IAA and IBA was in the range from 51.0 to 140.8 mg/g and from 4.3 to 7.3 mg/g for aminopropyl-modified adsorbents and pure silicas, respectively. The best adsorption performance was observed for IAA entrapment using both APTES-functionalized SBA-15 and MCF matrices (Q max of 140.8 and 137.0 mg/g, respectively) which can be ascribed to their larger pore volumes and pore diameters. Moreover, these silicas were characterized by the highest adsorption efficiency exceeding 90% at low pollutant concentration. The experimental points for adsorption of plant growth factors onto aminopropyl-modified mesoporous molecular sieves fitted well to the Langmuir equation

MgO-modified mesoporous silicas impregnated by potassium carbonate for carbon dioxide adsorption

Czech Academy of Sciences Publication Activity Database

Zukal, Arnošt; Pastva, Jakub; Čejka, Jiří

2013-01-01

Roč. 167, FEB 2013 (2013), s. 44-50 ISSN 1387-1811 R&D Projects: GA ČR GA203/08/0604 Institutional support: RVO:61388955 Keywords : mesoporous adsorbents * SBA-15 silica * introducing of MgO and K2CO3 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.209, year: 2013

Nitridated fibrous silica (KCC-1) as a sustainable solid base nanocatalyst

KAUST Repository

Bouhrara, Mohamed; Ranga, Chanakya; Fihri, Aziz; Shaikh, Rafik; Sarawade, Pradip; Emwas, Abdul-Hamid M.; Hedhili, Mohamed N.; Polshettiwar, Vivek

2013-01-01

We observed that support morphology has dramatic effects on the performance of nitridated silica as a base. By simply replacing conventional silica supports (such as SBA-15 and MCM-41) with fibrous nanosilica (KCC-1), we observed multifold enhancement in the catalytic activity of the nitridated solid base for Knoevenagel condensations and transesterification reactions. This enhancement of the activity can be explained by amine accessibility, which is excellent in KCC-1 due to its open and flexible fibrous structure, that facilitates penetration and interaction with basic amine sites. © 2013 American Chemical Society.

Nitridated fibrous silica (KCC-1) as a sustainable solid base nanocatalyst

KAUST Repository

Bouhrara, Mohamed

2013-09-03

We observed that support morphology has dramatic effects on the performance of nitridated silica as a base. By simply replacing conventional silica supports (such as SBA-15 and MCM-41) with fibrous nanosilica (KCC-1), we observed multifold enhancement in the catalytic activity of the nitridated solid base for Knoevenagel condensations and transesterification reactions. This enhancement of the activity can be explained by amine accessibility, which is excellent in KCC-1 due to its open and flexible fibrous structure, that facilitates penetration and interaction with basic amine sites. © 2013 American Chemical Society.

Synthesis of Hierarchically Structured Hybrid Materials by Controlled Self-Assembly of Metal-Organic Framework with Mesoporous Silica for CO2 Adsorption.

Science.gov (United States)

Chen, Chong; Li, Bingxue; Zhou, Lijin; Xia, Zefeng; Feng, Nengjie; Ding, Jing; Wang, Lei; Wan, Hui; Guan, Guofeng

2017-07-12

The HKUST-1@SBA-15 composites with hierarchical pore structure were constructed by in situ self-assembly of metal-organic framework (MOF) with mesoporous silica. The structure directing role of SBA-15 had an obvious impact on the growth of MOF crystals, which in turn affected the morphologies and structural properties of the composites. The pristine HKUST-1 and the composites with different content of SBA-15 were characterized by XRD, N 2 adsorption-desorption, SEM, TEM, FT-IR, TG, XPS, and CO 2 -TPD techniques. It was found that the composites were assembled by oriented growth of MOF nanocrystals on the surfaces of SBA-15 matrix. The interactions between surface silanol groups and metal centers induced structural changes and resulted in the increases in surface areas as well as micropore volumes of hybrid materials. Besides, the additional constraints from SBA-15 also restrained the expansion of HKUST-1, contributing to their smaller crystal sizes in the composites. The adsorption isotherms of CO 2 on the materials were measured and applied to calculate the isosteric heats of adsorption. The HS-1 composite exhibited an increase of 15.9% in CO 2 uptake capacity compared with that of HKUST-1. Moreover, its higher isosteric heats of CO 2 adsorption indicated the stronger interactions between the surfaces and CO 2 molecules. The adsorption rate of the composite was also improved due to the introduction of mesopores. Ten cycles of CO 2 adsorption-desorption experiments implied that the HS-1 had excellent reversibility of CO 2 adsorption. This study was intended to provide the possibility of assembling new composites with tailored properties based on MOF and mesoporous silica to satisfy the requirements of various applications.

Surface structural, morphological, and catalytic studies of homogeneously dispersed anisotropic Ag nanostructures within mesoporous silica

Energy Technology Data Exchange (ETDEWEB)

Sareen, Shweta [Thapar University, School of Chemistry and Biochemistry (India); Mutreja, Vishal [Maharishi Markandeshwar University, Department of Chemistry (India); Pal, Bonamali; Singh, Satnam, E-mail: ssingh@thapar.edu [Thapar University, School of Chemistry and Biochemistry (India)

2016-11-15

Highly dispersed anisotropic Ag nanostructures were synthesized within the channels of 3-aminopropyltrimethoxysilane (APTMS)-modified mesoporous SBA-15 for catalyzing the reduction of p-dinitrobenzene, p-nitrophenol, and p-nitroacetophenone, respectively. A green templating process without involving any reducing agent, by varying the amount (1–10 wt.%) of Ag loading followed by calcination at 350 °C under H{sub 2} led to change in the morphology of Ag nanoparticles from nanospheres (~7–8 nm) to nanorods (aspect ratio ~12–30 nm) without any deformation in mesoporous sieves. In comparison to white bare SBA-15, gray-colored samples were formed with Ag impregnation exhibiting absorption bands at 484 and 840 nm indicating the formation of anisotropic Ag nanostructures within mesoporous matrix. TEM and FE-SEM micrographs confirmed the presence of evenly dispersed Ag nanostructures within as well as on the surface of mesoporous matrix. AFM studies indicated a small decrease in the average roughness of SBA-15 from 20.59 to 19.21 nm for 4 wt.% Ag/m-SBA-15, illustrating the encapsulation of majority of Ag nanoparticles in the siliceous matrix and presence of small amount of Ag nanoparticles on the mesoporous support. Moreover, due to plugging of mesopores with Ag, a significant decrease in surface area from 680 m{sup 2}/g of SBA-15 to 385 m{sup 2}/g was observed. The Ag-impregnated SBA-15 catalyst displayed superior catalytic activity than did bare SBA-15 with 4 wt.% Ag-loaded catalyst exhibiting optimum activity for selective reduction of p-nitrophenol to p-aminophenol (100 %), p-nitroacetophenone to p-aminoacetophenone (100 %), and p-dinitrobenzene to p-nitroaniline (87 %), with a small amount of p-phenylenediamine formation.

Atomic-Level Organization of Vicinal Acid-Base Pairs through the Chemisorption of Aniline and Derivatives onto Mesoporous SBA15

KAUST Repository

Basset, Jean-Marie

2016-06-09

The design of novel heterogeneous catalysts with multiple adjacent functionalities is of high interest for heterogeneous catalysis. Herein, we report a method to obtain a majority bifunctional acid-base pairs on SBA15. Aniline reacts with SBA15 by opening siloxane bridges leading to N-phenylsilanamine-silanol pairs. In contrast with ammonia treated surfaces, the material is stable under air/moisture. Advanced solid state MAS NMR: 2D ¹H-¹H double-quantum, ¹H-¹³C HETCOR experiments and dynamic nuclear polarization enhanced ²⁹Si and ¹⁵N spectra demonstrate both the close proximity between the two moieties and the formation of a covalent Si-N surface bond and confirm the design of vicinal acid-base pairs. This approach was successfully applied to the design of a series of aniline derivatives bifunctional SBA15. A correlation of the substituents effects on the aromatic ring (Hammet parameters) on the kinetics of the model reaction of Knoevenagel is observed.

Highly selective epoxidation of styrene over mesoporous Au-Ti-SBA-15 via photocatalysis process: Synthesis, characterization, and catalytic application

Energy Technology Data Exchange (ETDEWEB)

Guo Yajie; Liu Zhengwang [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China); Wang Guangjian, E-mail: wgj2260@chnu.edu.cn [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China); Huang Yanhog; Kang Fangfang [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000, Anhui (China)

2011-11-15

Highly ordered Au-Ti-SBA-15 mesoporous molecular sieves were successfully synthesized by one-pot hydrothermal synthesis in acid medium, and were characterized by XRD, UV-vis, SEM, element-mapping, HRTEM, N{sub 2} adsorption, XPS, {sup 29}Si MAS NMR, NH{sub 3}-TPD and FT-IR. The as-prepared Au-Ti-SBA-15 samples were possessed of highly ordered mesostructures with larger pore diameter, pore volume and uniform mesopore size distribution. In the oxidation of styrene with H{sub 2}O{sub 2} as the oxidant over Au-Ti-SBA-15 catalyst under photo-irradiation, reaction parameters, such as molar ratio of H{sub 2}O{sub 2} to styrene, reaction time, solvent, the amount of catalyst, catalyst species, and the amount of 3% NaOH, were conditioned at length. As a result, highly selective epoxidation of styrene over catalyst was carried out perfectly for 10 min with high TOF of 4.75 Multiplication-Sign 10{sup 3} min{sup -1}.

Application of sulfonic acid functionalized nanoporous silica (SBA-Pr-SO3H in the green one-pot synthesis of triazoloquinazolinones and benzimidazoquinazolinones

Directory of Open Access Journals (Sweden)

Ghodsi Mohammadi Ziarani

2015-01-01

Full Text Available Sulfonic acid functionalized SBA-15 (SBA-Pr-SO3H with a pore size of 6 nm was proven to be an efficient heterogeneous nanoporous solid acid catalyst in the green one-pot synthesis of triazoloquinazolinones and benzimidazoquinazolinones from the reaction of aromatic aldehydes with 3-amino-1,2,4-triazole (or 2-aminobenzimidazole and dimedone under solvent free conditions.

Understanding the effect of post-synthesis ammonium treatment on the catalytic activity of Au/Ti-SBA-15 catalysts for the oxidation of propene

NARCIS (Netherlands)

Sacaliuc-Parvulescu, E.; Friedrich, H.; Palkovits, R.; Weckhuysen, B.M.; Nijhuis, T.A.

2008-01-01

Postsynthesis ammonium treatment induces a substantial increase in the catalytic activity of Au/Ti- SBA-15 catalysts for the direct vapor-phase epoxidation of propylene using hydrogen and oxygen. The PO formation rate of a calcined Au/Ti-SBA-15 catalyst prepared by this method increased from 4.3

A novel method for preparation of 8-hydroxyquinoline functionalized mesoporous silica: Aluminum complexes and photoluminescence studies

Energy Technology Data Exchange (ETDEWEB)

Badiei, Alireza, E-mail: abadiei@khayam.ut.ac.ir [School of Chemistry, College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Goldooz, Hassan [Department of Chemistry, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Ziarani, Ghodsi Mohammadi [Department of Chemistry, Faculty of Science, Alzahra University, Tehran (Iran, Islamic Republic of)

2011-03-15

8-Hydroxyquinoline (8-HQ) was attached to mesoporous silica by sulfonamide bond formation between 8-hydroxyquinoline-5-sulfonyl chloride (8-HQ-SO{sub 2}Cl) and aminopropyl functionalized SBA-15 (designated as SBA-SPS-Q) and then aluminum complexes of 8-HQ was covalently bonded to SBA-SPS-Q using coordinating ability of grafted 8-HQ.The prepared materials were characterized by powder X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier transform infrared (FT-IR), thermal analysis (TGA-DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), elemental analysis and fluorescence spectra. The environmental effects on the emission spectra of grafted 8-HQ and its complexes were studied and discussed in details.

Ordered Mesoporous Carbons as Novel and Efficient Adsorbent for Dye Removal from Aqueous Solution

OpenAIRE

Phuong T. Dang; Hoa T. H. Nguyen; Canh D. Dao; Giang H. Le; Quang K. Nguyen; Kien T. Nguyen; Hoa T. K. Tran; Tuyen V. Nguyen; Tuan A. Vu

2016-01-01

Ordered mesoporous carbons (OMCs) were successfully synthesized by using hard template and soft template methods. These materials were characterized by XRD, TEM, and N2 adsorption-desorption Brunauer-Emmett-Teller (BET). From the obtained results, it is revealed that the obtained OMCs samples showed high surface area (>1000 m2/g) with high pore volume, mainly mesopore volume (1.2–2.4 cm3/g). Moreover, OMCs samples had similar structure of the SBA-15 silica and exhibited high MB adsorption cap...

Preparation of Silica Monoliths with Macropores and Mesopores and of High Specific Surface Area with Low Shrinkage using a Template Induced Method

Energy Technology Data Exchange (ETDEWEB)

Guo, Jianyu [Shanghai Normal Univ., Shanghai (China); Lu, Yan [Shanghai Institute of Technology, Shanghai (China); Whiting, Roger [AUT Univ., Auckland (New Zealand)

2013-02-15

In this study we report a new method for the synthesis of a silica monolithic column bed with bimodal pores (throughpores and mesopores). The template induced synthesis method was used to direct bimodal pores simultaneously instead of the usual post base-treating method. Block polymer Pluronic F127 was chosen as a dual-function template to form hierarchically porous silica monolith with both macropores and mesopores. This is a simplification of the method of monolithic column preparation. Poly(ethylene glycol) was used as a partial substitute for F127 can effectively prevent shrinkage during the monolith aging process without losing much surface area (944 m{sup 2}/g to 807 m{sup 2}/g). More importantly, the resultant material showed a much narrower mesopore size (centered at 6 nm) distribution than that made using only F127 as the template reagent, which helps the mass transfer process. The solvent washing method was used to remove the remaining organic template, and it was proved to be effective enough. The new synthesis method makes the fabrication of the silica monolithic column (especially capillary column) much easier. All the structure parameters indicate that monolith PFA05 prepared by the above method is a good material for separation, with the merits of much higher surface area than usual commercial HPLC silica particles, suitable mesopore volume, narrow mesopore size distribution, low shrinkage and it is easily prepared.

Synthesis of magnetic hollow silica using polystyrene bead as a template

International Nuclear Information System (INIS)

Wu, W.; Caruntu, D.; Martin, A.; Yu, M.H.; O'Connor, C.J.; Zhou, W.L.; Chen, J.-F.

2007-01-01

In this paper, we report a new route to synthesize novel magnetic hollow silica nanospheres (MHSNs) using polystyrene particles as sacrificial templates, and TEOS and Fe 3 O 4 as precursors. TEM, EDS, XRD, and SQUID were applied to characterize MHSNs. TEM and EDS results show that the MHSNs consist of about 200 nm of hollow cores and ∼35 nm shells with ∼10 nm of Fe 3 O 4 nanoparticles embedded. The polystyrene beads were successfully removed by immersing the as-prepared silica nanocomposite in a toluene solution. XRD results demonstrate that the Fe 3 O 4 magnetic nanoparticles still keep spinel structure even heated at low temperature. The surface status of the polystyrene beads and Fe 3 O 4 nanoparticles has an important effect on the formation of the MHSNs. The MHSNs present a superparamagnetism at room temperature by SQUID measurement. The MHSNs have potential applications in biosystem and nanomedicine

Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wang Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Fang Dongmei; Li Qing [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); East China University of Science and Technology, Shanghai 200237 (China); Zhang Lingxia; Qian Rong; Zhu Yan; Qu Haiyun [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Du Yiping [East China University of Science and Technology, Shanghai 200237 (China)

2012-05-06

Highlights: Black-Right-Pointing-Pointer A modified SBA-15 mesoporous silica material (NH{sub 2}-SBA-15) was synthesized as sorbent. Black-Right-Pointing-Pointer The material was used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Black-Right-Pointing-Pointer The NH{sub 2}-SBA-15 enables retain Cr (VI) with an enrichment factor of 44. Black-Right-Pointing-Pointer The micro-column of NH{sub 2}-SBA-15 underwent more than 100 adsorption/desorption cycles. - Abstract: A modified SBA-15 mesoporous silica material NH{sub 2}-SBA-15 was synthesized successfully by grafting {gamma}-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L{sup -1} NH{sub 3}{center_dot}H{sub 2}O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min{sup -1} sample loading (300 s) and an elution flow rate of 2.0 mL min{sup -1} (24 s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 {mu}g L{sup -1} level with a detection limit of 0.2 {mu}g L{sup -1} (3 s, n = 10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607).

Preparation and physical characterization of calcium sulfate cement/silica-based mesoporous material composites for controlled release of BMP-2

Directory of Open Access Journals (Sweden)

Tan H

2015-07-01

Full Text Available Honglue Tan,1 Shengbing Yang,2 Pengyi Dai,1 Wuyin Li,1 Bing Yue2 1Luoyang Orthopedics and Traumatology Institution, Luoyang Orthopedic-Traumatological Hospital, Luoyang, 2Shanghai Key Laboratory of Orthopedic Implants, Department of Orthopedic Surgery, Shanghai Ninth People’s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai, People’s Republic of China Abstract: As a commonly used implant material, calcium sulfate cement (CSC, has some shortcomings, including low compressive strength, weak osteoinduction capability, and rapid degradation. In this study, silica-based mesoporous materials such as SBA-15 were synthesized and combined with CSC to prepare CSC/SBA-15 composites. The properties of SBA-15 were characterized by X-ray diffraction, transmission electron microscopy, and nitrogen adsorption–desorption isotherms. SBA-15 was blended into CSC at 0, 5, 10, and 20 wt%, referred to as CSC, CSC-5S (5% mass ratio, CSC-10S (10% mass ratio, and CSC-20S (20% mass ratio, respectively. Fourier-transform infrared spectroscopy and compression tests were used to determine the structure and mechanical properties of the composites, respectively. The formation of hydroxyapatite on composite surfaces was analyzed using scanning electron microscopy and X-ray diffraction after soaking in simulated body fluid. BMP-2 was loaded into the composites by vacuum freeze-drying, and its release characteristics were detected by Bradford protein assay. The in vitro degradation of the CSC/SBA-15 composite was investigated by measuring weight loss. The results showed that the orderly, nanostructured, mesoporous SBA-15 possessed regular pore size and structure. The compressive strength of CSC/SBA-15 increased with the increase in SBA-15 mass ratio, and CSC-20S demonstrated the maximum strength. Compared to CSC, hydroxyapatite that formed on the surfaces of CSC/SBA-15 was uniform and compact. The degradation rate of CSC/SBA-15 decreased with increasing

Optimal Surface Amino-Functionalization Following Thermo-Alkaline Treatment of Nanostructured Silica Adsorbents for Enhanced CO2 Adsorption

Directory of Open Access Journals (Sweden)

Obdulia Medina-Juárez

2016-11-01

Full Text Available Special preparation of Santa Barbara Amorphous (SBA-15, mesoporous silica with highly hexagonal ordered, these materials have been carried out for creating adsorbents exhibiting an enhanced and partially selective adsorption toward CO2. This creation starts from an adequate conditioning of the silica surface, via a thermo-alkaline treatment to increase the population of silanol species on it. CO2 adsorption is only reasonably achieved when the SiO2 surface becomes aminated after put in contact with a solution of an amino alkoxide compound in the right solvent. Unfunctionalized and amine-functionalized substrates were characterized through X-ray diffraction, N2 sorption, Raman spectroscopy, electron microscopy, 29Si solid-state Nuclear Magnetic Resonance (NMR, and NH3 thermal programmed desorption. These analyses proved that the thermo-alkaline procedure desilicates the substrate and eliminates the micropores (without affecting the SBA-15 capillaries, present in the original solid. NMR analysis confirms that the hydroxylated solid anchors more amino functionalizing molecules than the unhydroxylated material. The SBA-15 sample subjected to hydroxylation and amino-functionalization displays a high enthalpy of interaction, a reason why this solid is suitable for a strong deposition of CO2 but with the possibility of observing a low-pressure hysteresis phenomenon. Contrastingly, CH4 adsorption on amino-functionalized, hydroxylated SBA-15 substrates becomes almost five times lower than the CO2 one, thus giving proof of their selectivity toward CO2. Although the amount of retained CO2 is not yet similar to or higher than those determined in other investigations, the methodology herein described is still susceptible to optimization.

Silica-supported, single-site titanium catalysts for olefin epoxidation. A molecular precursor strategy for control of catalyst structure.

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Jarupatrakorn, Jonggol; Don Tilley, T

2002-07-17

A molecular precursor approach involving simple grafting procedures was used to produce site-isolated titanium-supported epoxidation catalysts of high activity and selectivity. The tris(tert-butoxy)siloxy titanium complexes Ti[OSi(O(t)Bu)(3)](4) (TiSi4), ((i)PrO)Ti[OSi(O(t)Bu)(3)](3) (TiSi3), and ((t)BuO)(3)TiOSi(O(t)Bu)(3) (TiSi) react with the hydroxyl groups of amorphous Aerosil, mesoporous MCM-41, and SBA-15 via loss of HO(t)Bu and/or HOSi(O(t)Bu)(3) and introduction of titanium species onto the silica surface. Powder X-ray diffraction, nitrogen adsorption/desorption, infrared, and diffuse reflectance ultraviolet spectroscopies were used to investigate the structures and chemical natures of the surface-bound titanium species. The titanium species exist mainly in isolated, tetrahedral coordination environments. Increasing the number of siloxide ligands in the molecular precursor decreases the amount of titanium that can be introduced this way, but also enhances the catalytic activity and selectivity for the epoxidation of cyclohexene with cumene hydroperoxide as oxidant. In addition, the high surface area mesoporous silicas (MCM-41 and SBA-15) are more effective than amorphous silica as supports for these catalysts. Supporting TiSi3 on the SBA-15 affords highly active cyclohexene epoxidation catalysts (0.25-1.77 wt % Ti loading) that provide turnover frequencies (TOFs) of 500-1500 h(-1) after 1 h (TOFs are reduced by about half after calcination). These results demonstrate that oxygen-rich siloxide complexes of titanium are useful as precursors to supported epoxidation catalysts.

Novelty of Dynamic Process in the Synthesis of Biocompatible Silica Nanotubes by Biomimetic Glycyldodecylamide as a Soft Template.

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Choi, Hyejung; Kim, Joong-Jo; Mo, Yong-Hwan; Reddy, Benjaram M; Park, Sang-Eon

2017-10-10

A dynamic process in the synthesis of silica nanotubes (SNTs) by utilizing glycyldodecylamide (GDA) as a soft template was thoroughly investigated. The morphological evolution from GDA to SNTs was deeply explored to elucidate the formation mechanism for optimizing the synthesis procedure. Various analytical tools, namely, XRD, FTIR, SEM, TEM, Z-potential, and N 2 adsorption/desorption isotherms, were employed during the synthesis procedure. The interactive structure of GDA was also investigated using TEM-EDX as a function of aging time. These studies revealed the stepwise morphology of nanograin, nanofiber, curved plate, and nanotube in the ethanol/water solution when aged at room temperature. The supramolecular GDA molded the vesicle type nanostructure which was surrounded by silica and facilitated the formation of uniform SNTs. The stimulus for GDA to be curved into a vesicle was the intermolecular hydrogen bonding between adjacent amide groups of the template molecules. This was illustrated by FTIR spectra of GDA-silica intermediate by detecting the transition of amide I peak from 1678 to 1635 cm -1 . The effect of hydrogen bonding became stronger when the sample was aged.

SBA-15-functionalized 3-oxo-ABNO as recyclable catalyst for aerobic oxidation of alcohols under metal-free conditions.

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Karimi, Babak; Farhangi, Elham; Vali, Hojatollah; Vahdati, Saleh

2014-09-01

The nitroxyl radical 3-oxo-9-azabicyclo [3.3.1]nonane-N-oxyl (3-oxo-ABNO) has been prepared using a simple protocol. This organocatalyst is found to be an efficient catalyst for the aerobic oxidation of a wide variety of alcohols under metal-free conditions. In addition, the preparation and characterization of a supported version of 3-oxo-ABNO on ordered mesoporous silica SBA-15 (SABNO) is described for the first time. The catalyst has been characterized using several techniques including simultaneous thermal analysis (STA), transmission electron microscopy (TEM), and nitrogen sorption analysis. This catalyst exhibits catalytic performance comparable to its homogeneous analogue and much superior catalytic activity in comparison with (2,2,6,6-tetramethylpiperidin-1-yl)oxy (TEMPO) for the aerobic oxidation of almost the same range of alcohols under identical reaction conditions. It is also found that SABNO can be conveniently recovered and reused at least 12 times without significant effect on its catalytic efficiency. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Facile synthesis of gold nanoparticles on propylamine functionalized SBA-15 and effect of surface functionality of its enhanced bactericidal activity against gram positive bacteria

International Nuclear Information System (INIS)

Bhuyan, Diganta; Saikia, Mrinal; Saikia, Lakshi; Gogoi, Animesh; Saikia, Ratul

2015-01-01

The facile synthesis of an SBA-15-pr- + NH 3 .Au 0 nano-hybrid material by spontaneous autoreduction of aqueous chloroaurate anions on propylamine functionalized SBA-15 was successfully demonstrated. The as-synthesized SBA-15-pr- + NH 3 .Au 0 nano-hybrid material was well characterized using low and wide angle x-ray diffraction (XRD), N 2 adsorption–desorption isotherms, Fourier transform infrared (FTIR), transmission electron microscopy (TEM), scanning electron microscopy-energy dispersive x-ray spectroscopy (SEM-EDX), x-ray photoelectron spectroscopy (XPS), UV-Visible spectroscopy and atomic absorption spectroscopy (AAS). The activity of the nano-hybrid material as a potent bactericidal agent was successfully tested against Gram positive/negative bacteria viz. Bacillus subtilis, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. The colony killing percentage of Gram positive bacteria was found to be higher than Gram negative bacteria due to the stronger electrostatic interaction between the positively-charged amine functionality of SBA-15 and the negatively charged functionality of the bacterial cell wall. (paper)

Enthalpy and interfacial free energy changes of water capillary condensed in mesoporous silica, MCM-41 and SBA-15.

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Kittaka, Shigeharu; Ishimaru, Shinji; Kuranishi, Miki; Matsuda, Tomoko; Yamaguchi, Toshio

2006-07-21

The effect of confinement on the solid-liquid phase transitions of water was studied by using DSC and FT-IR measurements. Enthalpy changes upon melting of frozen water in MCM-41 and SBA-15 were determined as a function of pore size and found to decrease with decreasing pore size. The melting point also decreased almost monotonically with a decrease in pore size. Analysis of the Gibbs-Thomson relation on the basis of the thermodynamic data showed that there were two stages of interfacial free energy change after the constant region, i.e., below a pore size of 6.0 nm: a gradual decrease down to 3.4 nm and another decrease after a small jump upward. This fact demonstrates that the simple Gibbs-Thomson relation, i.e., a linear relation between the melting point change and the inverse pore size, is limited to the range not far from the melting point of bulk water. FT-IR measurements suggest that the decrease in enthalpy change and interfacial free energy change with decreasing pore size reflect the similarity of the structures of both liquid and solid phases of water in smaller pores at lower temperatures.

Transition Metal Phosphide Nanoparticles Supported on SBA-15 as Highly Selective Hydrodeoxygenation Catalysts for the Production of Advanced Biofuels.

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Yang, Yongxing; Ochoa-Hernández, Cristina; de la Peña O'Shea, Víctor A; Pizarro, Patricia; Coronado, Juan M; Serrano, David P

2015-09-01

A series of catalysts constituted by nanoparticles of transition metal (M = Fe, Co, Ni and Mo) phosphides (TMP) dispersed on SBA-15 were synthesized by reduction of the corresponding metal phosphate precursors previously impregnated on the mesostructured support. All the samples contained a metal-loading of 20 wt% and with an initial M/P mole ratio of 1, and they were characterized by X-ray diffraction (XRD), N2 sorption, H2-TPR and transmission electron microscopy (TEM). Metal phosphide nanocatalysts were tested in a high pressure continuous flow reactor for the hydrodeoxygenation (HDO) of a methyl ester blend containing methyl oleate (C17H33-COO-CH3) as main component (70%). This mixture constitutes a convenient surrogate of triglycerides present in vegetable oils, and following catalytic hydrotreating yields mainly n-alkanes. The results of the catalytic assays indicate that Ni2P/SBA-15 catalyst presents the highest ester conversion, whereas the transformation rate is about 20% lower for MoP/SBA-15. In contrast, catalysts based on Fe and Co phosphides show a rather limited activity. Hydrocarbon distribution in the liquid product suggests that both hydrodeoxygenation and decarboxylation/decarbonylation reactions occur simultaneously over the different catalysts, although MoP/SBA-15 possess a selectivity towards hydrodeoxygenation exceeding 90%. Accordingly, the catalyst based on MoP affords the highest yield of n-octadecane, which is the preferred product in terms of carbon atom economy. Subsequently, in order to conjugate the advantages of both Ni and Mo phosphides, a series of catalysts containing variable proportions of both metals were prepared. The obtained results reveal that the mixed phosphides catalysts present a catalytic behavior intermediate between those of the monometallic phosphides. Accordingly, only marginal enhancement of the yield of n-octadecane is obtained for the catalysts with a Mo/Ni ratio of 3. Nevertheless, owing to this high selectivity

Synthesis and characterization of pharmaceutical surfactant templated mesoporous silica: Its application to controlled delivery of duloxetine

Energy Technology Data Exchange (ETDEWEB)

Mani, Ganesh; Pushparaj, Hemalatha; Peng, Mei Mei; Muthiahpillai, Palanichamy [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Udhumansha, Ubaidulla [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Department of Pharmaceutics, C.L. Baid Metha College of Pharmacy, Chennai (India); Jang, Hyun Tae, E-mail: htjang@hanseo.ac.kr [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of)

2014-03-01

Graphical abstract: - Highlights: • Usefulness of dual pharmaceutical surfactants in silica synthesis was evaluated. • Effects of concentration of secondary template (Tween-40) were studied. • Effects of fixed solvothermal condition on mesostructure formation were studied. • Duloxetine drug loading capability was studied. • Sustained release of duloxetine was evaluated. - Abstract: A new group of mesoporous silica nanoparticles (MSNs) were synthesized using combination pharmaceutical surfactants, Triton X-100 and Tween-40 as template and loaded with duloxetine hydrochloride (DX), for improving the sustained release of DX and patterns with high drug loading. Agglomerated spherical silica MSNs were synthesized by sol–gel and solvothermal methods. The calcined and drug loaded MSNs were characterized using X-ray diffraction (XRD), Braunner–Emmett–Teller (BET), thermogravimetric analysis (TGA), Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), diffuse reflectance ultraviolet–visible (DRS-UV–vis) spectroscopy. MSNs with high surface area and pore volume were selected and studied for their DX loading and release. The selected MSNs can accommodate a maximum of 34% DX within it. About 90% was released at 200 h and hence, the synthesized MSNs were capable of engulfing DX and sustain its release. Further form the Ritger and Peppas, Higuchi model for mechanism drug release from all the MSN matrices follows anomalous transport or Non-Fickian diffusion with the ‘r’ and ‘n’ value 0.9 and 0.45 < n < 1, respectively. So, from this study it could be concluded that the MSNs synthesized using pharmaceutical templates were better choice of reservoir for the controlled delivery of drug which requires sustained release.

Effect of sol aging time on the anti-reflective properties of silica coatings templated with phosphoric acid

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Wen Wen

Full Text Available Silica anti-reflective coatings have been prepared by a sol–gel dip-coating process using the sol containing phosphoric acid as a pore-forming template. The effect of the aging time of the sol on the anti-reflective properties has been investigated. The surface topography of the silica AR coatings has been characterized. With increasing sol aging time, more over-sized pores larger than 100 nm are formed in the silica coatings. These could act as scattering centers, scattering visible light and thereby lowering transmittance. The optimal aging time was identified as 1 day, and the corresponding silica coatings showed a maximum transmittance of 99.2%, representing an 8% increase compared to the bare glass substrate. Keywords: Thin films, Anti-reflective coatings, Aging, Dip-coating, Sol–gel preparation

Highly ordered mesoporous cobalt oxide nanostructures: synthesis, characterisation, magnetic properties, and applications for electrochemical energy devices.

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Wang, Guoxiu; Liu, Hao; Horvat, Josip; Wang, Bei; Qiao, Shizhang; Park, Jinsoo; Ahn, Hyojun

2010-09-24

Highly ordered mesoporous Co(3)O(4) nanostructures were prepared using KIT-6 and SBA-15 silica as hard templates. The structures were confirmed by small angle X-ray diffraction, high resolution transmission electron microscopy, and N(2) adsorption-desorption isotherm analysis. Both KIT-6 cubic and SBA-15 hexagonal mesoporous Co(3)O(4) samples exhibited a low Néel temperature and bulk antiferromagnetic coupling due to geometric confinement of antiferromagnetic order within the nanoparticles. Mesoporous Co(3)O(4) electrode materials have demonstrated the high lithium storage capacity of more than 1200 mAh g(-1) with an excellent cycle life. They also exhibited a high specific capacitance of 370 F g(-1) as electrodes in supercapacitors.

Self-immobilization of acidogenic mixed consortia on mesoporous material (SBA-15) and activated carbon to enhance fermentative hydrogen production

Energy Technology Data Exchange (ETDEWEB)

Mohan, S. Venkata; Mohanakrishna, G.; Sarma, P.N. [Bioengineering and Environmental Centre, Indian Institute of Chemical Technology, Hyderabad 500607 (India); Reddy, S. Sreevardhan; Raju, B. David; Rao, K.S. Rama [Catalysis and Physical Chemistry Division, Indian Institute of Chemical Technology, Hyderabad 500607 (India)

2008-11-15

The influence of self-immobilization of enriched acidogenic mixed consortia on fermentative hydrogen (H{sub 2}) production was studied on different supporting materials [SBA-15 (mesoporous) and activated carbon (granular; GAC and powder; PAC)] using chemical wastewater as substrate. Batch fermentation experiments were performed with same substrate at different organic loading rates (OLRs) under acidophilic microenvironment (pH 5.5) and room temperature (28 {+-} 2 C). Experimental data evidenced the effectiveness of attached growth on both the H{sub 2} yields and substrate degradation efficiency, particularly at higher loading rates. Among the three materials evaluated, immobilization on SBA-15 material showed comparatively effective performance in enhancing both H{sub 2} yield and substrate degradation. Suspended growth (SG-control) culture showed inhibition in terms of both H{sub 2} production and substrate degradation especially at applied higher loading rates. Immobilization on SBA-15 resulted in nine times higher H{sub 2} production (7.29 mol/kg COD{sub R}-day at OLR of 0.83 kg COD/m{sup 3}-day) than the lowest yield observed (suspended growth at OLR of 2.55 kg COD/m{sup 3}-day). Maximum substrate degradation rate (SDR) of 0.96 kg COD/m{sup 3}-day (OLR 2.55 kg COD/m{sup 3}-day) was also observed with SBA-15 immobilization, which is 1.62 times higher than the lowest substrate degradation observed with SG-control experiments with the same OLR. Attached growth on GAC and PAC also showed remarkable improvement in the process performance at higher OLRs compared to SG-control. (author)

Amine bridges grafted mesoporous silica, as a prolonged/controlled drug release system for the enhanced therapeutic effect of short life drugs

Energy Technology Data Exchange (ETDEWEB)

Rehman, Fozia, E-mail: foziaics@yahoo.com [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil); Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Ahmed, Khalid; Airoldi, Claudio [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil); Gaisford, Simon; Buanz, Asma [UCL School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX (United Kingdom); Rahim, Abdur; Muhammad, Nawshad [Interdisciplinary Research Centre in Biomedical Materials (IRCBM), COMSATS Institute of Information Technology, Lahore (Pakistan); Volpe, Pedro L.O. [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084–971 Campinas, SP (Brazil)

2017-03-01

Hybrid mesoporous silica SBA-15, with surface incorporated cross-linked long hydrophobic organic bridges was synthesized using stepwise synthesis. The synthesized materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-rays diffraction, thermogravimetry and scanning and transmission electron microscopy. The functionalized material showed highly ordered mesoporous network with a surface area of 629.0 m{sup 2} g{sup −1}. The incorporation of long hydrophobic amine chains on silica surface resulted in high drug loading capacity (21% Mass/Mass) and prolonged release of ibuprofen up till 75.5 h. The preliminary investigations suggests that the synthesized materials could be proposed as controlled release devices to prolong the therapeutic effect of short life drugs such as ibuprofen to increase its efficacy and to reduce frequent dosage. - Highlights: • Silica SBA-15 was synthesized and modified with long hydrophobic amine linkers. • These materials were characterized using different techniques. • The modified material showed high drug loading capacity and control ibuprofen release in biological fluids.

Amine bridges grafted mesoporous silica, as a prolonged/controlled drug release system for the enhanced therapeutic effect of short life drugs

International Nuclear Information System (INIS)

Rehman, Fozia; Ahmed, Khalid; Airoldi, Claudio; Gaisford, Simon; Buanz, Asma; Rahim, Abdur; Muhammad, Nawshad; Volpe, Pedro L.O.

2017-01-01

Hybrid mesoporous silica SBA-15, with surface incorporated cross-linked long hydrophobic organic bridges was synthesized using stepwise synthesis. The synthesized materials were characterized by elemental analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption, X-rays diffraction, thermogravimetry and scanning and transmission electron microscopy. The functionalized material showed highly ordered mesoporous network with a surface area of 629.0 m 2 g −1 . The incorporation of long hydrophobic amine chains on silica surface resulted in high drug loading capacity (21% Mass/Mass) and prolonged release of ibuprofen up till 75.5 h. The preliminary investigations suggests that the synthesized materials could be proposed as controlled release devices to prolong the therapeutic effect of short life drugs such as ibuprofen to increase its efficacy and to reduce frequent dosage. - Highlights: • Silica SBA-15 was synthesized and modified with long hydrophobic amine linkers. • These materials were characterized using different techniques. • The modified material showed high drug loading capacity and control ibuprofen release in biological fluids.

Soft-Templating Synthesis of Mesoporous Silica-Based Materials for Environmental Applications

Science.gov (United States)

Gunathilake, Chamila Asanka

Dissertation research is mainly focus on: 1) the development of mesoporous silica materials with organic pendant and bridging groups (isocyanurate, amidoxime, benzene) and incorporated metal (aluminum, zirconium, calcium, and magnesium) species for high temperature carbon dioxide (CO2) sorption, 2) phosphorous-hydroxy functionalized mesoporous silica materials for water treatment, and 3) amidoxime-modified ordered mesoporous silica materials for uranium sorption under seawater conditions. The goal is to design composite materials for environmental applications with desired porosity, surface area, and functionality by selecting proper metal oxide precursors, organosilanes, tetraethylorthosilicate, (TEOS), and block copolymer templates and by adjusting synthesis conditions. The first part of dissertation presents experimental studies on the merge of aluminum, zirconium, calcium, and magnesium oxides with mesoporous silica materials containing organic pendant (amidoxime) and bridging groups (isocyanurate, benzene) to obtain composite sorbents for CO2 sorption at ambient (0-25 °C) and elevated (60-120 °C) temperatures. These studies indicate that the aforementioned composite sorbents are fairly good for CO2 capture at 25 °C via physisorption mechanism and show a remarkably high affinity toward CO2 chemisorption at 60-120 °C. The second part of dissertation is devoted to silica-based materials with organic functionalities for removal of heavy metal ions such as lead from contaminated water and for recovery of metal ions such as uranium from seawater. First, ordered mesoporous organosilica (OMO) materials with diethylphosphatoethyl and hydroxyphosphatoethyl surface groups were examined for Pb2+ adsorption and showed unprecedented adsorption capacities up to 272 mg/g and 202 mg/g, respectively However, the amidoxime-modified OMO materials were explored for uranium extraction under seawater conditions and showed remarkable capacities reaching 57 mg of uranium per gram

Synthesis and Application of Cerium-Incorporated SBA-16 Supported Ni-Based Oxygen Carrier in Cyclic Chemical Looping Steam Methane Reforming

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Maryam Meshksar

2018-01-01

Full Text Available Hydrogen, as a clean energy carrier, could be produced aided by cyclic oxidation-reduction of oxygen carriers (OCs in contact with carbonaceous fuel in chemical looping steam methane reforming (CL-SMR process. In this study, the cerium was incorporated into the SBA-16 support structure to synthesize the Ni/Ce-SBA-16 OC. The supports were synthesized using hydrothermal method followed by impregnation of Ni and characterized via low and wide angle X-ray diffraction (XRD, Brunauer-Emmett-Teller (BET, scanning electron microscopy (SEM, coupled with energy dispersive X-ray (EDX spectroscopy, and transmission electron micrograph (TEM techniques. In addition, the effect of various Si/Ce molar ratios (20–60 in the support structure, Ni loading (10–30 wt %, reaction temperature (500–750 °C, and life time of optimal oxygen carrier over 16 cycles were investigated. The results of wide angle XRD and SEM revealed that the incorporation of CeO2 in the channels of SBA-16 caused the formation of nickel metallic particles with smaller size and prevents the coke formation. The results showed that OC with 15 wt % Ni and Si/Ce molar ratio of 40 (15Ni/Ce-SBA-16(40 has the best performance when compared with other OCs in terms of catalytic activity and structural properties. The methane conversion of about 99.7% was achieved at 700 °C using 15Ni/Ce-SBA-16(40 OC. We anticipate that the strategy can be extended to investigate a variety of novel modified mesoporous silica as the supporting material for the Ni based OCs.

Hierarchically mesoporous silica materials prepared from the uniaxially stretched polypropylene membrane and surfactant templates

International Nuclear Information System (INIS)

Wang Xiaocong; Ma Jin; Liu Jin; Zhou Chen; Zhao, Yan; Yi Shouzhi; Yang Zhenzhong

2006-01-01

Hierarchically mesoporous silica materials with a bimodal distribution were template-prepared from uniaxially stretched polypropylene membrane in the presence of a surfactant via a sol-gel process. Their regularity and morphologies were characterized by transmission electron microscopy (TEM), x-ray diffraction and Brunauer-Emmett-Teller (BET) surface area analysis. The larger channel pores formed by removing the microfibrils of uniaxially stretched polypropylene membrane have a broad pore size distribution, and their size is around 13 nm. In contrast, the smaller mesopores formed by surfactant templates have a narrow distribution; their size is about 3.9 nm. The size of the smaller pores could be tuned from 2 to 6 nm by selecting different surfactants and by changing the concentration of reactants

MIL-53(Fe), MIL-101, and SBA-15 porous materials: potential platforms for drug delivery.

Science.gov (United States)

Gordon, Jeff; Kazemian, Hossein; Rohani, Sohrab

2015-02-01

Conventional drug administration suffers from several drawbacks, including a lack of specificity for diseased tissue, the necessity of large and frequent doses, and adverse side effects. Great effort is currently being devoted to developing nanoparticle-based therapeutics capable of prolonging drug administration and providing better control. Here we demonstrate the use of flexible microporous MIL-53(Fe) and mesoporous MIL-101 and SBA-15 as matrices for the adsorption and in vitro drug delivery of acetaminophen, progesterone, and stavudine. A drug loading of 20 wt.% was achieved for each of the nanomaterials using an incipient wetness impregnation procedure. BET, DSC, and XRPD analyses indicated that the entire loaded amount of each of the model drugs had successfully been incorporated within the mesoporous channels of both MIL-101 and SBA-15. DSC analysis evidenced that a portion of each of the model drugs had deposited onto the outer surface of MIL-53(Fe) particles; however, the portion of each drug that had incorporated within the microporous channels was slowly delivered in a diffusion-controlled process, which occurred over a period of up to six days for acetaminophen. These results demonstrate the unique ability of MIL-53(Fe) to adapt its porosity and optimize drug-matrix interactions. Owing to its larger pore diameters and weaker host-guest interactions, MIL-101 release times were shorter, yet still prolonged, as evidenced by the complete release of stavudine after five days. Complete release of each of the drugs from SBA-15 occurred very quickly as a result of rapid drug dissolution and diffusion out of the mesopores. Copyright © 2014 Elsevier B.V. All rights reserved.

Optical oxygen sensing materials based on a novel dirhenium(I) complex assembled in mesoporous silica

International Nuclear Information System (INIS)

Liu Yanhong; Li Bin; Cong Yan; Zhang Liming; Fan Di; Shi Linfang

2011-01-01

A new dirhenium(I) complex fac-[{Re(CO) 3 (4,7-dinonadecyl-1,10-phenanthro -line)} 2 (4,4'-bipyridyl)] (trifluoromethanesulfonate) 2 (denoted as D-Re(I) ) is assembled in MCM-41 and SBA-15 type mesoporous silica support. The emission peaks of D-Re(I) in D-Re(I)/MCM-41 and D-Re(I)/SBA-15 are observed at 522 and 517 nm, respectively. Their long excited lifetimes, which are of the order of microseconds, indicate the presence of phosphorescence emission arising from the metal to ligand charge-transfer (MLCT) transition. The luminescence intensities of D-Re(I)/MCM-41 and D-Re(I)/SBA-15 decrease remarkably with increase in the oxygen concentration, meaning that they can be used as optical oxygen sensing materials based on luminescence quenching. The ratios I 0 /I 100 of D-Re(I)/MCM-41 and D-Re(I)/SBA-15 are estimated to be 5.6 and 20.1, respectively. The obtained Stern-Volmer oxygen quenching plots of the mesoporous sensing materials could be fitted well to the two-site Demas model and Lehrer model. - Research highlights: → Dirhenium(I) complex assembled in mesoporous molecular sieves for oxygen sensor design. → Large α-diimine ligand L used to improve oxygen sensing properties. → High sensitivity (I 0 /I 100 ) up to 20.1.

Ionic conductivity of sodium silicate glasses grown within confined volume of mesoporous silica template

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Chatterjee, Soumi; Saha, Shyamal Kumar; Chakravorty, Dipankar

2018-04-01

Nanodimensional sodium silicate glasses of composition 30Na2O.70SiO2 has been prepared within the pores of 5.5 nm of mesoporous silica as a template using the surfactant P123. The nanocomposite was characterized by X-ray diffraction, transmission electron microscope, and X-ray photoelectron spectroscopy. Electrical conductivity of the sample was studied by ac impedance spectroscopy. The activation energy for ionic conduction was found to be 0.13 eV with dc conductivity at room temperature of 10-6 S-cm-1. This is attributed to the creation of oxygen ion vacancies at the interface of mesoporous silica and nanoglass arising out of the presence of Si2+ species in the system. These nanocomposites are expected to be useful for applications in sodiumion battery for storage of renewable energy.

New strategy for surface functionalization of periodic mesoporous silica based on meso-HSiO1.5.

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Xie, Zhuoying; Bai, Ling; Huang, Suwen; Zhu, Cun; Zhao, Yuanjin; Gu, Zhong-Ze

2014-01-29

Organic functionalization of periodic mesoporous silicas (PMSs) offers a way to improve their excellent properties and wide applications owing to their structural superiority. In this study, a new strategy for organic functionalization of PMSs is demonstrated by hydrosilylation of the recently discovered "impossible" periodic mesoporous hydridosilica, meso-HSiO1.5. This method overcomes the disadvantages of present pathways for organic functionalization of PMSs with organosilica. Moreover, compared to the traditional functionalization on the surface of porous silicon by hydrosilylation, the template-synthesized meso-HSiO1.5 is more flexible to access functional-groups-loaded PMSs with adjustable microstructures. The new method and materials will have wider applications based on both the structure and surface superiorities.

Giant dielectric permittivity in interrupted silver nanowires grown within mesoporous silica

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Maity, Anupam; Samanta, Subha; Chatterjee, Soumi; Maiti, Ramaprasad; Biswas, Debasish; Saha, Shyamal K.; Chakravorty, Dipankar

2018-06-01

Nanoglasses in the system Ag2O–SiO2 were formed within the pores of mesoporous silica SBA-15 (Santa Barbara Amorphous). Silver nanowires of diameter 5 nm were grown within SBA-15 by the process of electrodeposition. The nanowires were disrupted by applying a suitable voltage pulse. Detailed transmission and scanning electron microscopy studies were carried out. The disrupted silver strands were found to have an average length of 90 nm. The density of interrupted strands was estimated from the electron micrographs and found to have values in the range (10–20)  ×  1010 cm‑2. Dielectric constant and dielectric loss factors of the nanocomposites of disrupted silver strand—containing Ag2O–SiO2 glass and SBA-15 were found to have values in the range 200–300 and 0.014–0.008 respectively at frequencies in the range 10 kHz–2 MHz. These values were found to be in satisfactory agreement with the theoretical model of Rice and Bernasconi emanating from the theory of Gorkhov and Eliashberg. These nanocomposites are expected to be useful in the fabrication of supercapacitors, after developing suitable electrode system for the material.

Enhancement of Ag-Based Plasmonic Photocatalysis in Hydrogen Production from Ammonia Borane by the Assistance of Single-Site Ti-Oxide Moieties within a Silica Framework.

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Verma, Priyanka; Kuwahara, Yasutaka; Mori, Kohsuke; Yamashita, Hiromi

2017-03-13

Ag nanoparticles (NPs) have gained great attention owing to their interesting plasmonic properties and efficient catalysis under visible-light irradiation. In this study, an Ag-based plasmonic catalyst supported on mesoporous silica with isolated and tetrahedrally coordinated single-site Ti-oxide moieties, namely, Ag/Ti-SBA-15, was designed with the purpose of utilizing the broad spectral range of solar energy. The Ti-SBA-15 support allows the deposition of small Ag NPs with a narrow size distribution. The chemical structure, morphology, and optical properties of the prepared catalyst were characterized by techniques such as UV/Vis, FT extended X-ray absorption fine structure, and X-ray photoelectron spectroscopy, field-emission SEM, TEM, and N 2 physisorption studies. The catalytic activity of Ag/Ti-SBA-15 in hydrogen production from ammonia borane by hydrolysis was significantly enhanced in comparison with Ag/SBA-15 without Ti-oxide moieties and Ag/TiO 2 /SBA-15 involving agglomerated TiO 2 , both in the dark and under light irradiation. Improved electron transfer under light irradiation caused by the creation of heterojunctions between Ag NPs and Ti-oxide moieties explains the results obtained in the present study. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

An efficient hybrid, nanostructured, epoxidation catalyst: titanium silsesquioxane-polystyrene copolymer supported on SBA-15.

Science.gov (United States)

Zhang, Lei; Abbenhuis, Hendrikus C L; Gerritsen, Gijsbert; Bhriain, Nollaig Ní; Magusin, Pieter C M M; Mezari, Brahim; Han, Wei; van Santen, Rutger A; Yang, Qihua; Li, Can

2007-01-01

A novel interfacial hybrid epoxidation catalyst was designed with a new immobilization method for homogeneous catalysts by coating an inorganic support with an organic polymer film containing active sites. The titanium silsesquioxane (TiPOSS) complex, which contains a single-site titanium active center, was immobilized successfully by in-situ copolymerization on a mesoporous SBA-15-supported polystyrene polymer. The resulting hybrid materials exhibit attractive textural properties (highly ordered mesostructure, large specific surface area (>380 m2 g-1) and pore volume (>or==0.46 cm3 g-1)), and high activity in the epoxidation of alkenes. In the epoxidation of cyclooctene with tert-butyl hydrogen peroxide (TBHP), the hybrid catalysts have rate constants comparable with that of their homogeneous counterpart, and can be recycled at least seven times. They can also catalyze the epoxidation of cyclooctene with aqueous H2O2 as the oxidant. In two-phase reaction media, the catalysts show much higher activity than their homogeneous counterpart due to the hydrophobic environment around the active centers. They behave as interfacial catalysts due to their multifunctionality, that is, the hydrophobicity of polystyrene and the polyhedral oligomeric silsesquioxanes (POSS), and the hydrophilicity of the silica and the mesoporous structure. Combination of the immobilization of homogeneous catalysts on two conventional supports, inorganic solid and organic polymer, is demonstrated to achieve novel heterogeneous catalytic ensembles with the merits of attractive textural properties, tunable surface properties, and optimized environments around the active sites.

Three-dimensional metallic opals fabricated by double templating

International Nuclear Information System (INIS)

Yan Qingfeng; Nukala, Pavan; Chiang, Yet-Ming; Wong, C.C.

2009-01-01

We report a simple and cost-effective double templating method for fabricating large-area three-dimensional metallic photonic crystals of controlled thickness. A self-assembled polystyrene opal was used as the first template to fabricate a silica inverse opal on a gold-coated glass substrate via sol-gel processing. Gold was subsequently infiltrated to the pores of the silica inverse opal using electrochemical deposition. A high-quality three-dimensional gold photonic crystal was obtained after removal of the secondary template (silica inverse opal). The effects of template sphere size and deposition current density on the gold growth rate, and the resulting morphology and growth mechanism of the gold opal, were investigated.

新型靛红衍生化β-环糊精键合SBA-15液相色谱固定相的制备与表征%Preparation and Characterization of a Novel Isatin Derivative of β-Cyclodextrin-bonded SBA-15 Stationary Phase for HPLC

Institute of Scientific and Technical Information of China (English)

张杨; 李来生; 程彪平; 周仁丹; 聂桂珍

2014-01-01

利用靛红的羰基与β-环糊精单取代乙二胺的缩合反应，合成得到一种靛红衍生化β-环糊精Schiff碱类化合物。以3-异氰酸丙基三乙氧基硅烷为偶联剂，将其键合到自制的有序介孔二氧化硅材料SBA-15表面，制得一种新型的靛红衍生化β-环糊精键合SBA-15液相色谱固定相( ISCDP)。分别对β-环糊精衍生物、SBA-15及固定相进行必要的结构表征。在反相色谱条件下，以卤代尿嘧啶类极性化合物和二取代苯位置异构体为探针，评价新固定相的基本色谱性能。在极性有机溶剂和反相模式下，将新固定相分别用于β-受体阻滞剂药物和丹磺酰化氨基酸对映体的拆分，探讨了相关色谱分离机理。实验表明，靛红吲哚环的引入，增强了环糊精类固定相对卤代尿嘧啶的反相色谱分离能力，分析时间小于7 min。固定相分离硝基苯胺、氨基苯酚和苯二酚的位置异构体时也表现出较高的立体选择性，其中对位异构体均最后被洗脱，这与包结作用相关；靛红衍生化β-环糊精配体也提高了固定相的手性分离能力，除疏水作用外，靛红衍生化β-环糊精配体还能提供偶极、氢键、π-π和包结等作用，多种协同作用力有利于提高新固定相的手性和非手性分离的选择性。 SBA-15作为键合基质，其有序的孔结构有利于保持色谱柱的良好渗透性和小的传质阻力，在快速高效分离分析中具有应用潜能。%An isatin derivative ofβ-cyclodextrin Schiff base was first synthesized by the condensation reaction between the carbonyl group of isatin and ethylenediamino group of the mono-substituted β-cyclodextrin. The Schiff base ligand was chemically linked to homemade ordered mesoporous SBA-15 silica gel via 3-( triethoxysilyl) propyl isocyanate coupling agent. In this way, a novel isatin derivative of β-cyclodextrin-bonded SBA-15 stationary phase ( ISCDP) was prepared

Well-defined azazirconacyclopropane complexes supported on silica structurally determined by 2D NMR comparative elucidation

KAUST Repository

El Eter, Mohamad; Hamzaoui, Bilel; Abou-Hamad, Edy; Pelletier, Jeremie; Basset, Jean-Marie

2013-01-01

Grafting of Zr(NMe2)4 on mesoporous silica SBA-15 afforded selectively well-defined surface species SiOZr(NMe2) (η2NMeCH2). 2D solid-state NMR (1H- 13C HETCOR, Multiple Quantum) experiments have shown a unique structural rearrangement occurring on the immobilised zirconium bis methylamido ligand. © The Royal Society of Chemistry 2013.

Jet-Fuel Range Hydrocarbons from Biomass-Derived Sorbitol over Ni-HZSM-5/SBA-15 Catalyst

Directory of Open Access Journals (Sweden)

Yujing Weng

2015-12-01

Full Text Available Aromatics and cyclic-hydrocarbons are the significant components of jet fuel with high energy-density. However, conventional technologies for bio-fuel production cannot produce these products without further aromatization and isomerization. In this work, renewable liquid fuel with high content of aromatics and cyclic-hydrocarbons was obtained through aqueous catalytic conversion of biomass sorbitol over Ni-HZSM-5/SBA-15 catalyst. Texture characteristics of the catalyst were determined by physisorption of N2, which indicated its bimodal pore structures were microporous (HZSM-5, pore width: 0.56 nm and mesoporous (SBA-15, pore width: 8 nm. The surface acidity included weak and strong acid sites, predominantly Lewis type, and was further confirmed by the NH3-TPD and Py-IR analysis. The catalytic performances were tested in a fixed-bed reactor under the conditions of 593 K, WHSV of 0.75 h−1, GHSV of 2500 h−1 and 4.0 MPa of hydrogen pressure, whereby oil yield of 40.4 wt. % with aromatics and cyclic-hydrocarbons content of 80.0% was obtained.

Functionalized silica nanoparticles as a carrier for Betamethasone Sodium Phosphate: Drug release study and statistical optimization of drug loading by response surface method.

Science.gov (United States)

Ghasemnejad, M; Ahmadi, E; Mohamadnia, Z; Doustgani, A; Hashemikia, S

2015-11-01

Mesoporous silica nanoparticles with a hexagonal structure (SBA-15) were synthesized and modified with (3-aminopropyl) triethoxysilane (APTES), and their performance as a carrier for drug delivery system was studied. Chemical structure and morphology of the synthesized and modified SBA-15 were characterized by SEM, BET, TEM, FT-IR and CHN technique. Betamethasone Sodium Phosphate (BSP) as a water soluble drug was loaded on the mesoporous silica particle for the first time. The response surface method was employed to obtain the optimum conditions for the drug/silica nanoparticle preparation, by using Design-Expert software. The effect of time, pH of preparative media, and drug/silica ratio on the drug loading efficiency was investigated by the software. The maximum loading (33.69%) was achieved under optimized condition (pH: 1.8, time: 3.54 (h) and drug/silica ratio: 1.7). The in vitro release behavior of drug loaded particles under various pH values was evaluated. Finally, the release kinetic of the drug was investigated using the Higuchi and Korsmeyer-Peppas models. Cell culture and cytotoxicity assays revealed the synthesized product doesn't have any cytotoxicity against human bladder cell line 5637. Accordingly, the produced drug-loaded nanostructures can be applied via different routes, such as implantation and topical or oral administration. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and characterization of novel mesocomposites Co3O4 and CuO@OMS (ordered mesoporous silica) as active catalysts for hydrocarbon oxidation

Science.gov (United States)

Comănescu, Cezar

2014-03-01

Novel metal nanoporous transition metal oxides M x O y (Co3O4, CuO) have been synthesized by thermal decomposition of inorganic salts precursors (acetates, nitrates) impregnated into hexagonal mesoporous silica (OMS, ordered mesoporous silica) of SBA-15 type (prepared in-house) at different precursor loadings, the mesocomposites thus obtained being monitored after each impregnation-calcination step by small and wide angle powder XRD. The pore size for the ordered silica host range from 5.08 to 7.06 nm. Retention of the hexagonal silica framework has been observed in spite of the temperatures up to 500 °C. Mesoporous Co3O4 has been obtained by leaching the silica through overnight HF dissolution, which partially preserved the small-range ordering found in the parent Co3O4@OMS composite prior to leaching. Both Co3O4 ( meso) and Co3O4@SBA-15 have been tested in methane oxidation and were found to be superior to the bulk Co3O4 performance, with mesoporous Co3O4 being able to fully oxidize methane to CO2 and H2O at 350 °C, while Co3O4@OMS exhibits a lower activity with 20 % conversion at 350 °C. CuO@OMS shows the lowest activity, with only 13 % conversion at 500 °C.

Hollow Mesoporous Carbon Microparticles and Micromotors with Single Holes Templated by Colloidal Silica-Assisted Gas Bubbles.

Science.gov (United States)

Huang, Xiaoxi; Zhang, Tao; Asefa, Tewodros

2017-07-01

A simple, new synthetic method that produces hollow, mesoporous carbon microparticles, each with a single hole on its surface, is reported. The synthesis involves unique templates, which are composed of gaseous bubbles and colloidal silica, and poly(furfuryl alcohol) as a carbon precursor. The conditions that give these morphologically unique carbon microparticles are investigated, and the mechanisms that result in their unique structures are proposed. Notably, the amount of colloidal silica and the type of polymer are found to hugely dictate whether or not the synthesis results in hollow asymmetrical microparticles, each with a single hole. The potential application of the particles as self-propelled micromotors is demonstrated. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A polyacrylonitrile copolymer-silica template for three-dimensional hierarchical porous carbon as a Pt catalyst support for the oxygen reduction reaction.

Science.gov (United States)

Liu, Minmin; Li, Jian; Cai, Chao; Zhou, Ziwei; Ling, Yun; Liu, Rui

2017-08-01

Herein, we report a novel route to construct a hierarchical three-dimensional porous carbon (3DC) through a copolymer-silica assembly. In the synthesis, silica acts as a hard template and leads to the formation of an interconnected 3D macropore, whereas styrene-co-acrylonitrile polymer has been used as both a carbon source and a soft template for micro- and meso-pores. The obtained 3DC materials possess a large surface area (∼550.5 m 2 g -1 ), which facilitates high dispersion of Pt nanoparticles on the carbon support. The 3DC-supported Pt electrocatalyst shows excellent performance in the oxygen reduction reaction (ORR). The easy processing ability along with the characteristics of hierarchical porosity offers a new strategy for the preparation of carbon nanomaterials for energy application.

Silica needle template fabrication of metal hollow microneedle arrays

International Nuclear Information System (INIS)

Zhu, M W; Li, H W; Chen, X L; Tang, Y F; Lu, M H; Chen, Y F

2009-01-01

Drug delivery through hollow microneedle (HMN) arrays has now been recognized as one of the most promising techniques because it minimizes the shortcomings of the traditional drug delivery methods and has many exciting advantages—pain free and tunable release rates, for example. However, this drug delivery method has been hindered greatly from mass clinical application because of the high fabrication cost of HMN arrays. Hence, we developed a simple and cost-effective procedure using silica needles as templates to massively fabricate HMN arrays by using popular materials and industrially applicable processes of micro- imprint, hot embossing, electroplating and polishing. Metal HMN arrays with high quality are prepared with great flexibility with tunable parameters of area, length of needle, size of hollow and array dimension. This efficient and cost-effective fabrication method can also be applied to other applications after minor alterations, such as preparation of optic, acoustic and solar harvesting materials and devices

Silica needle template fabrication of metal hollow microneedle arrays

Science.gov (United States)

Zhu, M. W.; Li, H. W.; Chen, X. L.; Tang, Y. F.; Lu, M. H.; Chen, Y. F.

2009-11-01

Drug delivery through hollow microneedle (HMN) arrays has now been recognized as one of the most promising techniques because it minimizes the shortcomings of the traditional drug delivery methods and has many exciting advantages—pain free and tunable release rates, for example. However, this drug delivery method has been hindered greatly from mass clinical application because of the high fabrication cost of HMN arrays. Hence, we developed a simple and cost-effective procedure using silica needles as templates to massively fabricate HMN arrays by using popular materials and industrially applicable processes of micro- imprint, hot embossing, electroplating and polishing. Metal HMN arrays with high quality are prepared with great flexibility with tunable parameters of area, length of needle, size of hollow and array dimension. This efficient and cost-effective fabrication method can also be applied to other applications after minor alterations, such as preparation of optic, acoustic and solar harvesting materials and devices.

Microwave-induced synthesis of highly dispersed gold nanoparticles within the pore channels of mesoporous silica

International Nuclear Information System (INIS)

Gu Jinlou; Fan Wei; Shimojima, Atsushi; Okubo, Tatsuya

2008-01-01

Highly dispersed gold nanoparticles have been incorporated into the pore channels of SBA-15 mesoporous silica through a newly developed strategy assisted by microwave radiation (MR). The sizes of gold are effectively controlled attributed to the rapid and homogeneous nucleation, simultaneous propagation and termination of gold precursor by MR. Diol moieties with high dielectric and dielectric loss constants, and hence a high microwave activation, were firstly introduced to the pore channels of SBA-15 by a simple addition reaction between amino group and glycidiol and subsequently served as the reduction centers for gold nanoparticles. Extraction of the entrapped gold from the nanocomposite resulted in milligram quantities of gold nanoparticles with low dispersity. The successful assembly process of diol groups and formation of gold nanoparticles were monitored and tracked by solid-state NMR and UV-vis measurements. Characterization by small angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the incorporation of gold nanoparticles would not breakup the structural integrity and long-range periodicity of SBA-15. The gold nanoparticles had a narrow size distribution with diameters in the size range of 5-10 nm through TEM observation. The average particles size is 7.9 nm via calculation by the Scherrer formula and TEM measurements. Nitrogen adsorption and desorption isotherms gave further evidence that the employed method was efficient and gold nanoparticles were successfully incorporated into the pore channels of SBA-15. - Graphical abstract: A facile and novel strategy has been developed to incorporate gold nanoparticles into the pore channels of mesoporous SBA-15 assisted by microwave radiation (MR) with mild reaction condition and rapid reaction speed. Due to the rapid and homogeneous nucleation, simultaneous propagation and termination by MR, the size of gold nanoparticles are effectively controlled

Comparison of the Acidity of Heteropolyacids Encapsulated in or Impregnated on SBA-15

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Pinto Teresa

2016-03-01

Full Text Available Heteropolyacids (HPA immobilized onto SBA-15 silica were prepared by two different ways using either impregnation or encapsulation methodologies. Two Keggin-type HPA, H3PW12O40 and H4SiW12O40 were considered in this study. The resulting hybrid materials were fully characterized by N2 adsorption-desorption isotherms, XRD, FT-IR, Raman, diffuse reflectance UV-Vis spectroscopies and 31P MAS NMR. All characterization methods showed that at room temperature the catalysts contained well-dispersed and intact Keggin units throughout the solid. The catalytic activity of these solids was investigated in the isomerization of n-hexane. The impregnated and encapsulated phosphotungstic catalysts performed similarly in catalysis showing that the amount of active sites was nearly the same in both catalysts. On the contrary, the tungstosilicic encapsulated material was completely inactive while its impregnated counterpart was even more active than the phosphotungstic derived catalysts. The acidity of the solids was measured by various methods: microcalorimetry of ammonia adsorption, ammonia desorption followed by Temperature Programmed Desorption (TPD and DRIFT/GC-MS and pyridine adsorption followed by infrared spectroscopy. Only pyridine adsorption and ammonia desorption followed by DRIFT/GC-MS agreed with the catalytic data. Ammonia adsorption followed by microcalorimetry was not able to differentiate between the four catalysts while the TPD experiments led to unreliable results, as not only the evolved ammonia but also other molecules such as water were taken into account in the measurements. The behavior difference between the encapsulated silico- and phosphotungstic acids was explained by a more pronounced encapsulation in the case of silicon.

无外加酸体系中AlSBA¯15为模板,有序介孔炭材料CMK¯3的合成与表征%Synthesis and characterization of ordered mesoporous carbons CMK_3 produced by tailoring the mesopores of an AlSBA_15 hard template synthesized without acid

Institute of Scientific and Technical Information of China (English)

石磊; 徐艳; 邢立淑; 李湘萍; 杨成; 林森

2014-01-01

在无外加酸体系中改变晶化温度合成AlSBA¯15介孔材料,并以此为刚性模板,蔗糖为碳源,合成出一系列具有不同孔结构的有序介孔炭材料CMK¯3,系统考察晶化温度对AlSBA¯15和其反相复制结构CMK¯3孔道结构的影响。结果显示在无外加酸合成体系中改变晶化温度可对AlSBA¯15的孔道结构进行有效调控,通过结构复制技术可制备出具有不同结构的CMK¯3。控制刚性模板AlSBA¯15的晶化温度为90益,所得介孔炭材料CMK¯3(CMK¯3(90))结构最佳,除介孔排列高度有序外,还具有高比表面积(1688 m2·g-1)和大孔容(0.95 cm3·g-1)。另外,对CMK¯3的微孔性质与刚性模板孔壁中的次级介孔结构的内在联系进行研究,发现调变刚性模板的晶化温度可以有效改善有序介孔炭材料CMK¯3的结构性质。%Highly ordered mesoporous carbons ( OMCs) designated CMK¯3 were synthesized using mesoporous Al¯SBA¯15 with different textural properties as hard templates and sucrose as a carbon source. Al¯SBA¯15 is an ordered mesoporous alumina¯silica synthesized with a soft template, P123. The effect of the aging temperature for the hard templates on the pore structure of CMK¯3 was investigated. X¯ray diffraction, N2 adsorption and transmission electron microscopy were used to characterize the pore structures of the hard templates and the resultant CMK¯3. Result indicates that CMK¯3 with different pore structures can be obtained by tailor¯ ing the pore structures of the hard templates bysimply controlling the aging temperature in an acid¯free medium. The best CMK¯3 possessed a highly¯ordered pore structure, and a very high BET surface area (1 688 m2 ·g-1 ) and pore volume (0. 95 cm3 ·g-1 ) when the hard template was aged at 90 ℃. The microporous character of the CMK¯3 was related to the thickness of the mesopore wall of the hard templates. The textural characteristics of the resultant CMK¯3 can be improved by simply

Facile synthesis of functionalized ionic surfactant templated mesoporous silica for incorporation of poorly water-soluble drug.

Science.gov (United States)

Li, Jing; Xu, Lu; Yang, Baixue; Wang, Hongyu; Bao, Zhihong; Pan, Weisan; Li, Sanming

2015-08-15

The present paper reported amino group functionalized anionic surfactant templated mesoporous silica (Amino-AMS) for loading and release of poorly water-soluble drug indomethacin (IMC) and carboxyl group functionalized cationic surfactant templated mesoporous silica (Carboxyl-CMS) for loading and release of poorly water-soluble drug famotidine (FMT). Herein, Amino-AMS and Carboxyl-CMS were facilely synthesized using co-condensation method through two types of silane coupling agent. Amino-AMS was spherical nanoparticles, and Carboxyl-CMS was well-formed spherical nanosphere with a thin layer presented at the edge. Drug loading capacity was obviously enhanced when using Amino-AMS and Carboxyl-CMS as drug carriers due to the stronger hydrogen bonding force formed between surface modified carrier and drug. Amino-AMS and Carboxyl-CMS had the ability to transform crystalline state of loaded drug from crystalline phase to amorphous phase. Therefore, IMC loaded Amino-AMS presented obviously faster release than IMC because amorphous phase of IMC favored its dissolution. The application of asymmetric membrane capsule delayed FMT release significantly, and Carboxyl-CMS favored sustained release of FMT due to its long mesoporous channels and strong interaction formed between its carboxyl group and amino group of FMT. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of uniform carbon at silica nanocables and luminescent silica nanotubes with well controlled inner diameters

International Nuclear Information System (INIS)

Qian Haisheng; Yu Shuhong; Ren Lei; Yang Yipeng; Zhang Wei

2006-01-01

Uniform carbon at silica nanocables and silica nanotubes with well-controlled inner diameters can be synthesized in an easy way by a sacrificial templating method. This was performed using carbon nanofibres as hard templates that were synthesized previously by a hydrothermal carbonization process. Silica nanotubes with well-controlled inner diameters were synthesized from carbon at silica core-shell nanostructures by removal of the core carbon component. The inner diameters of the as-prepared silica nanotubes can be well controlled from several nanometres to hundreds of nanometres by adjusting the diameters of the carbon nanofibres. The silica nanotubes synthesized by this method display strong photoluminescence in ultraviolet at room temperature. Such uniform silica nanotubes might find potential applications in many fields such as encapsulation, catalysis, chemical/biological separation, and sensing

Innovative preparation of Au/C by replication of gold-containing mesoporous silica catalysts

KAUST Repository

Kerdi, Fatmé

2010-01-01

A new strategy, based on the nanocasting concept, has been used to prepare gold nanoparticles (NPs) highly dispersed in meso-structured carbons. Gold is first introduced in various functionalized mesostructured silicas (MCM-48 and SBA-15) and particles are formed inside the porosity upon reduction of Au 3+ cations. Silica pores are then impregnated with a carbon precursor and the composite material is heated at 900°C under vacuum. Silica is then removed by acid leaching, leading to partially encapsulated gold particles in mesoporous carbon. Carbon prevents aggregation of gold particles at high temperature, both the mean size and distribution being similar to those observed in silica. However, while Au@SiO2 exhibit significant catalytic activity in the aerobic oxidation of trans-stilbene in the liquid phase, its Au@C mesostructured replica is quite inactive. © 2010 Elsevier B.V. All rights reserved.

32 CFR 644.512 - DA-SBA joint set-aside determination.

Science.gov (United States)

2010-07-01

... 32 National Defense 4 2010-07-01 2010-07-01 true DA-SBA joint set-aside determination. 644.512 Section 644.512 National Defense Department of Defense (Continued) DEPARTMENT OF THE ARMY (CONTINUED) REAL... Stone § 644.512 DA-SBA joint set-aside determination. Section 15 of the Small Business Act (15 U.S.C...

High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO2 using ionic liquid as a template

International Nuclear Information System (INIS)

Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

2011-01-01

Mesoporous silicas and Fe-SiO 2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 o C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 o C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 o C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO 2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 o C for 12 d or steam-treated at 600 o C for 6 h. -- Graphical abstract: Worm-like mesoporous silica and Fe-SiO 2 with high hydrothermal stability have been synthesized using ionic liquid 1-hexadecane-3-methylimidazolium bromide as a template under the assistance of NaF at high temperature. Display Omitted Research highlights: → Increasing aging temperature improved the hydrothermal stability of materials. →Addition of NaF enhanced the polymerization degree of silicates. → Mesoporous SiO 2 and Fe-SiO 2 obtained have remarkable hydrothermal stability.

Metathesis of 2-pentene over Mo and W supported mesoporous molecular sieves MCM-41 and SBA-15

Czech Academy of Sciences Publication Activity Database

Ibrahim, M. A.; Akhtar, M. N.; Čejka, Jiří; Montanari, E.; Balcar, Hynek; Kubů, Martin; Al-Khattaf, S. S.

2017-01-01

Roč. 53, SEP 2017 (2017), s. 119-126 ISSN 1226-086X R&D Projects: GA ČR(CZ) GAP106/12/0189 Institutional support: RVO:61388955 Keywords : metathesis * MCM-41 * SBA-15 Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry Impact factor: 4.421, year: 2016

Syngas Production from CO2 Reforming and CO2-steam Reforming of Methane over Ni/Ce-SBA-15 Catalyst

Science.gov (United States)

Tan, J. S.; Danh, H. T.; Singh, S.; Truong, Q. D.; Setiabudi, H. D.; Vo, D.-V. N.

2017-06-01

This study compares the catalytic performance of mesoporous 10 Ni/Ce-SBA-15 catalyst for CO2 reforming and CO2-steam reforming of methane reactions in syngas production. The catalytic performance of 10 Ni/Ce-SBA-15 catalyst for CO2 reforming and CO2-steam reforming of methane was evaluated in a temperature-controlled tubular fixed-bed reactor at stoichiometric feed composition, 1023 K and atmospheric pressure for 12 h on-stream with gas hourly space velocity (GHSV) of 36 L gcat -1 h-1. The 10 Ni/Ce-SBA-15 catalyst possessed a high specific BET surface area and average pore volume of 595.04 m2 g-1. The XRD measurement revealed the presence of NiO phase with crystallite dimension of about 13.60 nm whilst H2-TPR result indicates that NiO phase was completely reduced to metallic Ni0 phase at temperature beyond 800 K and the reduction temperature relied on different degrees of metal-support interaction associated with the location and size of NiO particles. The catalytic reactivity was significantly enhanced with increasing H2O/CO2 feed ratio. Interestingly, the H2/CO ratio for CO2-steam reforming of methane varied between 1 and 3 indicated the occurrence of parallel reactions, i.e., CH4 steam reforming giving a H2/CO of 3 whilst reverse water-gas shift (RWGS) reaction consuming H2 to produce CO gaseous product.

Topology of silica supported vanadium–titanium oxide catalysts for oxidative dehydrogenation of propane

OpenAIRE

Hamilton, N.; Wolfram, T.; Tzolova-Müller, G.; Hävecker, M.; Kröhnert, J.; Carrero, C.; Schomäcker, R.; Trunschke, A.; Schlögl, R.

2012-01-01

Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG geförderten) Allianz- bzw. Nationallizenz frei zugänglich. This publication is with permission of the rights owner freely accessible due to an Alliance licence and a national licence (funded by the DFG, German Research Foundation) respectively. Two-dimensional vanadia and titania surface clusters were hosted on the walls of the hierarchical pore system of mesoporous silica SBA-15. The topology of the catalyst surfa...

Optimization of the Adsorption of Malachite Green on the NH2-SBA-15 Nano-adsorbent Using the Taguchi Method by Qualitek-4 Software An Isotherm, Kinetic, and Thermodynamic Study

Directory of Open Access Journals (Sweden)

Arghavan Mirahsani

2015-01-01

Full Text Available SBA-15 nanoporous silica was prepared and functionalized with propylamine groups via post-synthesis grafting to develop efficient adsorbents of dyes in wastewater. The materials thus prepared were then characterized by XRD, N2 adsorption-desorption, and FTIR. Adsorption of a cationic dye, malachite green, on functionalized SBA-15 was investigated under various conditions of pH (5, 6, and 7, temperature (10, 20, and 30 °C, adsorbent dosage (0.1, 0.3, and 0.5 g/L, and dye concentration (50, 100, 150, 200, 250, 300 mg/L. Maximum equilibrium adsorption capacity to achieve maximum removal percentage (R%=100% in optimum conditions (dye concentration=100 mg/L, pH=7, adsorbent dosage= 0.3 g/L was estimated at 333 mg/g. The Taguchi method was used to optimize the adsorption performances of the materials , and then the isotherm, kinetic, and thermodynamic properties were analyzed under the optimum conditions. The results showed that the overall process was fast and its kinetics was well-fitted by pseudo-second-order kinetic model. The experimental data agreed well with Freundlich model. Therefore, the maximum amount of multilayer dye adsorbed was estimated as 500 mg/g. Based on the results obtained, this process may be regarded as an endothermic one with a negative ∆G, which shows the process is also spontaneous. Finally, the results indicate that the silica‐based nanoporous organic–inorganic hybrid material can be a promising sorbent for the removal of malachite green from aquatic solutions

A green strategy for lithium isotopes separation by using mesoporous silica materials doped with ionic liquids and benzo-15-crown-5

International Nuclear Information System (INIS)

Wen Zhou; Xiao-Li Sun; Lin Gu; Fei-Fei Bao; Xin-Xin Xu; Chun-Yan Pang; Zaijun Li; Zhi-Guo Gu; Jiangnan University, Wuxi

2014-01-01

Three new mesoporous silica materials IL15SGs (HF15SG, TF15SG and DF15SG) doped with benzo-15-crown-5 and imidazolium based ionic liquids (C 8 mim + PF 6 - , C 8 mim + BF 4 - or C 8 mim + NTf 2 - ) have been prepared by a simple approach to separating lithium isotopes. The formed mesoporous structures of silica gels have been confirmed by transmission electron microscopy image and N 2 gas adsorption-desorption isotherm. Imidazolium ionic liquids acted as templates to prepare mesoporous materials, additives to stabilize extractant within silica gel, and synergetic agents to separate the lithium isotopes. Factors such as lithium salt concentration, initial pH, counter anion of lithium salt, extraction time, and temperature on the lithium isotopes separation were examined. Under optimized conditions, the extraction efficiency of HF15SG, TF15SG and DF15SG were found to be 11.43, 10.59 and 13.07 %, respectively. The heavier isotope 7 Li was concentrated in the solution phase while the lighter isotope 6 Li was enriched in the gel phase. The solid-liquid extraction maximum single-stage isotopes separation factor of 6 Li- 7 Li in the solid-liquid extraction was up to 1.046 ± 0.002. X-ray crystal structure analysis indicated that the lithium salt was extracted into the solid phase with crown ether forming [(Li 0.5 ) 2 (B 15 ) 2 (H 2 O)] + complexes. IL15SGs were also easily regenerated by stripping with 20 mmol L -1 HCl and reused in the consecutive removal of lithium ion in five cycles. (author)

Nanopatterning Gold by Templated Solid State Dewetting on the Silica Warp and Weft of Diatoms

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Jon Hiltz

2016-01-01

Full Text Available The diatom, Nitzschia palea, exhibits complex silica shell (frustule topography that resembles the warp and weft pattern of woven glass. The surface is perforated with a rhombic lattice of roughly oblong pores between periodically undulating transverse weft costae. Exfoliated frustules can be used to template gold nanoparticles by thermally induced dewetting of thin gold films. Acting as templates for the process, the frustules give rise to two coexisting hierarchies of particle sizes and patterned distributions of nanoparticles. By examining temperature dependent dewetting of 5, 10, and 15 nm Au films for various annealing times, we establish conditions for particle formation and patterning. The 5 nm film gives distributions of small particles randomly distributed over the surface and multiple particles at the rhombic lattice points in the pores. Thicker films yield larger faceted particles on the surface and particles that exhibit shapes that are roughly conformal with the shape of the pore container. The pores and costae are sources of curvature instabilities in the film that lead to mass transport of gold and selective accumulation in the weft valleys and pores. We suggest that, with respect to dewetting, the frustule comprises 2-dimensional sublattices of trapping sites. The pattern of dewetting is radically altered by interposing a self-assembled molecular adhesive of mercaptopropyltrimethoxysilane between the Au film overlayer and the frustule. By adjusting the interfacial energy in this manner, a fractal-like overlay of Au islands coexists with a periodic distribution of nanoparticles in the pores.

CO2 activation through silylimido and silylamido zirconium hydrides supported on N-donor chelating SBA15 surface ligand

KAUST Repository

Pasha, Fahran Ahmad; Bendjeriou-Sedjerari, Anissa; Abou-Hamad, Edy; Huang, Kuo-Wei; Basset, Jean-Marie

2016-01-01

Density functional theory calculations and 2D 1H-13C HETCOR solid state NMR spectroscopy prove that CO2 can probe, by its own reactivity, different types of N-donor surface ligands on SBA15-supported ZrIV hydrides: [(≡Si-O-)(≡Si-N=)[Zr]H] and [(≡Si

13 CFR 120.1010 - SBA access to SBA Lender, Intermediary, and NTAP files.

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2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA access to SBA Lender, Intermediary, and NTAP files. 120.1010 Section 120.1010 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Risk-Based Lender Oversight Supervision § 120.1010 SBA access to SBA Lender...

Synthesis Mechanism and Thermal Optimization of an Economical Mesoporous Material Using Silica: Implications for the Effective Removal or Delivery of Ibuprofen.

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Shanmuga Kittappa

Full Text Available Mesoporous silica materials (MSMs were synthesized economically using silica (SiO2 as a precursor via a modified alkaline fusion method. The MSM prepared at 500°C (MSM-500 had the highest surface area, pore size, and volume, and the results of isotherms and the kinetics of ibuprofen (IBP removal indicated that MSM-500 had the highest sorption capacity and fastest removal speed vs. SBA-15 and zeolite. Compared with commercial granular activated carbon (GAC, MSM-500 had a ~100 times higher sorption rate at neutral pH. IBP uptake by MSM-500 was thermodynamically favorable at room temperature, which was interpreted as indicating relatively weak bonding because the entropy (∆adsS, -0.07 J mol(-1 K(-1 was much smaller. Five times recycling tests revealed that MSM-500 had 83-87% recovery efficiencies and slower uptake speeds due to slight deformation of the outer pore structure. In the IBP delivery test, MSM-500 drug loading was 41%, higher than the reported value of SBA-15 (31%. The in vitro release of IBP was faster, almost 100%, reaching equilibrium within a few hours, indicating its effective loading and unloading characteristics. A cost analysis study revealed that the MSM was ~10-70 times cheaper than any other mesoporous silica material for the removal or delivery of IBP.

Cloning nanocrystal morphology with soft templates

Science.gov (United States)

Thapa, Dev Kumar; Pandey, Anshu

2016-08-01

In most template directed preparative methods, while the template decides the nanostructure morphology, the structure of the template itself is a non-general outcome of its peculiar chemistry. Here we demonstrate a template mediated synthesis that overcomes this deficiency. This synthesis involves overgrowth of silica template onto a sacrificial nanocrystal. Such templates are used to copy the morphologies of gold nanorods. After template overgrowth, gold is removed and silver is regrown in the template cavity to produce a single crystal silver nanorod. This technique allows for duplicating existing nanocrystals, while also providing a quantifiable breakdown of the structure - shape interdependence.

An ultrasensitive sandwich-type electrochemical immunosensor based on the signal amplification system of double-deck gold film and thionine unite with platinum nanowire inlaid globular SBA-15 microsphere.

Science.gov (United States)

Wang, Ping; Li, Mingdang; Pei, Fubin; Li, Yueyun; Liu, Qing; Dong, Yunhui; Chu, Qingyan; Zhu, Hongjun

2017-05-15

A novel thionine unites with platinum nanowire inlaid globular SBA-15 (Pt NWs@g-SBA-15/Thi) not only utilizes as an efficient electrical signal probe but also constitutes an amplifying system with double-deck gold film (D-Au film) have been applied to the fabrication of sandwich-type immunosensor for detecting hepatitis B surface antigen (HBs Ag). The D-Au film can accelerate the electron transfer on the electrode interface due to the tunneling effect between the two Au films and can improve the load capacity of primary antibodies (Ab 1 ) because of the good biocompatibility. The Pt NWs@g-SBA-15/Thi with uniform globular morphology not only can effectively reduce the spatial limitation for loading the secondary antibodies (Ab 2 ) but also can provide outstanding pore accessibility of guest species from outside and offer catalytically active sites in a large scale. Besides, the presence of Thi can well enhance the electrical conductivity of Pt NWs@g-SBA-15/Thi. With the good cooperation between D-Au film and Pt NWs@g-SBA-15/Thi, a linear relationship between current signals and the concentrations of HBs Ag was obtained in the wide range from 10 fg/mL to 100ng/mL and the detection limit of HBs Ag was 3.3 fg/mL (signal-to-noise ratio of 3). Furthermore, the designed immunosensor with excellent selectivity, reproducibility and stability shows excellent performance in detection of human serum samples and provides a promising capacity for detecting a wide range of other tumor markers in clinical application. Copyright © 2017 Elsevier B.V. All rights reserved.

Ordered Mesoporous Carbons as Novel and Efficient Adsorbent for Dye Removal from Aqueous Solution

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Phuong T. Dang

2016-01-01

Full Text Available Ordered mesoporous carbons (OMCs were successfully synthesized by using hard template and soft template methods. These materials were characterized by XRD, TEM, and N2 adsorption-desorption Brunauer-Emmett-Teller (BET. From the obtained results, it is revealed that the obtained OMCs samples showed high surface area (>1000 m2/g with high pore volume, mainly mesopore volume (1.2–2.4 cm3/g. Moreover, OMCs samples had similar structure of the SBA-15 silica and exhibited high MB adsorption capacity with qm of 398 mg·g−1 for OMCs synthesis with hard template and 476 mg·g−1 for OMCs synthesis with soft template, respectively. From kinetics investigation, it is confirmed that MB adsorption from aqueous solution obeys the pseudo-second-order kinetic equation.

Synthesis of mesoporous hollow silica nanospheres using polymeric micelles as template and their application as a drug-delivery carrier.

Science.gov (United States)

Sasidharan, Manickam; Zenibana, Haruna; Nandi, Mahasweta; Bhaumik, Asim; Nakashima, Kenichi

2013-10-07

Mesoporous hollow silica nanospheres with uniform particle sizes of 31-33 nm have been successfully synthesized by cocondensation of tetramethoxysilane (TMOS) and alkyltrimethoxysilanes [RSi(OR)3], where the latter also acts as a porogen. ABC triblock copolymer micelles of poly(styrene-b-2-vinyl pyridine-b-ethylene oxide) (PS-PVP-PEO) with a core-shell-corona architecture have been employed as a soft template at pH 4. The cationic shell block with 2-vinyl pyridine groups facilitates the condensation of silica precursors under the sol-gel reaction conditions. Phenyltrimethoxysilane, octyltriethoxysilane, and octadecyltriethoxysilanes were used as porogens for generating mesopores in the shell matrix of hollow silica and the octadecyl precursor produced the largest mesopore among the different porogens, of dimension ca. 4.1 nm. The mesoporous hollow particles were thoroughly characterized by small-angle X-ray diffraction (SXRD), thermal (TG/DTA) and nitrogen sorption analyses, infra-red (FTIR) and nuclear magnetic resonance ((13)C-CP MAS NMR and (29)Si MAS NMR) spectroscopies, and transmission electron microscopy (TEM). The mesoporous hollow silica nanospheres have been investigated for drug-delivery application by an in vitro method using ibuprofen as a model drug. The hollow silica nanospheres exhibited higher storage capacity than the well-known mesoporous silica MCM-41. Propylamine functionalized hollow particles show a more sustained release pattern than their unfunctionalized counterparts, suggesting a huge potential of hollow silica nanospheres in the controlled delivery of small drug molecules.

Silica nanoparticles containing 159-Gadolinium as potential system for cancer treatment

International Nuclear Information System (INIS)

Oliveira, Andre Felipe de; Ferreira, Tiago Hilario; Sousa, Edesia Martins Barros de; Lacerda, Marco Aurelio

2013-01-01

Ordered silica nanoparticles are compounds highly organized which have very interesting textural characteristics, such as high thermal stability, well defined pore size, narrow size distribution and high area surface. Among the various types of nano materials ordered, the SBA-16 have a meso structure that can be considered very interesting due to the fact of the arrangement of mesoporous (tri dimensional as a cage) and spherical morphology, which make it in a promising material for a range of bioapplications such as incorporation of drugs and radioisotopes. In this study Gadodiamide® (Omniscan-General Electric Healthcare Company), a frequently non-ionic gadolinium complex contrasting used in MRI's was incorporated in the silica matrix SBA-16 as a carrier. From this gadolinium it is possible to obtain the isotope 159 Gd by neutron irradiation, wherein the isotope 158 Gd captures a neutron and becomes 159 Gd [ 15 '8Gd(n,c) 1 '5 9 Gd]. The 159 Gd is a beta (endpoint energy of 970.6 keV) and gamma (main energy: 363.54 keV) emitter with a half-life of 18.59 hours. These characteristics are similar to that of other isotopes already used in nuclear medicine such as 90 Y. In this work, the 158 Gd incorporated in the Gd-silica was activated by the neutron flux generated by the cyclotron located in the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) during the production of the 18 FDG. Atomic emission spectroscopy (ICP-AES) and infrared spectroscopy (FTIR) were used to confirm the presence of the gadolinium complex in the silica matrix. The antitumor activity of the complex after the irradiation was evaluated through cytotoxicity assay with T98 cell lines derived from a human glioblastoma multiform tumor. (author)

Adsorptive performance of chromium-containing ordered mesoporous silica on volatile organic compounds (VOCs

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Jianwei Fan

2017-09-01

Full Text Available Volatile organic compounds (VOCs are the primary poisonous emissions into the atmosphere in natural gas exploitation and disposing process. The adsorption method has been widely applied in actual production because of its good features such as low cost, low energy consumption, flexible devices needed, etc. The commonly used adsorbents like activated carbon, silicon molecular sieves and so on are not only susceptible to plugging or spontaneous combustion but difficult to be recycled. In view of this, a new adsorbent (CrSBA15 was made by the co-assembly method to synthesize the ordered mesoporous silica materials with different amounts of chromium to eliminate VOCs. This new adsorbent was characterized by small-angle-X-ray scattering (SAXS, nitrogen adsorption/desorption, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. Its adsorption performance to eliminate VOCs (toluene, benzene, cyclohexane and ethyl acetate used as typical pollutants was also tested systematically. Research results indicate that this new adsorbent of CrSBA-15(30, with the silicon/chromium ration being 30, owns the maximum micropore volume, and shows a higher adsorption performance in eliminating toluene, benzene, cyclohexane and ethyl acetate. Besides, it is cost-effective and much easier to be recycled than the activated carbon. In conclusion, CrSBA-15(30 is a good adsorbent to eliminate VOCs with broad application prospects. Keywords: Mesoporous materials, Silicon dioxide, Synthesis, Adsorption, Volatile organic compounds (VOCs, Recyclability, Energy saving

Low temperature oxidative desulfurization with hierarchically mesoporous titaniumsilicate Ti-SBA-2 single crystals.

Science.gov (United States)

Shi, Chengxiang; Wang, Wenxuan; Liu, Ni; Xu, Xueyan; Wang, Danhong; Zhang, Minghui; Sun, Pingchuan; Chen, Tiehong

2015-07-21

Hierarchically porous Ti-SBA-2 with high framework Ti content (up to 5 wt%) was firstly synthesized by employing organic mesomorphous complexes of a cationic surfactant (CTAB) and an anionic polyelectrolyte (PAA) as templates. The material exhibited excellent performance in oxidative desulfurization of diesel fuel at low temperature (40 °C or 25 °C) due to the unique hierarchically porous structure and high framework Ti content.

Molecular imprinting at walls of silica nanotubes for TNT recognition.

Science.gov (United States)

Xie, Chenggen; Liu, Bianhua; Wang, Zhenyang; Gao, Daming; Guan, Guijian; Zhang, Zhongping

2008-01-15

This paper reports the molecular imprinting at the walls of highly uniform silica nanotubes for the recognition of 2,4,6-trinitrotoluene (TNT). It has been demonstrated that TNT templates were efficiently imprinted into the matrix of silica through the strong acid-base pairing interaction between TNT and 3-aminopropyltriethoxysilane (APTS). TNT-imprinted silica nanotubes were synthesized by the gelation reaction between APTS and tetraethylorthosilicate (TEOS), selectively occurring at the porous walls of APTS-modified alumina membranes. The removal of the original TNT templates leaves the imprinted cavities with covalently anchored amine groups at the cavity walls. A high density of recognition sites with molecular selectivity to the TNT analyte was created at the wall of silica nanotubes. Furthermore, most of these recognition sites are situated at the inside and outside surfaces of tubular walls and in the proximity of the two surfaces due to the ultrathin wall thickness of only 15 nm, providing a better site accessibility and lower mass-transfer resistance. Therefore, greater capacity and faster kinetics of uptaking target species were achieved. The silica nanotube reported herein is an ideal form of material for imprinting various organic or biological molecules toward applications in chemical/biological sensors and bioassay.

Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

Science.gov (United States)

Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

2016-08-12

A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of nanoporous silicas as adsorbents for chlorinated aromatic compounds. A comparative study

Energy Technology Data Exchange (ETDEWEB)

Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Piotrowo 3, 60-965 Poznań (Poland); Adam Mickiewicz University, Faculty of Chemistry, Umultowska 89b, 61-614 Poznań (Poland); Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland)

2014-08-01

The removal of two selected environmental pollutants such as 2,4-dichlorophenoxyacetic acid (2,4-D) and Triclosan (TC) was examined by adsorption experiments on the modified SBA-15 and MCF mesoporous silicas. Mesoporous adsorbents were modified by a grafting process with (3-aminopropyl)triethoxysilane (APTES) and 1-[3-(trimethoxysilyl)propyl]urea (TMSPU). Mesoporous materials were synthesized and characterized by N{sub 2} adsorption–desorption experiment, transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), elemental analysis and adsorption studies. The results show that both APTES-functionalized SBA-15 and MCF nanoporous carriers are potentially good adsorbents for the removal of 2,4-D in a wide range of concentrations from 0.1 to 4 mg/cm{sup 3}. Maximum adsorption capacity of as-modified adsorbents for 2,4-D estimated from the Langmuir model was ∼ 280 mg/g. The ionic interaction between the adsorbent and 2,4-D seems to play a key role in the adsorption process of the pollutant on APTES-modified siliceous matrices. The efficiency of TC sorption onto all prepared mesoporous adsorbents was significantly lower as compared to the entrapment of 2,4-D. Experimental data were best fitted by the Langmuir isotherm model. The results of this study suggest that mesoporous silica-based materials are promising adsorbents for the removal of selected organic pollutants. - Graphical abstract: Adsorption of 2,4-dichlorophenoxyacetic acid and Triclosan inside 3-amino-functionalized mesoporous channel.

Periodically Arranged Arrays of Dendritic Pt Nanospheres Using Cage-Type Mesoporous Silica as a Hard Template.

Science.gov (United States)

Kani, Kenya; Malgras, Victor; Jiang, Bo; Hossain, Md Shahriar A; Alshehri, Saad M; Ahamad, Tansir; Salunkhe, Rahul R; Huang, Zhenguo; Yamauchi, Yusuke

2018-01-04

Dendritic Pt nanospheres of 20 nm diameter are synthesized by using a highly concentrated surfactant assembly within the large-sized cage-type mesopores of mesoporous silica (LP-FDU-12). After diluting the surfactant solution with ethanol, the lower viscosity leads to an improved penetration inside the mesopores. After Pt deposition followed by template removal, the arrangement of the Pt nanospheres is a replication from that of the mesopores in the original LP-FDU-12 template. Although it is well known that ordered LLCs can form on flat substrates, the confined space inside the mesopores hinders surfactant self-organization. Therefore, the Pt nanospheres possess a dendritic porous structure over the entire area. The distortion observed in some nanospheres is attributed to the close proximity existing between neighboring cage-type mesopores. This new type of nanoporous metal with a hierarchical architecture holds potential to enhance substance diffusivity/accessibility for further improvement of catalytic activity. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nanocasting of Periodic Mesoporous Materials as an Effective Strategy to Prepare Mixed Phases of Titania

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Luther Mahoney

2015-12-01

Full Text Available Mesoporous titanium dioxide materials were prepared using a nanocasting technique involving silica SBA-15 as the hard-template. At an optimal loading of titanium precursor, the hexagonal periodic array of pores in SBA-15 was retained. The phases of titanium dioxide could be easily varied by the number of impregnation cycles and the nature of titanium alkoxide employed. Low number of impregnation cycles produced mixed phases of anatase and TiO2(B. The mesoporous TiO2 materials were tested for solar hydrogen production, and the material consisting of 98% anatase and 2% TiO2(B exhibited the highest yield of hydrogen from the photocatalytic splitting of water. The periodicity of the pores was an important factor that influenced the photocatalytic activity. This study indicates that mixed phases of titania containing ordered array of pores can be prepared by using the nanocasting strategy.

A rational repeating template method for synthesis of 2D hexagonally ordered mesoporous precious metals.

Science.gov (United States)

Takai, Azusa; Doi, Yoji; Yamauchi, Yusuke; Kuroda, Kazuyuki

2011-03-01

A repeating template method is presented for the synthesis of mesoporous metals with 2D hexagonal mesostructures. First, a silica replica (i.e., silica nanorods arranged periodically) is prepared by using 2D hexagonally ordered mesoporous carbon as the template. After that, the obtained silica replica is used as the second template for the preparation of mesoporous ruthenium. After the ruthenium species are introduced into the silica replica, the ruthenium species are then reduced by a vapor-infiltration method by using the reducing agent dimethylamine borane. After the ruthenium deposition, the silica is chemically removed. Analysis by transmission and scanning electron microscopies, a nitrogen-adsorption-desorption isotherm, and small-angle X-ray scattering revealed that the mesoporous ruthenium had a 2D hexagonal mesostructure, although the mesostructural ordering is decreased compared to that of the original mesoporous carbon template. This method is widely applicable to other metal systems. By changing the metal species introduced into the silica replica, several mesoporous metals (palladium and platinum) can be synthesized. Ordered mesoporous ruthenium and palladium, which are not easily attainable by the soft-templating methods, can be prepared. This study has overcome the composition variation limitations of the soft-templating method. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biodiesel from Hydrolyzed Waste Cooking Oil Using a S-ZrO2/SBA-15 Super Acid Catalyst under Sub-Critical Conditions

Directory of Open Access Journals (Sweden)

Muhammad Nobi Hossain

2018-01-01

Full Text Available Due to rapid changes in food habits, a substantial amount of waste fat and used oils are generated each year. Due to strong policies, the disposal of this material into nearby sewers causes ecological and environmental problems in many parts of the world. For efficient management, waste cooking oil, a less expensive, alternative and promising feedstock, can be used as a raw material for producing biofuel. In the present study, we produced a biodiesel from hydrolyzed waste cooking oil with a subcritical methanol process using a synthesized solid super acid catalyst, a sulfated zirconium oxide supported on Santa Barbara Amorphous silica (S-ZrO2/SBA-15. The characterization of the synthesized catalyst was carried out using scanning electron microscopy (SEM, X-ray diffraction (XRD, and the Brunauer-Emmett-Teller (BET method. The catalytic effect on biodiesel production was examined by varying the parameters: temperatures of 120 to 200 °C, 5–20 min times, oil-to-methanol mole ratios between 1:5 to 1:20, and catalyst loadings of 1–2.5%. The maximum biodiesel yield was 96.383%, obtained under optimum reaction conditions of 140 °C, 10 min, and a 1:10 oil-to-methanol molar ratio with a 2.0% catalyst loading. We successfully reused the catalyst five times without regeneration with a 90% efficiency. The fuel properties were found to be within the limits set by the biodiesel standard.

Investigating the mesostructure of ordered porous silica nanocomposites by transmission electron microscopy techniques

Energy Technology Data Exchange (ETDEWEB)

Bullita, S.; Casula, M. F., E-mail: casulaf@unica.it [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) (Italy); Piludu, M. [Department of Biomedical Sciences, University of Cagliari, Monserrato (Canada) (Italy); Falqui, A. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) Italy and KAUST-King Abdullah University of Science and Technology, Jeddah (Saudi Arabia); Carta, D. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada), Italy and Faculty of Physical Sciences and Engineering, University of Southampton, Southampton (United Kingdom); Corrias, A. [INSTM and Department of Chemical and Geological Science, University of Cagliari, Monserrato (Canada) Italy and School of Physical Sciences, Ingram Building, University of Kent, Canterbury (United Kingdom)

2014-10-21

Nanocomposites made out of FeCo alloy nanocrystals supported onto pre-formed mesoporous ordered silica which features a cubic arrangement of pores (SBA-16) were investigated. Information on the effect of the nanocrystals on the mesostructure (i.e. pore arrangement symmetry, pore size, and shape) were deduced by a multitechnique approach including N2 physisorption, low angle X-ray diffraction, and Transmission electron microscopy. It is shown that advanced transmission electron microscopy techniques are required, however, to gain direct evidence on key compositional and textural features of the nanocomposites. In particular, electron tomography and microtomy techniques make clear that the FeCo nanocrystals are located within the pores of the SBA-16 silica, and that the ordered mesostructure of the nanocomposite is retained throughout the observed specimen.

Characterization of Metal-Doped Methylated Microporous Silica for Molecular Separations

DEFF Research Database (Denmark)

El-Feky, Hany Hassan; Briceno, Kelly; Szalata, Kamila

2015-01-01

Novel silica xerogels are prepared and developed by sol-gel method in the present study. The preparation involves cobalt-doping within the organic templated silica matrices, where methyltriethoxysilane (MTES), which contains methyl groups as a covalently bonded organic template is used. The synth...

Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

KAUST Repository

Chaignon, J.; Bouizi, Y.; Davin, L.; Calin, N.; Albela, B.; Bonneviot, L.

2015-01-01

© The Royal Society of Chemistry 2015. Hexagonal mesostructured templated silicas were produced in less than 10 minutes using an ultra-fast microwave assisted hydrothermal synthesis. Typically, 10 g can be prepared at once in a commercial microwave device usually devoted to analytical digestion. Undesired alcohol side-products were avoided using inexpensive water colloidal silica instead of silicon alkoxides as the silicon source. In comparison with classical heating activation, the absence of pore expansion and pore wall thickening even for synthesis temperatures as high as 190 °C evidenced that heat transfer and diffusion of matter had no time to take place. Comparison between the chemically extracted and calcined samples shows that the structure was better stabilized for autoclaving above 150 °C. However, a fast temperature ramping and final temperatures above 180 °C were required to sear structures of the highest quality comparable to that of the best conventional methods. This is rationalized by assuming a sequential flake-by-flake assembly of the pore-wall at the micelle palisade. Notably, tosylate counterions yielded better structural characteristics than bromide counterions and allowed better opportunities for surfactant recycling.

NiMo Catalysts Supported on the Nb Modified Mesoporous SBA-15 and HMS: Effect of Thioglycolic Acid Addition on HDS.

Czech Academy of Sciences Publication Activity Database

Palcheva, R.; Kaluža, Luděk; Dimitrov, L.; Tyuliev, G.; Avdeev, G.; Jirátová, Květa; Spojakina, A.

2016-01-01

Roč. 50, JUN 25 (2016), s. 24-34 ISSN 0926-860X R&D Projects: GA ČR GAP106/11/0902 Institutional support: RVO:67985858 Keywords : HDS * mesoporous SBA-15 and HMS * thioglycolic acid Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.339, year: 2016

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials.

Science.gov (United States)

Hesemann, Peter; Nguyen, Thy Phung; Hankari, Samir El

2014-04-11

The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS) recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA), mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the "anionic templating" strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

Effect of the nature of the surface on the reactivity of nanoporous silica under irradiation

International Nuclear Information System (INIS)

Le Caer, S.; Alam, M.S.; Chatelain, C.; Brunet, F.; Charpentier, T.; Renault, J.P.; Brodie-Linder, N.; Alba-Simionesco, C.

2011-01-01

Complete text of publication follows. Materials such as concrete, clays and zeolites which embed radioactive wastes adsorb in their pores significant amounts of water that can be decomposed under ionizing radiation leading to the formation of H 2 which is potentially explosive. It is well established that the H 2 production arises from chemi- or physi-sorbed OH groups at the surface of oxides. In this context, we have studied the behaviour of water confined in nanoporous silica. To distinguish the behavior of the two kinds of OH, we have performed different thermal treatments on SBA-15 materials prior to their irradiation. The IR analysis and H 2 measurements have proven that in the radiolysis of SBA-15 materials, silanol groups are only attacked when they are in the majority with respect to adsorbed water. However they are much less efficient at producing H 2 . The comparison between water content before and after electron irradiation and the corresponding H 2 production indicates that water desorption is the main route to adsorbed water loss. On the other hand, surface silanol groups are more susceptible to attack, leading to H 2 production when SBA-15 samples have undergone extensive thermal treatment. The surface of nanoporous glasses were then grafted using chloroaklyldimethylsilane. The effect of irradiation on these grafted surfaces was studied by means of mass spectrometry and NMR experiments. These different techniques reveal an original reactivity of the surface under irradiation.

H2 uptake in the Li-dispersed silica nano-tubes

International Nuclear Information System (INIS)

Jin Bae Lee; Soon Chang Lee; Sang Moon Lee; Hae Jin Kim

2006-01-01

Highly ordered Li-dispersed silica nano-tubes were prepared by sol-gel template method for hydrogen storage. Isolated Li-dispersed silica nano-tubes can be easily obtained by removing the AAO template with 2M NaOH. From the XRD study, the Li-dispersed silica nano-tubes showed the amorphous phase with silica frameworks. The uniform length and diameter of Li-dispersed silica nano-tubes could be examined with the electron microscopy studies. The wall thickness and diameter of nano-tubes are about 50-60 nm and 200-400 nm, respectively. The obtained Li-dispersed silica nano-tubes have the hydrogen adsorption capacity 2.25 wt% at 77 K under 47 atm. (authors)

Generation of Well-Defined Pairs of Silylamine on Highly Dehydroxylated SBA-15: Application to the Surface Organometallic Chemistry of Zirconium

KAUST Repository

Azzi, Joachim

2012-11-01

Design of a new well-defined surface organometallic species [O-(=Si–NH)2Zr(IV)Np2] has been obtained by reaction of tetraneopentyl zirconium (ZrNp4) on SBA-15 surface displaying mainly silylamine pairs [O-(=Si–NH2)2]. These surface species have been achieved by an ammonia treatment of a highly dehydroxylated SBA-15 at 1000°C (SBA-151000). This support is known to contain mainly strained reactive siloxane bridges (≡Si-O-Si≡)[1] along with a small amount of isolated plus germinal silanols =Si(OH)2. Chemisorption of ammonia occurs primarily by opening these siloxane bridges[2] to generate silanol/silylamine pairs [O-(=Si–NH2)(=SiOH)] followed by substitution of the remaining silanol. Further treatment using hexamethyldisilazane (HMDS) results in the protection of the isolated remaining silanol groups by formation of ≡Si-O-SiMe3 and =Si(OSiMe3)2 but leaves ≡SiNH2 untouched. After reaction of this functionalized surface with ZrNp4, this latter displays mainly a bi-podal zirconium neopentyl organometallic complex [O-(=Si–NH)2Zr(IV)Np2] which has been fully characterized by diverse methods such as infrared transmission spectroscopy, magic angle spinning solid state nuclear magnetic resonance, surface elemental analysis, small angle X-ray powder diffraction (XRD), nitrogen adsorption and energy filtered transmission electron microscopy (EFTEM). These different characterization tools unambiguously prove that the zirconium organometallic complex reacts mostly with silylamine pairs to give a bi-podal zirconium bis-neopentyl complex, uniformly distributed into the channels of SBA-151000. Therefore this new material opens a new promising research area in Surface Organometallic Chemistry which, so far, was dealing mainly with O containing surface. It is expected that vicinal amine functions may play a very different role as compared with classical inorganic supports. Given the importance in the last decades of N containing ligands in catalysis, one may expect

Biomimetic synthesis of proline-derivative templated mesoporous silica for increasing the brain distribution of diazepam and improving the pharmacodynamics of nimesulide

DEFF Research Database (Denmark)

Li, Heran; Wang, Jianxin; Cong, Jialiang

2017-01-01

Herein a new kind of proline-derivative templated mesoporous silica with curved channels (CMS) was biomimetically synthesized and applied as carrier to improve the drug dissolution and bioavailability of hydrophobic diazepam (DZP) and nimesulide (NMS). Drugs can be incorporated into CMS with high...... improved, and the inhibition rates of 1:3 NMS/CMS in all pharmacodynamics tests varied from 102.2% to 904.3%....

A membrane electrode assembled photoelectrochemical cell with a solar-responsive cadmium sulfide-zinc sulfide-titanium dioxide/mesoporous silica photoanode

Science.gov (United States)

Chen, Ming; Chen, Rong; Zhu, Xun; Liao, Qiang; An, Liang; Ye, Dingding; Zhou, Yuan; He, Xuefeng; Zhang, Wei

2017-12-01

In this work, a membrane electrode assembled photoelectrochemical cell (PEC) is developed for the electricity generation by degrading the organic compounds. The photocatalyst is prepared by the incorporation of mesoporous silica SBA-15 into TiO2 and the photosensitization of CdS-ZnS to enhance the photoanode performance, while the cathode employs the air-breathing mode to enhance the oxygen transport. The experimental results show that the developed PEC exhibits good photoresponse to the illumination and the appropriate SBA-15 mass ratio in the photoanode enables the enhancement of the performance. It is also shown that the developed PEC yields better performance in the alkaline environment than that in the neutral environment. Increasing the KOH concentration can improve the cell performance. There exist optimal liquid flow rate and organics concentration leading to the best performance. Besides, it is found that increasing the light intensity can generate more electron-hole pairs and thus enhance the cell performance. These results are helpful for optimizing the design.

Nitrogen-doped mesoporous carbons for high performance supercapacitors

Science.gov (United States)

Wu, Kai; Liu, Qiming

2016-08-01

The mesoporous carbons have been synthesized by using α-D(+)-Glucose, D-Glucosamine hydrochloride or their mixture as carbon precursors and mesoporous silicas (SBA-15 or MCF) as hard templates. The as-prepared products show a large pore volume (0.59-0.97 cm3 g-1), high surface areas (352.72-1152.67 m2 g-1) and rational nitrogen content (ca. 2.5-3.9 wt.%). The results of electrochemical tests demonstrate that both heteroatom doping and suitable pore structure play a decisive role in the performance of supercapacitors. The representative sample of SBA-15 replica obtained using D-Glucosamine hydrochloride only exhibits high specific capacitance (212.8 F g-1 at 0.5 A g-1) and good cycle durability (86.1% of the initial capacitance after 2000 cycles) in 6 M KOH aqueous electrolyte, which is attributed to the contribution of double layer capacitance and pseudo-capacitance. The excellent electrochemical performance makes it a promising electrode material for supercapacitors.

Extraction of gelatin from catfish bone using NaOH and its utilization as a template on mesoporous silica alumina

Science.gov (United States)

Nuryanto, R.; Trisunaryanti, W.; Falah, I. I.; Triyono

2018-04-01

Gelatin extraction from catfish bone using NaOH and its utilization as a template on a synthesis of mesoporous silica-alumina had been investigated. The extraction was prepared by immersing 25 g catfish bone in 125 mL of NaOH in concentration of 0.0; 0.05; 0.10; 0.15 and 0.20 M for 24 h, then washing with demineralized water until pH 7, followed by immersed the bone into 125 mL of 1 M HCl for 1 h, then washed using demineralized water into pH 5. To produce gelatin the bone was refluxed with 100 mL demineralized water at 70°C for 5 h then evaporated at 50°C. The dry gelatin was characterized using FTIR and electrophoresis (SDS-PAGE). The best performance of gelatin was produced by NaOH 0.10 M. The gelatin consists of amide A, B, I, II, III and molecular weight of 25-200kDa. Silica and Alumina material prepared from Lapindo mud extraction. Dry Lapindo mud crushed and filtered until pass 100 mesh, then reflux using 6 M HCl (1:4 w/V) at 90°C for 5h then filtered. The filtrate was consisting alumina solution adding with 6 M NaOH (2/3 V/V) them filtered. The filtrate then injected by CO2 gas for 30 minutes and filtered, the residue was calcined at 500°C for 5h. The residual of Lapindo mud dried and refluxed with 6 M NaOH (1:4 w/v) at 90 °C. After 5h filtered and the filtrate added by HCl to pH 8 and filtered, the residual then dried. The Si and Al were then analyzed by XRF and consist of silica and alumina for 99.1 and 87.73%, respectively. Silica-alumina was prepared using silica and alumina extracted from Lapindo mud. 6 g of SiO2 and 2 g of NaOH was immersed in 62 mL of demineralized water then added with alumina solution (0.204 g alumina in 30 mL demineralized water). The gelatin solution (5 g gelatin in 70 mL demineralized water) was dropped into the silica-alumina while stirring at 50°C for 4 h and aging for 24 h. The synthesized silica alumina was analysed using FTIR and surface area analyser. The FT-IR spectra indicated the TO4 (T=Si, Al) vibration at wave

Chlorodiethylaluminum supported on silica: A dinuclear aluminum surface species with bridging μ2-Cl-ligand as a highly efficient co-catalyst for the Ni-catalyzed dimerization of ethene

KAUST Repository

Kermagoret, Anthony

2014-05-01

Silica-supported chloro alkyl aluminum co-catalysts (DEAC@support) were prepared via Surface Organometallic Chemistry by contacting diethylaluminum chloride (DEAC) and high specific surface silica materials, i.e. SBA-15, MCM-41, and Aerosil SiO2. Such systems efficiently activate NiCl 2(PBu3)2 for catalytic ethene dimerization, with turnover frequency (TOF) reaching up to 498,000 molC2H4/ (molNi h) for DEAC@MCM-41. A detailed analysis of the DEAC@SBA-15 co-catalyst structure by solid-state aluminum-27 NMR at high-field (17.6 T and 20.0 T) and ultrafast spinning rates allows to detect six sites, characterized by a distribution of quadrupolar interaction principal values CQ and isotropic chemical shifts δiso. Identification of the corresponding Al-grafted structures was possible by comparison of the experimental NMR signatures with these calculated by DFT on a wide range of models for the aluminum species (mono- versus di-nuclear, mono- versus bis-grafted with bridging Cl or ethyl). Most of the sites were identified as dinuclear species with retention of the structure of DEAC, namely with the presence of μ2-Cl-ligands between two aluminum, and this probably explains the high catalytic performance of this silica-supported co-catalysts. © 2014 Elsevier Inc. All rights reserved.

Tunable pores in mesoporous silica films studied using a pulsed slow positron beam

International Nuclear Information System (INIS)

He Chunqing; Muramatsu, Makoto; Ohdaira, Toshiyuki; Oshima, Nagayasu; Kinomura, Atsushi; Suzuki, Ryoichi; Kobayashi, Yoshinori

2007-01-01

Positron annihilation lifetime spectroscopy (PALS) based on a pulsed slow positron beam was applied to study mesoporous silica films, synthesized using amphiphilic PEO-PPO-PEO triblock copolymers as structure-directing agents. The pore size depends on the loading of different templates. Larger pores were formed in silica films templated by copolymers with higher molecular-weights. Using 2-dimensional PALS, open porosity of silica films was also found to be influenced by the molecular-weight as well as the ratio of hydrophobic PPO moiety of the templates

Synthesis of mesoporous zeolite catalysts by in situ formation of carbon template over nickel nanoparticles

DEFF Research Database (Denmark)

Abildstrøm, Jacob Oskar; Kegnæs, Marina; Hytoft, Glen

2016-01-01

A novel synthesis procedure for the preparation of the hierarchical zeolite materials with MFI structure based on the carbon templating method with in situ generated carbon template is presented in this study. Through chemical vapour deposition of coke on nickel nanoparticles supported on silica...... oxide, a carbon-silica composite is obtained and exploited as a combined carbon template/silica source for zeolite synthesis. This approach has several advantages in comparison with conventional carbon templating methods, where relatively complicated preparative strategies involving multistep...... impregnation procedures and rather expensive chemicals are used. Removal of the carbon template by combustion results in zeolite single crystals with intracrystalline pore volumes between 0.28 and 0.48 cm3/g. The prepared zeolites are characterized by XRD, SEM, TEM and physisorption analysis. The isomerization...

Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction

International Nuclear Information System (INIS)

Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Fattahpour, Peyman

2011-01-01

Highlights: → The polypyrrole/SBA15) nanocomposite was used as a novel coating for SPME fiber. → The proposed fiber was used for the extraction of polycyclic aromatic hydrocarbons. → The proposed SPME fiber is thermal stable, and it has a low limit of detection. → The SPME fiber was applied in polluted river water and wastewater samples. - Abstract: A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70 deg. C, extraction time 20 min, ionic strength 20% (W V -1 ), stirring rate 500 rpm, desorption temperature 270 deg. C, desorption time 5 min) the repeatability for one fiber (n = 3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL -1 . The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260 deg. C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high

13 CFR 120.1722 - SBA's offset rights.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA's offset rights. 120.1722... of SBA Secondary Market Guarantee Program for First Lien Position 504 Loan Pools § 120.1722 SBA's offset rights. SBA shall have the right to offset any amount owed by Lender to SBA, including, without...

Fabrication of Mesoporous Silica/Alumina Hybrid Membrane Film Nanocomposites using Template Sol-Gel Synthesis of Amphiphilic Triphenylene

Science.gov (United States)

Lintang, H. O.; Jalani, M. A.; Yuliati, L.; Salleh, M. M.

2017-05-01

Herein we reported that by introducing a one-dimensional (1D) substrate with a porous structure such as anodic aluminum oxide (AAO) membrane, mesoporous silica/alumina hybrid nanocomposites were successfully fabricated by using amphiphilic triphenylene (TPC10TEG) as a template in sol-gel synthesis (TPC10TEG/silicahex). For the optical study of the nanocomposites, TPC10TEG/silicahex showed absorption peak at 264 nm due to the ordered and long-range π-π stacking of the disc-like aromatic triphenylene core. Moreover, the hexagonal arrangement of TPC10TEG/silicahex was proven based on their diffraction peaks of d 100 and d 200 at 2θ = 2.52° and 5.04° and images of transmission electron microscopy (TEM), respectively. For fabrication of mesoporous silica/alumina hybrid membrane, TPC10TEG/silicahex was drop-casted onto AAO membrane for penetration into the porous structure via gravity. X-ray diffraction (XRD) analysis on the resulted hybrid nanocomposites showed that the diffraction peaks of d 100 and d 200 of TPC10TEG/silicahex were still preserved, indicating that the hexagonal arrangements of mesoporous silica were maintained even on AAO substrate. The morphology study on the hybrid nanocomposites using TEM, scanning electron microscope (SEM) and field emission scanning electron microscope (FE-SEM) showed the successful filling of most AAO channels with the TPC10TEG/silicahex nanocomposites.

Functionalized nanostructured silica by tetradentate-amine chelating ligand as efficient heavy metals adsorbent : Applications to industrial effluent treatment

Energy Technology Data Exchange (ETDEWEB)

Shahbazi, Afsaneh [Shahid Beheshti University, Tehran (Iran, Islamic Republic of); Younesi, Habibollah [Tarbiat Modares University, Noor (Iran, Islamic Republic of); Badiei, Alireza [University of Tehran, Tehran (Iran, Islamic Republic of)

2014-09-15

Organofunctionalized nanostructured silica SBA-15 with tri(2-aminoethyl)amine tetradentate-amine ligand was synthesized and applied as adsorbent for the removal of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} from both synthetic wastewater and real paper mill and electroplating industrial effluents. The prepared materials were characterized by XRD, N{sub 2} adsorption-desorption, TGA, and FT-IR analysis. The Tren-SBA-15 was found to be a fast adsorbent for heavy metal ions from single solution with affinity for Cu{sup 2+}, Pb{sup 2+}, than for Cd{sup 2+} due to the complicated impacts of metal ion electronegativity. The kinetic rate constant decreased with increasing metal ion concentration due to increasing of ion repulsion force. The equilibrium batch experimental data is well described by the Langmuir isotherm. The maximum adsorption capacity was 1.85 mmol g{sup -1} for Cu{sup 2+}, 1.34 mmol g{sup -1} for Pb{sup 2+}, and 1.08 mmol g{sup -1} for Cd{sup 2+} at the optimized adsorption conditions (pH=4, T=323 K, t=2 h, C0=3 mmol L{sup -1}, and adsorbent dose=1 g L{sup -1}). All Gibbs energy was negative as expected for spontaneous interactions, and the positive entropic values from 103.7 to 138.7 J mol{sup -1} K{sup -1} also reinforced this favorable adsorption process in heterogeneous system. Experiment with real wastewaters showed that approximately a half fraction of the total amount of studied metal ions was removed within the first cycle of adsorption. Hence, desorption experiments were performed by 0.3M HCl eluent, and Tren-SBA-15 successfully reused for four adsorption/desorption cycles to complete removal of metal ions from real effluents. The regenerated Tren-SBA-15 displayed almost similar adsorption capacity of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} even after four recycles. The results suggest that Tren-SBA-15 is a good candidate as an adsorbent in the removal of Cu{sup 2+}, Pb{sup 2+}, and Cd{sup 2+} from aqueous solutions.

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials

Directory of Open Access Journals (Sweden)

Peter Hesemann

2014-04-01

Full Text Available The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA, mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

Comparative study of the porosity induced by CTAB and Tween as silica templates

International Nuclear Information System (INIS)

Cardinal, M.F.; Lovino, M.; Bernik, D.L.

2007-01-01

In this study doped-silicon polymers were synthesized using the non-ionic surfactant Tween 80 as template. The obtained material was compared with silicates doped with the cationic surfactant CTAB. Both materials were synthesized by sol-gel process with tetraethoxysilane (TEOS) as silicon source. In the synthesis procedure reported herein the main difference to previous reports is that the obtained solids were dried smoothly at 55 o C avoiding surfactant calcination. The aim of this work is to obtain new biomaterials appropriate to be used for encapsulation devices in which the surfactant kept within the silica network has two roles: (1) to improve the mechanical resistance in drying-swelling processes preventing crack formation (2) to hold and protect the encapsulated molecules keeping intact their bioactivity during TEOS polymerization. Structural features such as pore size and surface topology were studied by means of N 2 adsorption, X-ray diffraction and AFM microscopy. The influence of surfactant net charge and molecular shape on the materials obtained is discussed

13 CFR 120.462 - What are SBA's additional requirements on capital maintenance for SBA Supervised Lenders?

Science.gov (United States)

2010-01-01

... capital that each SBA Supervised Lender must maintain to protect against the credit risk and other general... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false What are SBA's additional requirements on capital maintenance for SBA Supervised Lenders? 120.462 Section 120.462 Business Credit and...

Insignificant influence of the matrix on the melting of ice confined in decorated mesoporous silica

Science.gov (United States)

Xu, Yunbo; Zhao, Zhenyan; Wang, Lianwen

2018-01-01

For a critical examination of matrix effect on the melting of confined ice, mesoporous silica (SBA-15) are synthesised and decorated with n-Alkyl and aminopropyl groups to tune the surface hydrophobicity. Water contact angle to these decorated surfaces are estimated to be about 100° and 60°, respectively. By examining the melting of ice confined in these decorated samples, we find that the influence of the matrix is indeed not significant. The reported apparent matrix effect is more likely method effect in the determination of pore diameters as was demonstrated in our previous studies (Philos. Mag. 93 (2013), p. 1827).

Characterization of silica particles prepared via urease-catalyzed urea hydrolysis and activity of urease in sol–gel silica matrix

International Nuclear Information System (INIS)

Kato, Katsuya; Nishida, Masakazu; Ito, Kimiyasu; Tomita, Masahiro

2012-01-01

Highlights: ► Silica precipitation occurred via urease-catalytic reactions. ► Higher urease activity for silica synthesis enables mesostructure of silica–urease composites. ► Urease encapsulating in silica matrix retained high activity. - Abstract: Urease templated precipitation of silica synthesized by sol–gel chemistry produces a composite material allowing high urease activity. This study investigates the structural properties of the composite material that allow for the retention of the urease hydrolysis activity. Scanning (SEM) and transmission (TEM) electron microscopy reveal that the composite has a mesoporous structure composed of closely packed spherical structures ∼20–50 nm in diameter. Brunauer–Emmett–Teller (BET) analysis revealed that the surface area and pore volume of the composite prepared under the conditions of 50 mM urea and 25 °C is relatively high (324 m 2 /g and 1.0 cm 3 /g). These values are equivalent to those of usual mesoporous silica materials synthesized from the self-assembly of triblock copolymers as organic templates. In addition, after encapsulating in a sol–gel silica matrix, urease retained high activity (∼90% of the activity compared with native urease). Our results suggest a new method for synthesizing mesoporous silica materials with highly tunable pore sizes and shapes under mild conditions.

CO2 activation through silylimido and silylamido zirconium hydrides supported on N-donor chelating SBA15 surface ligand

KAUST Repository

Pasha, Fahran Ahmad

2016-01-04

Density functional theory calculations and 2D 1H-13C HETCOR solid state NMR spectroscopy prove that CO2 can probe, by its own reactivity, different types of N-donor surface ligands on SBA15-supported ZrIV hydrides: [(≡Si-O-)(≡Si-N=)[Zr]H] and [(≡Si-NH-)(≡Si-X-)[Zr]H2] (X = O or NH). Moreover, [(≡Si-O-)(≡Si-N=)[Zr]H] activates CO2 more efficiently than the other complexes and leads to a carbimato Zr formate.

Conductivity of liquid lithium electrolytes with dispersed mesoporous silica particles

International Nuclear Information System (INIS)

Sann, K.; Roggenbuck, J.; Krawczyk, N.; Buschmann, H.; Luerßen, B.; Fröba, M.; Janek, J.

2012-01-01

Highlights: ► The conductivity of disperse lithium electrolytes with mesoporous fillers is studied. ► In contrast to other investigations in literature, no conductivity enhancement could be observed for standard battery electrolytes and typical mesoporous fillers in various combinations. ► Disperse electrolytes can become relevant in terms of battery safety. ► Dispersions of silicas and electrolyte with LiPF 6 as conducting salt are not stable, although the silicas were dried prior to preparation and the electrolyte water content was controlled. Surface modification of the fillers improved the stability. ► The observed conductivity decrease varied considerably for various fillers. - Abstract: The electrical conductivity of disperse electrolytes was systematically measured as a function of temperature (0 °C to 60 °C) and filler content for different types of fillers with a range of pore geometry, pore structure and specific surface area. As fillers mesoporous silicas SBA-15, MCM-41 and KIT-6 with pore ranges between 3 nm and 15 nm were dispersed in commercially available liquid lithium electrolytes. As electrolytes 1 M of lithium hexafluorophosphate (LiPF 6 ) in a mixture of ethylene carbonate (EC) and diethylene carbonate (DEC) at the ratio 3:7 (wt/wt) and the same solvent mixture with 0.96 M lithium bis(trifluoromethanesulfon)imide (LiTFSI) were used. No conductivity enhancement could be observed, but with respect to safety aspects the highly viscous disperse pastes might be useful. The conductivity decrease varied considerably for the different fillers.

Selective production of oxygenates from CO2 hydrogenation over mesoporous silica supported Cu-Ga nanocomposite catalyst

KAUST Repository

Huang, Kuo-Wei

2017-11-23

Carbon dioxide hydrogenation to oxygenates (methanol and dimethyl ether (DME)) was investigated over bifunctional supported copper catalysts promoted with gallium (Ga). Supported Cu-Ga nanocomposite catalysts were characterized by X-ray diffraction, transmission electron microscopy with energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and H2 temperature programmed reduction. In comparison with Cu-SBA-15 based catalysts, Ga promoted catalysts prepared by the urea deposition method (CuGa/SBA-15-UDP) was found active and selective for CO2 hydrogenation to oxygenates. The use of Ga as the promoter showed increased acidic sites as confirmed by the NH3-TPD, Pyridine-IR and 2,6-lutidine-IR studies. The favorable effect of Ga on CO2 conversion and selectivity to oxygenate may come from the strong interaction of Ga with silica, which is responsible for the enhanced metal surface area, formation of nanocomposite and metal dispersion. Notably, incorporation of Ga to Cu/SiO2 showed a several-fold higher rate for methanol formation (13.12 mol/gCu·sec) with a reasonable rate for the DME formation (2.15 mol/gCu·sec) as compared to those of Cu/SiO2 catalysts.

A facile template method to synthesize significantly improved LiNi0.5Mn1.5O4 using corn stalk as a bio-template

International Nuclear Information System (INIS)

Liu, Guiyang; Kong, Xin; Sun, Hongyan; Wang, Baosen; Yi, Zhongzhou; Wang, Quanbiao

2014-01-01

In order to simplify the template method for the synthesis of cathode materials for lithium ion batteries, a facile template method using plant stalks as bio-templates has been introduced. Based on this method, LiNi 0.5 Mn 1.5 O 4 spinel with a significantly improved electrochemical performance has been synthesized using corn stalk as a template. X-ray diffraction (XRD), Fourier transform infrared pectroscopy (FTIR) and scanning electron microscope (SEM) have been used to investigate the phase composition and micro-morphologies of the products. Charge-discharge measurements in lithium cells, cyclic voltammetry (CV) and Electrochemical impedance spectroscopy (EIS) have been used to study the electrochemical performance of the products. The results indicate that the templated product exhibits higher crystallinity than that of non-templated product. Both of the templated product and the non-templated product are combination of the ordered space group P4 3 32 and the disordered Fd-3 m. The specific BET surface area of the templated product is about twice larger than that of the non-templated product. Moreover, the electrochemical performances of the templated product including specific capacity, cycling stability and rate capability are significantly improved as compared with the non-templated product, due to its higher crystallinity, larger Li + diffusion coefficient and lower charge transfer resistance

Preparation, characterization and catalytic activity of mesoporous Ag2HPW12O40/SBA-15 and Ag2HPW12O40/TiO2 composites

International Nuclear Information System (INIS)

Holclajtner-Antunović, Ivanka; Bajuk-Bogdanović, Danica; Popa, Alexandru; Sasca, Viorel; Nedić Vasiljević, Bojana; Rakić, Aleksandra; Uskoković-Marković, Snežana

2015-01-01

The current study reports the synthesis and characterization of tungstophosphoric acid and its acid silver salt supported on mesoporous molecular sieve SBA-15 and TiO 2 . Because silver salts are partially insoluble, the SBA-15 and TiO 2 supported silver acid salts were prepared by two step sequential impregnations. The synthesized catalysts were characterized by various physicochemical methods such as Fourier transform infrared and Raman spectroscopy, differential thermal analysis, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and nitrogen physisorption at −196 °C. It is observed that both active phases keep their Keggin-type structure after being supported on the supports while their specific surface area is considerably increased by deposition on mesoporous substrates. The results also indicated that the synthesized catalysts retained the morphology specific for each of the supports, while their thermal stability is increased in comparison with their active phases. The catalytic activity of the prepared catalysts was probed for the vapor phase dehydration of ethanol at 300 °C. Results revealed that all the catalysts show considerably improved catalytic activity in comparison to the bulk active phases. - Highlights: • SBA-15 and TiO 2 supported Ag 2 HPW 12 O 40 and H 3 PW 12 O 40 were prepared. • Active phases are uniformly dispersed without changing morphology of the substrates. • Composites are more thermally stable than active phases. • Composites exhibit high catalytic activity for gas phase ethanol dehydration

13 CFR 120.460 - What are SBA's additional requirements for SBA Supervised Lenders?

Science.gov (United States)

2010-01-01

... company and does not have its own board of directors) must adopt an internal control policy which provides... the SBA Supervised Lender regulations that follow. (b) Operations and internal controls. Each SBA... operations, programs, and resources. The internal control policy must, at a minimum: (1) Direct management to...

Heat storage properties of organic phase-change materials confined in the nanospace of mesoporous SBA-15 and CMK-3.

Science.gov (United States)

Kadoono, Tomosuke; Ogura, Masaru

2014-03-28

A novel type of material encapsulating phase-change materials (PCMs) is reported concerning their implication for use as thermal energy storage devices. The composites of siliceous SBA-15 or carbonaceous CMK-3 mesoporous assemblies and organic PCMs could be used to make leak-free devices that retain their capabilities over many thermal cycles for heat storage/release. A confinement effect was observed that alters the thermal properties of the encapsulated PCM, especially in CMK-3 without any similar effects in other carbon materials.

Spectroscopy of nanosized composites silicon-organic polymer/nanoporous silicas

International Nuclear Information System (INIS)

Ostapenko, N.; Kozlova, N.; Suto, S.; Watanabe, A.

2006-01-01

Fluorescence and excitation spectra (T=5-290 K) of nanosized silicon-organic polymers poly(di-n-hexylsilane) and poly(methyl(phenyl)silane) incorporated into porous silica materials MCM-41 and SBA-15 have been studied with varying pore diameter from 2.8 to 10 nm. The controlled variation of the pore diameter in a wide range (2.8-10 nm) permitted us, for the first time, to investigate the optical properties of the polymers on their transition from isolated macromolecules to a film. It is found that this transition depends on polymer type and occurs via the formation of new spatially independent structures of the polymers not observed in the spectra of the film, namely, via the formation of disordered and (or) ordered conformations of polymer chains and clusters

Thiol-functionalized silica colloids, grains, and membranes for irreversible adsorption of metal(oxide) nanoparticles

NARCIS (Netherlands)

Claesson, E.M.; Philipse, A.P.

2007-01-01

Thiol-functionalization is described for silica surfaces from diverging origin, including commercial silica nanoparticles and St¨ober silica as well as silica structures provided by porous glasses and novel polymer-templated silica membranes. The functionalization allows in all cases for the

Multi-template synthesis of hierarchically porous carbon spheres with potential application in supercapacitors

NARCIS (Netherlands)

Zhou, Weizheng; Lin, Zhixing; Tong, Gangsheng; Stoyanov, Simeon D.; Yan, Deyue; Mai, Yiyong; Zhu, Xinyuan

2016-01-01

A new and simple multi-template approach towards hierarchical porous carbon (HPC) materials was reported. HPC spheres were prepared by using hierarchical silica capsules (HSCs) as the hard template and triblock copolymer Pluronic P123 as the soft template. Three types of pores were tunably

Temperature dependence of positron lifetime in ordered porous silica (SBA-3)

International Nuclear Information System (INIS)

Kunishige, S.; Koshimizu, M.; Asai, K.

2009-01-01

The temperature dependence of positron lifetime in uniform mesopores was analyzed. We used SBA-3 as the sample material, which possesses an ordered porous structure with uniform cylindrical mesopores. The positron lifetime corresponding to the annihilation in the mesopores increased gradually with a decrease in temperature down to 100 K, and its relative intensity also increased concomitantly. This result was attributed to the lower probability of the escape of the ortho-positronium (o-Ps) from the mesopores into the intergrain space at lower temperatures. An anomalous and sudden increase in the lifetime was observed at around 100 K; this result was in agreement with an increase in the positron lifetime reported in a previous study. It was revealed that the increase in the lifetime is very steep in cases of uniform mesopores, suggesting that the temperature dependence is influenced by the pore size.

13 CFR 120.1721 - SBA's right to investigate.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA's right to investigate. 120... Establishment of SBA Secondary Market Guarantee Program for First Lien Position 504 Loan Pools § 120.1721 SBA's right to investigate. SBA may undertake such investigation as it deems necessary to determine whether it...

Synthesis of cobalt-containing mesoporous catalysts using the ultrasonic-assisted “pH-adjusting” method: Importance of cobalt species in styrene oxidation

Energy Technology Data Exchange (ETDEWEB)

Li, Baitao, E-mail: btli@scut.edu.cn; Zhu, Yanrun; Jin, Xiaojing

2015-01-15

Cobalt-containing SBA-15 and MCM-41 (Co-SBA-15 and Co-MCM-41) mesoporous catalysts were prepared via ultrasonic-assisted “pH-adjusting” technique in this study. Their physiochemical structures were comprehensively characterized and correlated with catalytic activity in oxidation of styrene. The nature of cobalt species depended on the type of mesoporous silica as well as pH values. The different catalytic performance between Co-SBA-15 and Co-MCM-41 catalysts originated from cobalt species. Cobalt species were homogenously incorporated into the siliceous framework of Co-SBA-15 in single-site Co(II) state, while Co{sub 3}O{sub 4} particles were loaded on Co-MCM-41 catalysts. The styrene oxidation tests showed that the single-site Co(II) state was more beneficial to the catalytic oxidation of styrene. The higher styrene conversion and benzaldehyde selectivity over Co-SBA-15 catalysts were mainly attributed to single-site Co(II) state incorporated into the framework of SBA-15. The highest conversion of styrene (34.7%) with benzaldehyde selectivity of 88.2% was obtained over Co-SBA-15 catalyst prepared at pH of 7.5, at the mole ratio of 1:1 (styrene to H{sub 2}O{sub 2}) at 70 °C. - Graphical abstract: Cobalt-containing mesoporous silica catalysts were developed via ultrasonic-assisted “pH-adjusting” technique. Compared with Co{sub 3}O{sub 4} in Co-MCM-41, the single-site Co(II) state in Co-SBA-15 was more efficient for the styrene oxidation. - Highlights: • Fast and cost-effective ultrasonic technique for preparing mesoporous materials. • Incorporation of Co via ultrasonic irradiation and “pH-adjusting”. • Physicochemical comparison between Co-SBA-15 and Co-MCM-41. • Correlation of styrene oxidation activity and catalyst structural property.

Study of Catalyst, Aging Time and Surfactant Effects on Silica Inorganic Polymer Characteristics

Directory of Open Access Journals (Sweden)

M. Pakizeh

2007-06-01

Full Text Available In the present study the sol-gel method is used for synthesis of amorphous nanostructure silica polymer using tetraethoxysilane (TEOS as silicon source. This polymer can be used in manufacturing of nanoporous asymmetricmembranes. The effect of catalyst on silica particle size has been studied under acidic and basic conditions.زAcid-catalyzed reaction leads to the formation of fine particles while the base-catalyzed reaction produceslarger particles. The presence of cationic template surfactant namely cetyl pyridinium bromide (CPBزdirects the structural formation of the polymer by preventing the highly branched polymeric clusters. This will increase the effective area of the produced silica membrane. Nitrogen physisorption tests by Brunaver- Emmett-Teller (BET and Barrett-Joyner-Halenda (BJH methods revealed that the surface area of the membrane increases significantly around 5-folds when acid-catalyzed reaction is used. 29Si-NMR test is also used to study the aging time effect on the level of silica polymer branching. The results show that in acidic condition, aging time up to three weeks can still affect branching. The calcinations process in which the organic materials and CPB (surfactant are burned and released from the silica particles, is studied on template free silica materials as well as templated silica materials using TGA and DTA techniques.

13 CFR 120.601 - SBA Secondary Market.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA Secondary Market. 120.601 Section 120.601 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Secondary Market Fiscal and Transfer Agent (fta) § 120.601 SBA Secondary Market. The SBA secondary market...

One-step synthesis of dye-incorporated porous silica particles

Energy Technology Data Exchange (ETDEWEB)

Liu Qing; DeShong, Philip; Zachariah, Michael R., E-mail: mrz@umd.edu [University of Maryland, Department of Chemistry and Biochemistry (United States)

2012-07-15

Fluorescent nanoparticles have a variety of biomedical applications as diagnostics and traceable drug delivery agents. Highly fluorescent porous silica nanoparticles were synthesized in a water/oil phase by a microemulsion method. What is unique about the resulting porous silica nanoparticles is the combination of a single-step, efficient synthesis and the high stability of its fluorescence emission in the resulting materials. The key of the success of this approach is the choice of a lipid dye that functions as a surrogate surfactant in the preparation. The surfactant dye was incorporated at the interface of the inorganic silica matrix and organic environment (pore template), and thus insures the stability of the dye-silica hybrid structure. The resulting fluorescent silica materials have a number of properties that make them attractive for biomedical applications: the availability of various color of the resulting nanoparticle from among a broad spectrum of commercially dyes, the controllablity of pore size (diameters of {approx}5 nm) and particle size (diameters of {approx}40 nm) by adjusting template monomer concentration and the water/oil ratio, and the stability and durability of particle fluorescence because of the deep insertion of surfactant's tail into the silica matrix.

Mesoporous MEL, BEA, and FAU zeolite crystals obtained by in situ formation of carbon template over metal nanoparticles

DEFF Research Database (Denmark)

Abildstrøm, Jacob Oskar; Ali, Zahra Nasrudin; Mentzel, Uffe Vie

2016-01-01

Here, we report the synthesis and characterization of hierarchical zeolite materials with MEL, BEA and FAU structures. The synthesis is based on the carbon templating method with an in situ-generated carbon template. Through the decomposition of methane and deposition of coke over nickel nanopart......Here, we report the synthesis and characterization of hierarchical zeolite materials with MEL, BEA and FAU structures. The synthesis is based on the carbon templating method with an in situ-generated carbon template. Through the decomposition of methane and deposition of coke over nickel...... nanoparticles supported on silica, a carbon–silica composite is obtained and exploited as a combined carbon template/silica source for the zeolite synthesis. The mesoporous zeolite materials were all prepared by hydrothermal crystallization in alkaline media followed by removal of the carbon template...... by combustion, which results in zeolite single crystals with intracrystalline pore volumes of up to 0.44 cm3 g−1. The prepared zeolite structures are characterized by XRD, SEM, TEM and N2 physisorption measurements....

Synthetic opal as a template for nanostructured materials

Science.gov (United States)

White, Paul A.; Heales, Lindsey; Barber, Richard L.; Turney, Terence W.

2001-04-01

Synthetic opal has been used as a template for making 3D inverse opals of silica, titania and silicone rubber. The materials are mesoporous with connected pores and channels and have better opalescence than the opal templates they replace. Thin films of synthetic opal have been grown onto glass substrates by spin coating and these have also been used as templates for making thin films of inverse opal and as masks for depositing metal nanodots. This method produced hexagonally patterned 50 nm gold dots on a flat graphite substrate.

Silica biomineralization via the self-assembly of helical biomolecules.

Science.gov (United States)

Liu, Ben; Cao, Yuanyuan; Huang, Zhehao; Duan, Yingying; Che, Shunai

2015-01-21

The biomimetic synthesis of relevant silica materials using biological macromolecules as templates via silica biomineralization processes attract rapidly rising attention toward natural and artificial materials. Biomimetic synthesis studies are useful for improving the understanding of the formation mechanism of the hierarchical structures found in living organisms (such as diatoms and sponges) and for promoting significant developments in the biotechnology, nanotechnology and materials chemistry fields. Chirality is a ubiquitous phenomenon in nature and is an inherent feature of biomolecular components in organisms. Helical biomolecules, one of the most important types of chiral macromolecules, can self-assemble into multiple liquid-crystal structures and be used as biotemplates for silica biomineralization, which renders them particularly useful for fabricating complex silica materials under ambient conditions. Over the past two decades, many new silica materials with hierarchical structures and complex morphologies have been created using helical biomolecules. In this review, the developments in this field are described and the recent progress in silica biomineralization templating using several classes of helical biomolecules, including DNA, polypeptides, cellulose and rod-like viruses is summarized. Particular focus is placed on the formation mechanism of biomolecule-silica materials (BSMs) with hierarchical structures. Finally, current research challenges and future developments are discussed in the conclusion. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of silica-sustained electrospun polyvinylpyrrolidone fibers with uniform mesopores via oxidative removal of template molecules by H2O2 treatment

International Nuclear Information System (INIS)

Kang, Haigang; Zhu, Yihua; Shen, Jianhua; Yang, Xiaoling; Chen, Cheng; Cao, Huimin; Li, Chungzhong

2010-01-01

Silica-sustained electrospun PVP fibers with uniform mesopores were synthesized via facile oxidative removal of template molecules by H 2 O 2 extraction. Tetraethyl orthosilicate, polyvinylpyrrolidone (PVP), and triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer pluronic P 123 compose the electrospinning sol to fabricate the silica-sustained PVP hybrid fibers. The effect of different post-treatment methods on the pore size distribution was investigated by calcination and extraction, respectively. Experimental results showed that oxidative removal of structure-directing agent P 123 in the hybrid fibers by H 2 O 2 treatment can easily form narrow pore size distribution, and the incorporation of 3D silica skeleton built by hot steam aging facilitated preserving the original cylindrical morphology of fibers. Scanning electron microscopy (SEM), N 2 adsorption-desorption isotherm, transmission electron microscopy (TEM), X-ray diffraction (XRD), FT-IR spectra and thermogravimetric analysis (TGA) were used to characterize the hybrid fibers. The hybrid fibers can be expected to have potential applications in drug release or tissue engineering because of their suitable pore size, large surface area and good biocompatibility.

Summary different routes for procurement of molecular sieves type AL-SBA-15

International Nuclear Information System (INIS)

Figueiroa, D.S.; Santos, J.O.P.N.; Medeiros, C.D.; Sousa, B.V.

2012-01-01

The search for new materials to assist industrial development, especially in the chemical industry has been growing more and more. Molecular sieves are great examples of these materials that aim the improvement of various chemical processes. The present work aimed to synthesize the molecular sieve Al-SBA-15 by two different synthesis procedures. In procedure A was used a temperature of 40°C for 24 hours during stirring process. For B process the stirring procedure was done at room temperature. The molar composition of reactants was: 1.0 SiO 2 : 0.04 Al 2 O 3 :0.0168 EO 20 PO 70 EO 20 : 5.85 HCl: 160 H 2 O. The pH of the reaction gel was adjusted to 7 and after the gel was putted under 100 deg C for 48 hours for the heat treatment. Then the sample was calcined under flowing air at 500° C for 6 hours. By techniques such as XRD and SEM, it was confirmed the formation of the hexagonal mesoporous structure, with an orderly distribution of its pores, also indicating the successful incorporation of aluminum into the hexagonal structure of the catalyst support. (author)

Preparation of ionic liquid-modified SBA-15 doped with molybdovanadophosphoric acid for oxidative desulfurization

International Nuclear Information System (INIS)

Zhuang, Jiang Zhou; Jin, Xiao Yin; Shen, Xian Lin; Tan, Jun Jun; Nie, Long Hui; Xiang, Jian; Hu, Bing

2015-01-01

A series of catalysts, ionic liquid-modified SBA-15 (denoted ILSBA) doped with H 5 PMo 10 V 2 O 40 (HPMoV 2 ) have been synthesized and characterized by XRD, FT-IR, 1 H NMR, TG-DTA, and TEM. The catalyst was used for the removal of dibenzothiophene (DBT) in model oil combined with hydrogen peroxide (the oxidant) and acetonitrile (the phase-transfer agent). It was observed that the sulfur content of DBT can be reduced from 500 to 2 ppm by adjusting the amount of catalyst, the reaction temperatures and the reaction time. Besides, the catalyst activity for different sulfur compounds showed a huge difference which may be mainly affected by the electron densities of sulfur atom. Moreover, the catalyst can be recycled seven times without a significant loss in activity, which could be ascribed to the strong electrostatic interaction between ILSBA and HPMoV 2 . In addition, a postulated mechanism was proposed to reveal the oxidative desulfurization process

13 CFR 106.500 - What is SBA's Gift authority?

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false What is SBA's Gift authority? 106... AND NON-FEE BASED SBA-SPONSORED ACTIVITIES AND GIFTS Gifts § 106.500 What is SBA's Gift authority? This section covers SBA's Gift acceptance authority under sections 4(g), 8(b)(1)(G), 5(b)(9) and 7(k)(2...

Low-cost route for synthesis of mesoporous silica materials with high silanol groups and their application for Cu(II) removal

International Nuclear Information System (INIS)

Wang Yangang; Huang Sujun; Kang Shifei; Zhang Chengli; Li Xi

2012-01-01

Graphical abstract: A simple and low-cost route to synthesize mesoporous silica materials with high silanol groups has been demonstrated by means of a sol–gel process using citric acid as the template and acid catalyst, further studies on the adsorption of Cu(II) onto the representative amine-functionalized mesoporous silica showed that it had a high Cu(II) removal efficiency. Highlights: ► A low-cost route to synthesize mesoporous silica with high silanol groups was demonstrated. ► Citric acid as the template and acid catalyst for the reaction of tetraethylorthosilicate. ► Water extraction method was an effective technique to remove template which can be recycled. ► The mesoporous silica with high silanol groups was easily modified by functional groups. ► A high Cu(II) removal efficiency on the amine-functionalized mesoporous silica. - Abstract: We report a simple and low-cost route for the synthesis of mesoporous silica materials with high silanol groups by means of a sol–gel process using citric acid as the template, tetraethylorthosilicate (TEOS) as the silica source under aqueous solution system. The citric acid can directly work as an acid catalyst for the hydrolysis of TEOS besides the function as a pore-forming agent in the synthesis. It was found that by using a water extraction method the citric acid template in as-prepared mesoporous silica composite can be easily removed and a high degree of silanol groups were retained in the mesopores, moreover, the citric acid template in the filtrate can be recycled after being dried. The structural properties of the obtained mesoporous silica materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and nitrogen adsorption–desorption analysis. Furthermore, an adsorption of Cu(II) from aqueous solution on the representative amine-functionalized mesoporous silica was investigated

13 CFR 107.1720 - Characteristics of SBA's guarantee.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false Characteristics of SBA's guarantee. 107.1720 Section 107.1720 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION SMALL BUSINESS... Characteristics of SBA's guarantee. If SBA agrees to guarantee a Licensee's Debentures or Participating Securities...

Preparation of Al-SBA-15 Pellets with Low Amount of Additives: Effect of Binder Content on Texture and Mechanical Properties. Application to Friedel-Crafts Alkylation

Czech Academy of Sciences Publication Activity Database

Topka, Pavel; Karban, Jindřich; Soukup, Karel; Jirátová, Květa; Šolcová, Olga

2011-01-01

Roč. 168, č. 1 (2011), s. 433-440 ISSN 1385-8947 R&D Projects: GA ČR GA104/09/0694; GA AV ČR KAN400720701 Institutional research plan: CEZ:AV0Z40720504 Keywords : mesoporous aluminosilicates * pellets * Al-SBA-15 Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 3.461, year: 2011

Mesoporous silica nanotubes hybrid membranes for functional nanofiltration

International Nuclear Information System (INIS)

El-Safty, Sherif A; Shahat, Ahmed; Mekawy, Moataz; Nguyen, Hoa; Warkocki, Wojciech; Ohnuma, Masato

2010-01-01

The development of nanofiltration systems would greatly assist in the production of well-defined particles and biomolecules with unique properties. We report a direct, simple synthesis of hexagonal silica nanotubes (NTs), which vertically aligned inside anodic alumina membranes (AAM) by means of a direct templating method of microemulsion phases with cationic surfactants. The direct approach was used as soft templates for predicting ordered assemblies of surfactant/silica composites through strong interactions within AAM pockets. Thus, densely packed NTs were successfully formed in the entirety of the AAM channels. These silica NTs were coated with layers of organic moieties to create a powerful technique for the ultrafine filtration. The resulting modified-silica NTs were chemically robust and showed affinity toward the transport of small molecular particles. The rigid silica NTs inside AAM channels had a pore diameter of ≤ 4 nm and were used as ultrafine filtration systems for noble metal nanoparticles (NM NPs) and semiconductor nanocrystals (SC NCs) fabricated with a wide range of sizes (1.0-50 nm) and spherical/pyramidal morphologies. Moreover, the silica NTs hybrid membranes were also found to be suitable for separation of biomolecules such as cytochrome c (CytC). Importantly, this nanofilter design retains high nanofiltration efficiency of NM NPs, SC NCs and biomolecules after a number of reuse cycles. Such retention is crucial in industrial applications.

New insight into silica deposition in horsetail (Equisetum arvense

Directory of Open Access Journals (Sweden)

Exley Christopher

2011-07-01

Full Text Available Abstract Background The horsetails (Equisetum sp are known biosilicifiers though the mechanism underlying silica deposition in these plants remains largely unknown. Tissue extracts from horsetails grown hydroponically and also collected from the wild were acid-digested in a microwave oven and their silica 'skeletons' visualised using the fluor, PDMPO, and fluorescence microscopy. Results Silica deposits were observed in all plant regions from the rhizome through to the stem, leaf and spores. Numerous structures were silicified including cell walls, cell plates, plasmodesmata, and guard cells and stomata at varying stages of differentiation. All of the major sites of silica deposition in horsetail mimicked sites and structures where the hemicellulose, callose is known to be found and these serendipitous observations of the coincidence of silica and callose raised the possibility that callose might be templating silica deposition in horsetail. Hydroponic culture of horsetail in the absence of silicic acid resulted in normal healthy plants which, following acid digestion, showed no deposition of silica anywhere in their tissues. To test the hypothesis that callose might be templating silica deposition in horsetail commercially available callose was mixed with undersaturated and saturated solutions of silicic acid and the formation of silica was demonstrated by fluorimetry and fluorescence microscopy. Conclusions The initiation of silica formation by callose is the first example whereby any biomolecule has been shown to induce, as compared to catalyse, the formation of silica in an undersaturated solution of silicic acid. This novel discovery allowed us to speculate that callose and its associated biochemical machinery could be a missing link in our understanding of biosilicification.

Template-mediated, Hierarchical Engineering of Ordered Mesoporous Films and Powders

Science.gov (United States)

Tian, Zheng

Hierarchical control over pore size, pore topology, and meso/mictrostructure as well as material morphology (e.g., powders, monoliths, thin films) is crucial for meeting diverse materials needs among applications spanning next generation catalysts, sensors, batteries, sorbents, etc. The overarching goal of this thesis is to establish fundamental mechanistic insight enabling new strategies for realizing such hierarchical textural control for carbon materials that is not currently achievable with sacrificial pore formation by 'one-pot' surfactant-based 'soft'-templating or multi-step inorganic 'hard-templating. While 'hard'-templating is often tacitly discounted based upon its perceived complexity, it offers potential for overcoming key 'soft'-templating challenges, including bolstering pore stability, accommodating a more versatile palette of replica precursors, realizing ordered/spanning porosity in the case of porous thin films, simplifying formation of bi-continuous pore topologies, and inducing microstructure control within porous replica materials. In this thesis, we establish strategies for hard-templating of hierarchically porous and structured carbon powders and tunable thin films by both multi-step hard-templating and a new 'one-pot' template-replica precursor co-assembly process. We first develop a nominal hard-templating technique to successfully prepare three-dimensionally ordered mesoporous (3DOm) and 3DOm-supported microporous carbon thin films by exploiting our ability to synthesize and assemble size-tunable silica nanoparticles into scalable, colloidal crystalline thin film templates of tunable mono- to multi-layer thickness. This robust thin film template accommodates liquid and/or vapor-phase infiltration, polymerization, and pyrolysis of various carbon sources without pore contraction and/or collapse upon template sacrifice. The result is robust, flexible 3DOm or 3DOm-supported ultra-thin microporous films that can be transferred by stamp

Thermally stable silica-coated hydrophobic gold nanoparticles.

Science.gov (United States)

Kanehara, Masayuki; Watanabe, Yuka; Teranishi, Toshiharu

2009-01-01

We have successfully developed a method for silica coating on hydrophobic dodecanethiol-protected Au nanoparticles with coating thickness ranging from 10 to 40 nm. The formation of silica-coated Au nanoparticles could be accomplished via the preparation of hydrophilic Au nanoparticle micelles by cationic surfactant encapsulation in aqueous phase, followed by hydrolysis of tetraethylorthosilicate on the hydrophilic surface of gold nanoparticle micelles. Silica-coated Au nanoparticles exhibited quite high thermal stability, that is, no agglomeration of the Au cores could be observed after annealing at 600 degrees C for 30 min. Silica-coated Au nanoparticles could serve as a template to derive hollow nanoparticles. An addition of NaCN solution to silica-coated Au nanoparticles led the formation of hollow silica nanoparticles, which were redispersible in deionized water. The formation of the hollow silica nanoparticles results from the mesoporous structures of the silica shell and such a mesoporous structure is applicable to both catalyst support and drug delivery.

Novel Shape-Stabilized Phase Change Materials Composed of Polyethylene Glycol/Nonsurfactant-Templated Mesoporous Silica: Preparation and Thermal Properties

Science.gov (United States)

Chen, Yan; Zhu, Yingying; Wang, Jinbao; Lv, Mengjiao; Zhang, Xiongjie; Gao, Junkai; Zhang, Zijun; Lei, Hao

2017-12-01

A novel shape-stabilized phase change material (PEG/TAMS), fabricated using tannic acid-templated mesoporous silica (TAMS) as a support for polyethylene glycol, was developed for thermal energy storage. The method used to synthesize TAMS was simple, cost effective, environmentally friendly, and free of surfactant. The characterization results indicated that PEG was physically absorbed to TAMS and that TAMS had no influence on the crystal structure of PEG. According to the TGA thermograms, PEG/TAMS has excellent thermal stability and can be applied over a wide temperature range. Additionally, the differential scanning calorimetry results suggested that PEG/TAMS has good thermal properties and that its fusion and solidification enthalpies reached 114.7 J/g and 102.4 J/g, respectively. The results indicated that PEG/TAMS has great potential for practical applications.

Synthesis of porous carbon/silica nanostructured microfiber with ultrahigh surface area

Science.gov (United States)

Zhou, Dan; Dong, Yan; Cui, Liru; Lin, Huiming; Qu, Fengyu

2014-12-01

Carbon/silica-nanostructured microfibers were synthesized via electrospinning method using phenol-formaldehyde resin and tetraethyl orthosilicate as carbon and silica precursor with triblock copolymer Pluronic P123 as soft template. The prepared samples show uniform microfiber structure with 1 μm in diameter and dozens of microns in length. Additionally, the mesopores in the material is about 2-6 nm. When the silica component was removed by HF, the porous carbon microfibers (PCMFs) were obtained. In addition, after the carbon/silica composites were calcined in air, the porous silica microfibers (PSiMFs) were obtained, revealing the converse porous nanostructure as PCMFs. It is a simple way to prepare PCMFs and PSiMFs with silica and carbon as the template to each other. Additionally, PCMFs possess an ultrahigh specific surface area (2,092 m2 g-1) and large pore volume. The electrochemical performance of the prepared PCMF material was investigated in 6.0 M KOH electrolyte. The PCMF electrode exhibits a high specific capacitance (252 F g-1 at 0.5 A g-1). Then, superior cycling stability (97 % retention after 4,000 cycles) mainly is due to its unique nanostructure.

13 CFR 120.464 - Reports to SBA.

Science.gov (United States)

2010-01-01

... submit to SBA a summary of any changes in the SBA Supervised Lender's organization or financing (within... reasons and documentation. The waiver decision of the appropriate Office of Capital Access official in...

Effect of surface hydroxyl groups on heat capacity of mesoporous silica

Science.gov (United States)

Marszewski, Michal; Butts, Danielle; Lan, Esther; Yan, Yan; King, Sophia C.; McNeil, Patricia E.; Galy, Tiphaine; Dunn, Bruce; Tolbert, Sarah H.; Hu, Yongjie; Pilon, Laurent

2018-05-01

This paper quantifies the effect of surface hydroxyl groups on the effective specific and volumetric heat capacities of mesoporous silica. To achieve a wide range of structural diversity, mesoporous silica samples were synthesized by various methods, including (i) polymer-templated nanoparticle-based powders, (ii) polymer-templated sol-gel powders, and (iii) ambigel silica samples dried by solvent exchange at room temperature. Their effective specific heat capacity, specific surface area, and porosity were measured using differential scanning calorimetry and low-temperature nitrogen adsorption-desorption measurements. The experimentally measured specific heat capacity was larger than the conventional weight-fraction-weighted specific heat capacity of the air and silica constituents. The difference was attributed to the presence of OH groups in the large internal surface area. A thermodynamic model was developed based on surface energy considerations to account for the effect of surface OH groups on the specific and volumetric heat capacity. The model predictions fell within the experimental uncertainty.

Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

KAUST Repository

Werghi, Baraa; Bendjeriou-Sedjerari, Anissa; Jedidi, Abdesslem; Abou-Hamad, Edy; Cavallo, Luigi; Basset, Jean-Marie

2016-01-01

The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

Single-Site Tetracoordinated Aluminum Hydride Supported on Mesoporous Silica. From Dream to Reality!

KAUST Repository

Werghi, Baraa

2016-09-26

The reaction of mesoporous silica (SBA15) dehydroxylated at 700 °C with diisobutylaluminum hydride, i-Bu2AlH, gives after thermal treatment a single-site tetrahedral aluminum hydride with high selectivity. The starting aluminum isobutyl and the final aluminum hydride have been fully characterized by FT-IR, advanced SS NMR spectroscopy (1H, 13C, multiple quanta (MQ) 2D 1H-1H, and 27Al), and elemental analysis, while DFT calculations provide a rationalization of the occurring reactivity. Trimeric i-Bu2AlH reacts selectively with surface silanols without affecting the siloxane bridges. Its analogous hydride catalyzes ethylene polymerization. Indeed, catalytic tests show that this single aluminum hydride site is active in the production of a high-density polyethylene (HDPE). © 2016 American Chemical Society.

Preparation of ionic liquid-modified SBA-15 doped with molybdovanadophosphoric acid for oxidative desulfurization

Energy Technology Data Exchange (ETDEWEB)

Zhuang, Jiang Zhou; Jin, Xiao Yin; Shen, Xian Lin; Tan, Jun Jun; Nie, Long Hui; Xiang, Jian; Hu, Bing [Dept. of chool of Chemistry and Chemical Engineering, Hubei University of Technology, Wuhan (China)

2015-07-15

A series of catalysts, ionic liquid-modified SBA-15 (denoted ILSBA) doped with H{sub 5}PMo{sub 10}V{sub 2}O{sub 40} (HPMoV{sub 2}) have been synthesized and characterized by XRD, FT-IR, {sup 1}H NMR, TG-DTA, and TEM. The catalyst was used for the removal of dibenzothiophene (DBT) in model oil combined with hydrogen peroxide (the oxidant) and acetonitrile (the phase-transfer agent). It was observed that the sulfur content of DBT can be reduced from 500 to 2 ppm by adjusting the amount of catalyst, the reaction temperatures and the reaction time. Besides, the catalyst activity for different sulfur compounds showed a huge difference which may be mainly affected by the electron densities of sulfur atom. Moreover, the catalyst can be recycled seven times without a significant loss in activity, which could be ascribed to the strong electrostatic interaction between ILSBA and HPMoV{sub 2}. In addition, a postulated mechanism was proposed to reveal the oxidative desulfurization process.

Epoxy Crosslinked Silica Aerogels (X-Aerogels)

Science.gov (United States)

fabrizio, Eve; Ilhan, Faysal; Meador, Mary Ann; Johnston, Chris; Leventis, Nicholas

2004-01-01

NASA is interested in the development of strong lightweight materials for the dual role of thermal insulator and structural component for space vehicles; freeing more weight for useful payloads. Aerogels are very-low density materials (0.010 to 0.5 g/cc) that, due to high porosity (meso- and microporosity), can be, depending on the chemical nature of the network, ideal thermal insulators (thermal conductivity approx. 15 mW/mK). However, aerogels are extremely fragile. For practical application of aerogels, one must increase strength without compromising the physical properties attributed to low density. This has been achieved by templated growth of an epoxy polymer layer that crosslinks the "pearl necklace" network of nanoparticles: the framework of a typical silica aerogel. The requirement for conformal accumulation of the epoxy crosslinker is reaction both with the surface of silica and with itself. After cross-linking, the strength of a typical aerogel monolith increases by a factor of 200, in the expense of only a 2-fold increase in density. Strength is increased further by coupling residual unreacted epoxides with diamine.

Fast determination of Ziziphora tenuior L. essential oil by inorganic-organic hybrid material based on ZnO nanoparticles anchored to a composite made from polythiophene and hexagonally ordered silica.

Science.gov (United States)

Piryaei, Marzieh; Abolghasemi, Mir Mahdi; Nazemiyeh, Hossein

2015-01-01

In this paper, for the first time, an inorganic-organic hybrid material based on ZnO nanoparticles was anchored to a composite made from polythiophene and hexagonally ordered silica (ZnO/PT/SBA-15) for use in solid-phase fibre microextraction (SPME) of medicinal plants. A homemade SPME apparatus was used for the extraction of volatile components of Ziziphora tenuior L. A simplex method was used for optimisation of five different parameters affecting the efficiency of the extraction. The main constituents extracted by ZnO/PT/SBA-15 and PDMS fibres and hydrodistillation (HD) methods, respectively, included pulegone (51.25%, 53.64% and 56.68%), limonene (6.73%, 6.58% and 8.3%), caryophyllene oxide (5.33%, 4.31% and 4.53%) and 1,8-cineole (4.21%, 3.31% and 3.18%). In comparison with the HD method, the proposed technique could equally monitor almost all the components of the sample, in an easier way, in a shorter time and requiring a much lower amount of the sample.

13 CFR 120.395 - What is SBA's collateral position?

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false What is SBA's collateral position? 120.395 Section 120.395 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Special Purpose Loans Builders Loan Program § 120.395 What is SBA's collateral position? SBA will require...

Fabrication of highly hydrophobic two-component thermosetting polyurethane surfaces with silica nanoparticles

Science.gov (United States)

Yang, Guang; Song, Jialu; Hou, Xianghui

2018-05-01

Highly hydrophobic thermosetting polyurethane (TSU) surfaces with micro-nano hierarchical structures were developed by a simple process combined with sandpaper templates and nano-silica embellishment. Sandpapers with grit sizes varying from 240 to 7000 grit were used to obtain micro-scale roughness on an intrinsic hydrophilic TSU surface. The surface wettability was investigated by contact angle measurement. It was found that the largest contact angle of the TSU surface without nanoparticles at 102 ± 3° was obtained when the template was 240-grit sandpaper and the molding progress started after 45 min curing of TSU. Silica nanoparticles modified with polydimethylsiloxane were scattered onto the surfaces of both the polymer and the template to construct the desirable nanostructures. The influences of the morphology, surface composition and the silica content on the TSU surface wettability were studied by scanning electron microscopy (SEM), attenuated total reflection (ATR) infrared (IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and contact angle measurements. The surface of the TSU/SiO2 nanocomposites containing 4 wt% silica nanoparticles exhibited a distinctive dual-scale structure and excellent hydrophobicity with the contact angle above 150°. The mechanism of wettability was also discussed by Wenzel model and Cassie-Baxter model.

13 CFR 120.150 - What are SBA's lending criteria?

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false What are SBA's lending criteria... Policies Applying to All Business Loans Credit Criteria for Sba Loans § 120.150 What are SBA's lending... depth of management; (c) Strength of the business; (d) Past earnings, projected cash flow, and future...

Selective Hydrogenation of Furfural to Furfuryl Alcohol in the Presence of a Recyclable Cobalt/SBA-15 Catalyst.

Science.gov (United States)

Audemar, Maïté; Ciotonea, Carmen; De Oliveira Vigier, Karine; Royer, Sébastien; Ungureanu, Adrian; Dragoi, Brindusa; Dumitriu, Emil; Jérôme, François

2015-06-08

The hydrogenation of furfural to furfuryl alcohol was performed in the presence of a Co/SBA-15 catalyst. High selectivity (96 %) at a conversion higher than 95 % is reported over this catalytic system. As the conversion of furfural to furfuryl alcohol occurs over metallic Co sites, the effect of reduction temperature, H2 pressure, and reaction temperature were studied. Optimum reaction conditions were: 150 °C, 1.5 h, 2.0 MPa of H2 . The catalyst was recyclable, and furfuryl alcohol was recovered with a purity higher than 90 %. The effect of the solvent concentration was also studied. With a minimum of 50 wt % of solvent, the selectivity to furfuryl alcohol and the conversion of furfural remained high (both over 80 %). Likewise, the activity of the catalyst is maintained even in pure furfural, which confirms the real potential of the proposed catalytic system. This catalyst was also used in the hydrogenation of levulinic acid to produce γ-valerolactone selectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of polymer matrix and adsorption onto silica materials on the migration of alpha-tocopherol into 95% ethanol from active packaging.

Science.gov (United States)

Heirlings, L; Siró, I; Devlieghere, F; Van Bavel, E; Cool, P; De Meulenaer, B; Vansant, E F; Debevere, J

2004-11-01

In this study, the effect of polymer materials with different polarity, namely low density polyethylene (LDPE) and ethylene vinyl acetate (EVA), on the migration behaviour of alpha-tocopherol from active packaging was investigated. The antioxidant was also adsorbed onto silica materials, namely SBA-15 (Santa Barbara-15) and Syloblock, in order to protect the antioxidant during extrusion and to ensure a controlled and sufficient release during the shelf-life of the food product. Migration experiments were performed at 7.0 +/- 0.5 degrees C and 95% ethanol was used as fatty food simulant. All films contained a high concentration of alpha-tocopherol, approximately 2000 mg kg(-1), to obtain an active packaging. Polymer matrix had a small influence on the migration profile. The migration of 80% of total migrated amount of antioxidant was retarded for 2.4 days by using LDPE instead of EVA. When alpha-tocopherol was adsorbed onto both silica materials, the migration of 80% of total migrated amount of antioxidant was retarded for 3.4 days in comparison to pure alpha-tocopherol. No difference was seen between the migration profiles of alpha-tocopherol adsorbed onto both silica materials. In the case of pure alpha-tocopherol, 82% of the initial amount of alpha-tocopherol in the film migrated into the food simulant at a rather fast migration rate. In the case of adsorption on silica materials, a total migration was observed. These antioxidative films can have positive food applications.

Synthesis of porous carbon/silica nanostructured microfiber with ultrahigh surface area

Energy Technology Data Exchange (ETDEWEB)

Zhou, Dan; Dong, Yan; Cui, Liru; Lin, Huiming, E-mail: hiuminglin@gmail.com; Qu, Fengyu, E-mail: qufengyu2012@yahoo.cn, E-mail: qufengyu@hrbnu.edu.cn [Harbin Normal University, College of Chemistry and Chemical Engineering (China)

2014-12-15

Carbon/silica-nanostructured microfibers were synthesized via electrospinning method using phenol-formaldehyde resin and tetraethyl orthosilicate as carbon and silica precursor with triblock copolymer Pluronic P123 as soft template. The prepared samples show uniform microfiber structure with ∼1 μm in diameter and dozens of microns in length. Additionally, the mesopores in the material is about 2–6 nm. When the silica component was removed by HF, the porous carbon microfibers (PCMFs) were obtained. In addition, after the carbon/silica composites were calcined in air, the porous silica microfibers (PSiMFs) were obtained, revealing the converse porous nanostructure as PCMFs. It is a simple way to prepare PCMFs and PSiMFs with silica and carbon as the template to each other. Additionally, PCMFs possess an ultrahigh specific surface area (2,092 m{sup 2} g{sup −1}) and large pore volume. The electrochemical performance of the prepared PCMF material was investigated in 6.0 M KOH electrolyte. The PCMF electrode exhibits a high specific capacitance (252 F g{sup −1} at 0.5 A g{sup −1}). Then, superior cycling stability (97 % retention after 4,000 cycles) mainly is due to its unique nanostructure.

Topotactic conversion of layered silicate RUB-15 to silica sodalite through interlayer condensation in N-methylformamide.

Science.gov (United States)

Koike, Masakazu; Asakura, Yusuke; Sugihara, Megumi; Kuroda, Yoshiyuki; Tsuzura, Hidehiro; Wada, Hiroaki; Shimojima, Atsushi; Kuroda, Kazuyuki

2017-08-08

Silica sodalite was obtained using topotactic conversion of layered silicate RUB-15 through stepwise processes that consisted of the control of stacking sequence of the layers, interlayer condensation by refluxing, and elimination of intercalated guest species. The interlayer condensation of RUB-15, in which acetic acid was pre-intercalated between the layers to control the stacking sequence, afforded a sodalite framework containing organic guest species by refluxing in N-methylformamide (NMF). The pre-intercalated acetic acid molecules were largely replaced with NMF. This formation process of silica sodalite containing large amounts of intercalated organic guest species is in clear contrast to the previously reported process that used direct calcination of an intercalation compound of layered RUB-15 accommodating acetic acid between the layers. Calcination of the condensed product provided sodalite with fewer defects than the directly calcined product, thus indicating the advantage of the stepwise process. The method reported here is useful for the preparation of pure silica sodalite with relatively low defects and plate-like morphology.

Preparation and characterization of monodisperse large-porous silica microspheres as the matrix for protein separation.

Science.gov (United States)

Xia, Hongjun; Wan, Guangping; Zhao, Junlong; Liu, Jiawei; Bai, Quan

2016-11-04

High performance liquid chromatography (HPLC) is a kind of efficient separation technology and has been used widely in many fields. Micro-sized porous silica microspheres as the most popular matrix have been used for fast separation and analysis in HPLC. In this paper, the monodisperse large-porous silica microspheres with controllable size and structure were successfully synthesized with polymer microspheres as the templates and characterized. First, the poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) microspheres (P GMA-EDMA ) were functionalized with tetraethylenepentamine (TEPA) to generate amino groups which act as a catalyst in hydrolysis of tetraethyl orthosilicate (TEOS) to form Si-containing low molecular weight species. Then the low molecular weight species diffused into the functionalized P GMA-EDMA microspheres by induction force of the amino groups to form polymer/silica hybrid microspheres. Finally, the organic polymer templates were removed by calcination, and the large-porous silica microspheres were obtained. The compositions, morphology, size distribution, specific surface area and pore size distribution of the porous silica microspheres were characterized by infrared analyzer, scanning-electron microscopy, dynamic laser scattering, the mercury intrusion method and thermal gravimetric analysis, respectively. The results show that the agglomeration of the hybrid microspheres can be overcome when the templates were functionalized with TEPA as amination reagent, and the yield of 95.7% of the monodisperse large-porous silica microspheres can be achieved with high concentration of polymer templates. The resulting large-porous silica microspheres were modified with octadecyltrichlorosilane (ODS) and the chromatographic evaluation was performed by separating the proteins and the digest of BSA. The baseline separation of seven kinds of protein standards was achieved, and the column delivered a better performance when separating BSA digests

13 CFR 120.434 - What are SBA's requirements for loan pledges?

Science.gov (United States)

2010-01-01

... satisfactory SBA performance, as determined by SBA in its discretion. The Lender's Risk Rating, among other... BUSINESS LOANS Lenders Other Conveyances § 120.434 What are SBA's requirements for loan pledges? (a) Except... 7(a) loan, which consent SBA may withhold in its sole discretion; (b) The Lender must be in good...

Microporous Silica Based Membranes for Desalination

Directory of Open Access Journals (Sweden)

João C. Diniz da Costa

2012-09-01

Full Text Available This review provides a global overview of microporous silica based membranes for desalination via pervaporation with a focus on membrane synthesis and processing, transport mechanisms and current state of the art membrane performance. Most importantly, the recent development and novel concepts for improving the hydro-stability and separating performance of silica membranes for desalination are critically examined. Research into silica based membranes for desalination has focussed on three primary methods for improving the hydro-stability. These include incorporating carbon templates into the microporous silica both as surfactants and hybrid organic-inorganic structures and incorporation of metal oxide nanoparticles into the silica matrix. The literature examined identified that only metal oxide silica membranes have demonstrated high salt rejections under a variety of feed concentrations, reasonable fluxes and unaltered performance over long-term operation. As this is an embryonic field of research several target areas for researchers were discussed including further improvement of the membrane materials, but also regarding the necessity of integrating waste or solar heat sources into the final process design to ensure cost competitiveness with conventional reverse osmosis processes.

Preparation of Mesoporous Carbons from Acrylonitrile-methyl Methacrylate Copolymer/Silica Nanocomposites Synthesized by in-situ Emulsion Polymerization

Institute of Scientific and Technical Information of China (English)

BAO Yongzhong; ZHAO Wenting; HUANG Zhiming

2013-01-01

Acrylonitrile-methyl methacrylate (AN-MMA) copolymer/silica nanocomposites were synthesized by in-situ emulsion polymerization initiated by 2,2′-azobis(2-amidinopropane) dihydrochloride absorbed onto colloidal silica particles,and the mesoporous carbon materials were prepared through carbonization of the obtained AN-MMA copolymer/silica nanocomposites,followed by HF etching.Thermogravimetric analysis of AN-MMA copolymer/silica nanocomposites showed that the carbon yield of copolymer was slightly decreased as silica particle incorporated.N2 adsorption-desorption,scan electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and morphology of the mesoporous carbon materials.Both SEM and TEM results showed that disordered mesopores were formed in the obtained carbon material mainly through templating effect of silica nanoparticles.The diameter of mesopores was mainly distributed in the range from 5 nm to 15 nm.The mean pore diameter and total pore volume of the material increased as the mass fraction of silica in the nanocomposites increased from 0 to 24.93％.The significant increase of the mean pore diameter and the decrease of surface area for the carbon material prepared from the nanocomposite with 24.93％ silica were caused by partial aggregation of silica nanoparticles in the polymer matrix.

Comparison of different mesoporous silicas for off-line solid phase extraction of 17β-estradiol from waters and its determination by HPLC-DAD.

Science.gov (United States)

Gañán, Judith; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

2013-09-15

Functionalized (SBA-C₁₈ and SM-C₁₈) and non-functionalized (SBA-15 and SM) mesoporous silicas were then examined as sorbents for solid-phase extraction of 17β-estradiol in aqueous media. Experiments were run in order to test critical factors affecting the procedure extraction efficiency, including the type of sorbent, the analyte concentration, the solvent and volume used for elution and the sample volume. Among the prepared materials, SBA-C₁₈ had the highest adsorption affinity towards 17β-estradiol and under optimized conditions (200mg of sorbent, 150 mL of water sample, elution with 3 × 2 mL of methanol) this sorbent proved good extraction capacity and elution efficiency for this hormone from aqueous media (recovery near 100%). To evaluate the analytical applicability of the proposed method, it was applied to the determination of 17β-estradiol in drinking water by high performance liquid chromatography with a photodiode array detector. Calibration curves were shown to be linear between 1.25 and 100 mg L(-1)with correlation coefficients ≥0.999 (n=5) for 17β-estradiol. The instrumental detection and quantitation limits calculated were 0.38 and 1.25 mg L(-1), respectively. The relative standard deviation obtained values were ≤3% and the mean recoveries obtained were of 82%. The results suggest that SBA-C18 is a promising material for the off-line solid phase extraction of 17β-estradiol from waters. Copyright © 2013 Elsevier B.V. All rights reserved.

The Epoxidation of Limonene over the TS-1 and Ti-SBA-15 Catalysts

Directory of Open Access Journals (Sweden)

Agnieszka Wróblewska

2014-11-01

Full Text Available Limonene belongs to a group of very important intermediates used in the production of fine chemicals. This monoterpene compound can be obtained from peels of oranges or lemon which are a (biomass waste from the orange juice industry. Thus, limonene is a renewable, easy available and a relatively cheap compound. This work presents preliminary studies on the process of limonene epoxidation over zeolite type catalysts such as: TS-1 and Ti-SBA-15. In these studies methanol was used as a solvent and as an oxidizing agent a 60 wt % hydrogen peroxide solution was applied. The activity of each catalyst was investigated for four chosen temperatures (0 °C, 40 °C, 80 °C and 120 °C. The reaction time was changed from 0.5 to 24 h. For each catalyst the most beneficial conditions (the appropriate temperature and the reaction time have been established. The obtained results were compared and the most active catalyst was chosen. These studies have also shown different possible ways of limonene transformation, not only in the direction of 1,2-epoxylimonene and its corresponding diol, but also in direction of carveol, carvone and perillyl alcohol—compounds with a lot of applications. The possible mechanisms of formation of the allylic oxidation products were proposed.

One-dimensional ferromagnetic array compound [Co3(SBA)2(OH)2(H2O)2]n, (SBA = 4-sulfobenzoate)

Science.gov (United States)

Honda, Zentaro; Nomoto, Naoyuki; Fujihara, Takashi; Hagiwara, Masayuki; Kida, Takanori; Sawada, Yuya; Fukuda, Takeshi; Kamata, Norihiko

2018-06-01

We report on the syntheses, crystal structure, and magnetic properties of the transition metal coordination polymer [Co3(SBA)2(OH)2(H2O)2]n, (SBA = 4-sulfobenzoate) in which CoO6 octahedra are linked through their edges, forming one-dimensional (1D) Co(II) arrays running along the crystal a-axis. These arrays are further perpendicularly bridged by SBA ligand to construct a three-dimensional framework. Its magnetic properties have been investigated, and ferromagnetic interactions within the arrays have been found. From heat capacity measurements, we have found that this compound exhibits a three-dimensional ferromagnetic phase transition at TC = 1.54 K, and the specific heat just above TC shows a Schottky anomaly which originates from an energy gap caused by uniaxial magnetic anisotropy. These results suggest that [Co3(SBA)2(OH)2(H2O)2]n consists of weakly coupled 1D ferromagnetic Ising arrays.

Highly selective coextraction of rhodamine B and dibenzyl phthalate based on high-density dual-template imprinted shells on silica microparticles.

Science.gov (United States)

Long, Zerong; Xu, Weiwei; Peng, Yumei; Lu, Yi; Luo, Qian; Qiu, Hongdeng

2017-01-01

A simple one-pot approach based on molecularly imprinted polymer shells dispersed on the surface of silica for simultaneous determination of rhodamine B and dibenzyl phthalate (DBzP) has been developed. Highly dense molecularly imprinted polymer shells were formed in the mixture of acetonitrile and toluene by the copolymerization of methacrylic acid and ethylene glycol dimethacrylate, as well as two templates, rhodamine B and dibenzyl phthalate, directed by the vinyl end groups functional monolayer at surface silica microspheres after 3-methacryloxypropyl trimethoxysilane modification. The obtained imprinted polymer shells showed large average pore diameter (102.5 nm) and about 100 nm shell thickness. The imprinted particles also showed high imprinting factor (α RhB = 3.52 and α DBzP = 3.94), rapid binding kinetics, and excellent selective affinity capacity for rhodamine B and dibenzyl phthalate containing another three competitors in mixed solution. Moreover, the imprinted particles coupled with ultra high performance liquid chromatography was successfully applied to simultaneous analysis of rhodamine B and dibenzyl phthalate in two spiked beverage samples with average recoveries in the range of 88.0-93.0% for rhodamine B and 84.0-92.0% for dibenzyl phthalate with the relative standard deviation lower than 5.1%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The influence of supercritical carbon dioxide (SC-CO2) processing conditions on drug loading and physicochemical properties.

Science.gov (United States)

Ahern, Robert J; Crean, Abina M; Ryan, Katie B

2012-12-15

Poor water solubility of drugs can complicate their commercialisation because of reduced drug oral bioavailability. Formulation strategies such as increasing the drug surface area are frequently employed in an attempt to increase dissolution rate and hence, improve oral bioavailability. Maximising the drug surface area exposed to the dissolution medium can be achieved by loading drug onto a high surface area carrier like mesoporous silica (SBA-15). The aim of this work was to investigate the impact of altering supercritical carbon dioxide (SC-CO(2)) processing conditions, in an attempt to enhance drug loading onto SBA-15 and increase the drug's dissolution rate. Other formulation variables such as the mass ratio of drug to SBA-15 and the procedure for combining the drug and SBA-15 were also investigated. A model drug with poor water solubility, fenofibrate, was selected for this study. High drug loading efficiencies were obtained using SC-CO(2), which were influenced by the processing conditions employed. Fenofibrate release rate was enhanced greatly after loading onto mesoporous silica. The results highlighted the potential of this SC-CO(2) drug loading approach to improve the oral bioavailability of poorly water soluble drugs. Copyright © 2012 Elsevier B.V. All rights reserved.

Covalent Anchoring of Chloroperoxidase and Glucose Oxidase on the Mesoporous Molecular Sieve SBA-15

Directory of Open Access Journals (Sweden)

Martin Hartmann

2010-02-01

Full Text Available Functionalization of porous solids plays an important role in many areas, including heterogeneous catalysis and enzyme immobilization. In this study, large-pore ordered mesoporous SBA-15 molecular sieves were synthesized with tetraethyl orthosilicate (TEOS in the presence of the non-ionic triblock co-polymer Pluronic P123 under acidic conditions. These materials were grafted with 3 aminopropyltrimethoxysilane (ATS, 3-glycidoxypropyltrimethoxysilane (GTS and with 3 aminopropyltrimethoxysilane and glutaraldehyde (GA-ATS in order to provide covalent anchoring points for enzymes. The samples were characterized by nitrogen adsorption, powder X-ray diffraction, solid-state NMR spectroscopy, elemental analysis, diffuse reflectance fourier transform infrared spectroscopy and diffuse reflectance UV/Vis spectroscopy. The obtained grafted materials were then used for the immobilization of chloroperoxidase (CPO and glucose oxidase (GOx and the resulting biocatalysts were tested in the oxidation of indole. It is found that enzymes anchored to the mesoporous host by the organic moieties can be stored for weeks without losing their activity. Furthermore, the covalently linked enzymes are shown to be less prone to leaching than the physically adsorbed enzymes, as tested in a fixed-bed reactor under continuous operation conditions.

13 CFR 120.621 - SBA guarantee of an Individual Certificate.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA guarantee of an Individual Certificate. 120.621 Section 120.621 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Secondary Market The Sba Guarantee of A Certificate § 120.621 SBA guarantee of an Individual...

Acid-base equilibria inside amine-functionalized mesoporous silica.

Science.gov (United States)

Yamaguchi, Akira; Namekawa, Manato; Kamijo, Toshio; Itoh, Tetsuji; Teramae, Norio

2011-04-15

Acid-base equilibria and effective proton concentration inside a silica mesopore modified with a trimethyl ammonium (TMAP) layer were studied by steady-state fluorescence experiments. The mesoporous silica with a dense TMAP layer (1.4 molecules/nm(2)) was prepared by a post grafting of N-trimethoxysilylpropyl-N,N,N-trimethylammonium at surfactant-templated mesoporous silica (diameter of silica framework =3.1 nm). The resulting TMAP-modified mesoporous silica strongly adsorbed of anionic fluorescence indicator dyes (8-hydroxypyrene-1,3,6-trisulfonate (pyranine), 8-aminopyrene-1,3,6-trisulfonate (APTS), 5,10,15,20-tetraphenyl-21H,23H-porphinetetrasulfonic acid disulfuric acid (TPPS), 2-naphthol-3,6-disulfonate (2NT)) and fluorescence excitation spectra of these dyes within TMAP-modified mesoporous silica were measured by varying the solution pH. The fluorescence experiments revealed that the acid-base equilibrium reactions of all pH indicator dyes within the TMAP-modified silica mesopore were quite different from those in bulk water. From the analysis of the acid-base equilibrium of pyranine, the following relationships between solution pH (pH(bulk)) and the effective proton concentration inside the pore (pH(pore)) were obtained: (1) shift of pH(pore) was 1.8 (ΔpH(pore)=1.8) for the pH(bulk) change from 2.1 to 9.1 (ΔpH(bulk)=7.0); (2) pH(pore) was not simply proportional to pH(bulk); (3) the inside of the TMAP-modified silica mesopore was suggested to be in a weak acidic or neutral condition when pH(bulk) was changed from 2.0 to 9.1. Since these relationships between pH(bulk) and pH(pore) could explain the acid-base equilibria of other pH indicator dyes (APTS, TPPS, 2NT), these relationships were inferred to describe the effective proton concentration inside the TMAP-modified silica mesopore. © 2011 American Chemical Society

13 CFR 120.620 - SBA guarantee of a Pool Certificate.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA guarantee of a Pool Certificate. 120.620 Section 120.620 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Secondary Market The Sba Guarantee of A Certificate § 120.620 SBA guarantee of a Pool Certificate...

13 CFR 120.1719 - SBA's right to recover from Seller.

Science.gov (United States)

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false SBA's right to recover from Seller. 120.1719 Section 120.1719 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION BUSINESS LOANS Establishment of SBA Secondary Market Guarantee Program for First Lien Position 504 Loan Pools § 120.1719 SBA's...

Modification of mesoporous silica surface applied as drug delivery system; Modificacao de silica mesoporosa aplicada como sistema de liberacao de droga

Energy Technology Data Exchange (ETDEWEB)

Andrade, G.F.; Sousa, A.; Sousa, E.M.B., E-mail: graciellefandrade@yahoo.com.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

2010-07-01

A mesoporous silica with ordered cubic structure, SBA16, was chemically modified with different alcoxisilanos using solvents with different solubility parameters (methanol and toluene), to evaluate its effectiveness as a matrix for the controlled delivery of atenolol. The structural characteristics of the material were evaluated by small angle XRD, N{sub 2} adsorption and scanning electron microscopy. The degree of functionalization of the matrix was evaluated using techniques of FTIR, thermal analysis and elemental analysis CHN. It was found that the type of solvent influences the degree of functionalization and this significantly affects the release process. (author)

Hard template synthesis of porous carbon nitride materials with improved efficiency for photocatalytic CO_2 utilization

International Nuclear Information System (INIS)

Ovcharov, M.; Shcherban, N.; Filonenko, S.; Mishura, A.; Skoryk, M.; Shvalagin, V.; Granchak, V.

2015-01-01

Graphical abstract: - Highlights: • Porous carbon nitrides were obtained via bulk and matrix pyrolysis of melamine. • Carbon nitride obtained in MCF has the highest bandgap and photocatalytic activity. • Acetaldehyde was the major product of the photoreduction reaction of CO2. - Abstract: Porous carbon nitrides of different morphology were obtained via bulk and hard template (SBA-15 and MCF) pyrolysis of melamine. Matrix method allowed obtaining ordered porous C_3N_4 with higher bandgap (2.87 eV) in the contrary to the bulk sample (2.45 eV). Obtained carbon nitrides were found to be p-type semiconductors with catalytic activity towards photoreduction of carbon dioxide with water vapour. Carbon nitride obtained in MCF has the higher bandgap, developed surface, sponge-like morphology, spatially ordering and it's characterized by the highest photocatalytic activity.

Bent silica nanosheets directed from crystalline templates controlled by proton donors

International Nuclear Information System (INIS)

Matsukizono, Hiroyuki; Jin, Ren-Hua

2011-01-01

Linear poly(ethyleneimine) (LPEI) is easily crystallizable with the formation of various morphologies in the aqueous medium when its hot solution cooled down to room temperature. Herein, we prepared a series of crystalline precipitates of LPEI grown in the presence of proton donating compounds such as Tris–HCl, tartaric acid, amino acids, and used the precipitates in directing silica deposition. Since the proton donating compounds can mediate the pH with donating the proton to LPEI, the crystallization of LPEI evidently depended on the concentrations of the proton donating compounds. It was found that the precipitates grown in the conditions of the pH ranged 8.2–8.5 directed well-controlled bent nanosheet of silica/LPEI composites. The bent nanosheet is constructed by multi-layered structures with a little slippage between layers. The bent nanosheet silica has slit-like pore with ca. 10 nm width.

Ordered mesoporous polymer-silica hybrid nanoparticles as vehicles for the intracellular controlled release of macromolecules.

Science.gov (United States)

Kim, Tae-Wan; Slowing, Igor I; Chung, Po-Wen; Lin, Victor Shang-Yi

2011-01-25

A two-dimensional hexagonal ordered mesoporous polymer-silica hybrid nanoparticle (PSN) material was synthesized by polymerization of acrylate monomers on the surface of SBA-15 mesoporous silica nanoparticles. The structure of the PSN material was analyzed using a series of different techniques, including transmission electron microscopy, powder X-ray diffraction, and N(2) sorption analysis. These structurally ordered mesoporous polymer-silica hybrid nanoparticles were used for the controlled release of membrane-impermeable macromolecules inside eukaryotic cells. The cellular uptake efficiency and biocompatibility of PSN with human cervical cancer cells (HeLa) were investigated. Our results show that the inhibitory concentration (IC(50)) of PSN is very high (>100 μg/mL per million cells), while the median effective concentration for the uptake (EC(50)) of PSN is low (EC(50) = 4.4 μg/mL), indicating that PSNs are fairly biocompatible and easily up-taken in vitro. A membrane-impermeable macromolecule, 40 kDa FITC-Dextran, was loaded into the mesopores of PSNs at low pH. We demonstrated that the PSN material could indeed serve as a transmembrane carrier for the controlled release of FITC-Dextran at the pH level inside live HeLa cells. We believe that further developments of this PSN material will lead to a new generation of nanodevices for intracellular controlled delivery applications.

Magnetic solid-phase extraction based on mesoporous silica-coated magnetic nanoparticles for analysis of oral antidiabetic drugs in human plasma

Energy Technology Data Exchange (ETDEWEB)

Souza, Karynne Cristina de; Andrade, Gracielle Ferreira [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil); Vasconcelos, Ingrid; Oliveira Viana, Iara Maíra de; Fernandes, Christian [Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Belo Horizonte, MG (Brazil); Martins Barros de Sousa, Edésia, E-mail: sousaem@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil)

2014-07-01

In the present work, magnetic nanoparticles embedded into mesoporous silica were prepared in two steps: first, magnetite was synthesized by oxidation–precipitation method, and next, the magnetic nanoparticles were coated with mesoporous silica by using nonionic block copolymer surfactants as structure-directing agents. The mesoporous SiO{sub 2}-coated Fe{sub 3}O{sub 4} samples were functionalized using octadecyltrimethoxysilane as silanizing agent. The pure and functionalized silica nanoparticles were physicochemically and morphologically characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N{sub 2} adsorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resultant magnetic silica nanoparticles were applied as sorbents for magnetic solid-phase extraction (MSPE) of oral antidiabetic drugs in human plasma. Our results revealed that the magnetite nanoparticles were completely coated by well-ordered mesoporous silica with free pores and stable pore walls, and that the structural and magnetic properties of the Fe{sub 3}O{sub 4} nanoparticles were preserved in the applied synthesis route. Indeed, the sorbent material was capable of extracting the antidiabetic drugs from human plasma, being useful for the sample preparation in biological matrices. - Highlights: • SBA-15/Fe{sub 3}O{sub 4} was synthesized and functionalized with octadecyltrimethoxysilane. • Magnetite nanoparticles were completely coated by well-ordered mesoporous silica. • The samples were used as sorbent for magnetic solid-phase extraction (MSPE). • The sorbent material was capable of extracting drugs from human plasma. • The extraction ability makes the material a candidate to be employed as MSPE.

75 FR 13145 - SBA Lender Risk Rating System

Science.gov (United States)

2010-03-18

... SMALL BUSINESS ADMINISTRATION [Docket No. SBA-2010-0004] SBA Lender Risk Rating System AGENCY: Small Business Administration. ACTION: Notice; extension of comment period and correction. SUMMARY: On... of Credit Risk Management, U.S. Small Business Administration, 409 Third Street, SW., 8th Floor...

Formation of Uniform Hollow Silica microcapsules

Science.gov (United States)

Yan, Huan; Kim, Chanjoong

2013-03-01

Microcapsules are small containers with diameters in the range of 0.1 - 100 μm. Mesoporous microcapsules with hollow morphologies possess unique properties such as low-density and high encapsulation capacity, while allowing controlled release by permeating substances with a specific size and chemistry. Our process is a one-step fabrication of monodisperse hollow silica capsules with a hierarchical pore structure and high size uniformity using double emulsion templates obtained by the glass-capillary microfluidic technique to encapsulate various active ingredients. These hollow silica microcapsules can be used as biomedical applications such as drug delivery and controlled release.

Organized mesoporous silica films as templates for the elaboration of organized nanoparticle networks

International Nuclear Information System (INIS)

Gacoin, T; Besson, S; Boilot, J P

2006-01-01

Tremendous work achieved in the last 20 years on nanoparticle synthesis has allowed us to study many new physical properties that are found in the nanometre size range. New developments are now expected when considering assemblies of nanoparticles such as 2D or 3D organized arrays. These systems are indeed expected to exhibit original physical properties resulting from particle-particle interactions. Studies in this field are clearly dependent on the elaboration of materials with controlled particle size, organization and interparticle distance. This paper presents a strategy of elaboration that is based on the use of organized mesoporous silica films as templates. These films are made by sol-gel polymerization around surfactant assemblies and further elimination of the surfactant. This provides porous matrices with a pore organization that is the almost perfect replica of the initial micellar structure. The use of such films for the elaboration of organized arrays of nanoparticles is detailed in the case of CdS and Ag particles. The formation of particles inside the pores is achieved through impregnation with precursors that are allowed to diffuse inside the pores. This leads to particles with a size and a spatial arrangement that is directly related to the initial pore structure of the films. This process opens a wide range of investigations due to the relative ease of fabrication over large surfaces and the numerous possibilities offered by the elaboration of porous films with different pore sizes and organizations

Soft-to-hard templating to well-dispersed N-doped mesoporous carbon nanospheres via one-pot carbon/silica source copolymerization

Institute of Scientific and Technical Information of China (English)

Qinglu Kong; Lingxia Zhang; Min Wang; Mengli Li; Heliang Yao; Jianlin Shi

2016-01-01

Here we report a new approach referred as "softto-hard templating" strategy via the copolymerization of carbon source (dopamine) and silica source (tetraethyl orthosilicate) for the synthesis of well dispersed N-doped mesoporous carbon nanospheres (MCNs),which exhibit high performance for electrochemical supercapacitor.This method overcomes the shortcoming of uncontrolled dispersity and complicated procedures of soft-or hard-tem-plating methods,respectively.Moreover,the synthesized MCNs feature enriched heteroatom N-doping and easy functionalization by noble-metal nanoparticles during the one-pot synthesis.All the above characters make the asprepared MCNs a promising platform in a variety of applications.To demonstrate the applicability of the synthesized nitrogen-doped MCNs,this material has been employed as an electrode for high-performance electrochemical supercapacitor,which shows a capacitance of 223 and 140 F/g at current densities of 0.5 and 10 A/g in 1 mol/L KOH electrolyte,respectively.

Preparation, characterization and catalytic activity of mesoporous Ag{sub 2}HPW{sub 12}O{sub 40}/SBA-15 and Ag{sub 2}HPW{sub 12}O{sub 40}/TiO{sub 2} composites

Energy Technology Data Exchange (ETDEWEB)

Holclajtner-Antunović, Ivanka; Bajuk-Bogdanović, Danica [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Popa, Alexandru; Sasca, Viorel [Institute of Chemistry Timişoara, Bl. Mihail Viteazul 24, 300223 Timişoara (Romania); Nedić Vasiljević, Bojana; Rakić, Aleksandra [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11158 Belgrade (Serbia); Uskoković-Marković, Snežana, E-mail: snezaum@pharmacy.bg.ac.rs [Faculty of Pharmacy, University of Belgrade, Vojvode Stepe 450, 11221 Belgrade (Serbia)

2015-06-15

The current study reports the synthesis and characterization of tungstophosphoric acid and its acid silver salt supported on mesoporous molecular sieve SBA-15 and TiO{sub 2}. Because silver salts are partially insoluble, the SBA-15 and TiO{sub 2} supported silver acid salts were prepared by two step sequential impregnations. The synthesized catalysts were characterized by various physicochemical methods such as Fourier transform infrared and Raman spectroscopy, differential thermal analysis, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and nitrogen physisorption at −196 °C. It is observed that both active phases keep their Keggin-type structure after being supported on the supports while their specific surface area is considerably increased by deposition on mesoporous substrates. The results also indicated that the synthesized catalysts retained the morphology specific for each of the supports, while their thermal stability is increased in comparison with their active phases. The catalytic activity of the prepared catalysts was probed for the vapor phase dehydration of ethanol at 300 °C. Results revealed that all the catalysts show considerably improved catalytic activity in comparison to the bulk active phases. - Highlights: • SBA-15 and TiO{sub 2} supported Ag{sub 2}HPW{sub 12}O{sub 40} and H{sub 3}PW{sub 12}O{sub 40} were prepared. • Active phases are uniformly dispersed without changing morphology of the substrates. • Composites are more thermally stable than active phases. • Composites exhibit high catalytic activity for gas phase ethanol dehydration.

Organic or organometallic template mediated clay synthesis

Science.gov (United States)

Gregar, Kathleen C.; Winans, Randall E.; Botto, Robert E.

1994-01-01

A method for incorporating diverse Varieties of intercalants or templates directly during hydrothermal synthesis of clays such as hectorite or montmorillonite-type layer-silicate clays. For a hectorite layer-silicate clay, refluxing a gel of silica sol, magnesium hydroxide sol and lithium fluoride for two days in the presence of an organic or organometallic intercalant or template results in crystalline products containing either (a) organic dye molecules such as ethyl violet and methyl green, (b) dye molecules such as alcian blue that are based on a Cu(II)-phthalocyannine complex, or (c) transition metal complexes such as Ru(II)phenanthroline and Co(III)sepulchrate or (d) water-soluble porphyrins and metalloporphyrins. Montmorillonite-type clays are made by the method taught by U.S. Pat. No. 3,887,454 issued to Hickson, Jun. 13, 1975; however, a variety of intercalants or templates may be introduced. The intercalants or templates should have (i) water-solubility, (ii) positive charge, and (iii) thermal stability under moderately basic (pH 9-10) aqueous reflux conditions or hydrothermal pressurized conditions for the montmorillonite-type clays.

Effect of support structure on CO2 adsorption properties of pore-expanded hyperbranched aminosilicas

KAUST Repository