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Sample records for modified silica mcm-41

  1. Laccase immobilized on methylene blue modified mesoporous silica MCM-41/PVA

    International Nuclear Information System (INIS)

    Xu Xinhua; Lu Ping; Zhou Yumei; Zhao Zhenzhen; Guo Meiqing

    2009-01-01

    The mesoporous silica sieve MCM-41 containing methylene blue (MB) provides a suitable immobilization of biomolecule matrix due to its uniform pore structure, high surface areas, good biocompatibility and nice conductivity. Based on this, a facilely fabricated amperometric biosensor by entrapping laccase into the MB modified MCM-41/PVA composite film has been developed. Laccase from Trametes versicolor is assembled on a composite film of MCM-41 containing MB/PVA modified Au electrode and the electrode is characterized with respect to transmission electron microscopy (TEM) and scanning electron microscopic (SEM), Cyclic voltammetry (CV), response time, detection limit, linear range and activity of laccase. The laccase modified electrode remains good redox behavior in pH 4.95 acetate buffer solution, at room temperature in present of 0.1 mM catechol. The response time (t 90% ) of the modified electrode is less than 4 s for catechol. The detection limit is 0.331 μM and the linear detect range is about from 4.0 μM to 87.98 μM for catechol with a correlation coefficient of 0.99913(S/N = 3). The apparent Michaelis-Menten (K M app ) is estimated using the Lineweaver-Burk equation and the K M app value is about 0.256 mM. This work demonstrated that the mesoporous silica MCM-41 containing MB provides a novel support for laccase immobilization and the construction of biosensors with a faster response and better bioactivity.

  2. Preparation and use of chemically modified MCM-41 and silica gel as selective adsorbents for Hg(II) ions

    International Nuclear Information System (INIS)

    Puanngam, Mahitti; Unob, Fuangfa

    2008-01-01

    Adsorbents for Hg(II) ion extraction were prepared using amorphous silica gel and ordered MCM-41. Grafting with 2-(3-(2-aminoethylthio)propylthio)ethanamine was used to functionalize the silica. The functionalized adsorbents were characterized by nitrogen adsorption, X-ray diffraction, 13 C MAS NMR spectroscopy and thermogravimetric analysis. The adsorption properties of the modified silica gel and MCM-41 were compared using batch method. The effect of pH, stirring time, ionic strength and foreign ions were studied. The extraction of Hg(II) ions occurred rapidly with the modified MCM-41 and the optimal pH range for the extraction by the modified materials was pH 4-7. Foreign ions, especially Cl - had some effect on the extraction efficiency of the modified silica gel and the modified MCM-41. The adsorption behavior of both adsorbents could be described by a Langmuir model at 298 K, and the maximum adsorption capacity of the modified silica gel and MCM-41 at pH 3 was 0.79 and 0.70 mmol g -1 , respectively. The modified MCM-41 showed a larger Langmuir constant than that of the modified silica gel, indicating a better ability for Hg(II) ion adsorption. The results indicate that the structure of the materials affects the adsorption behavior. These materials show a potential for the application as effective and selective adsorbents for Hg(II) removal from water

  3. Alcohols react with MCM-41 at room temperature and chemically modify mesoporous silica.

    Science.gov (United States)

    Björklund, Sebastian; Kocherbitov, Vitaly

    2017-08-30

    Mesoporous silica has received much attention due to its well-defined structural order, high surface area, and tunable pore diameter. To successfully employ mesoporous silica for nanotechnology applications it is important to consider how it is influenced by solvent molecules due to the fact that most preparation procedures involve treatment in various solvents. In the present work we contribute to this important topic with new results on how MCM-41 is affected by a simple treatment in alcohol at room temperature. The effects of alcohol treatment are characterized by TGA, FTIR, and sorption calorimetry. The results are clear and show that treatment of MCM-41 in methanol, ethanol, propanol, butanol, pentanol, or octanol at room temperature introduces alkoxy groups that are covalently bound to the silica surface. It is shown that alcohol treated MCM-41 becomes more hydrophobic and that this effect is sequentially more prominent going from methanol to octanol. Chemical formation of alkoxy groups onto MCM-41 occurs both for calcined and hydroxylated MCM-41 and the alkoxy groups are hydrolytically unstable and can be replaced by silanol groups after exposure to water. The results are highly relevant for mesoporous silica applications that involve contact or treatment in protic solvents, which is very common.

  4. Novel acridone-modified MCM-41 type silica: Synthesis, characterization and fluorescence tuning

    Directory of Open Access Journals (Sweden)

    Maximilian Hemgesberg

    2011-06-01

    Full Text Available A Mobil Composition of Matter (MCM-41 type mesoporous silica material containing N-propylacridone groups has been successfully prepared by co-condensation of an appropriate organic precursor with tetraethyl orthosilicate (TEOS under alkaline sol–gel conditions. The resulting material was fully characterized by means of X-ray diffraction (XRD, N2-adsorption–desorption, transmission electron microscopy (TEM, IR and UV–vis spectroscopy, as well as 29Si and 13C CP-MAS NMR techniques. The material features a high inner surface area and a highly ordered two-dimensional hexagonal pore structure. The fluorescence properties of the organic chromophore can be tuned via complexation of its carbonyl group with scandium triflate, which makes the material a good candidate for solid state sensors and optics. The successful synthesis of highly ordered MCM materials through co-condensation was found to be dependent on the chemical interaction of the different precursors.

  5. Tailoring MCM-41 mesoporous silica particles through modified sol-gel process for gas separation

    Science.gov (United States)

    Sang, Wong Yean; Ching, Oh Pei

    2017-10-01

    Mobil Composition of Matter-41 (MCM-41) is recognized as a potential filler to enhance permeability of mixed matrix membrane (MMM). However, the required loading for available micron-sized MCM-41 was considerably high in order to achieve desired separation performance. In this work, reduced-size MCM-41 was synthesized to minimize filler loading, improve surface modification and enhance polymer-filler compatibility during membrane fabrication. The effect of reaction condition, stirring rate and type of post-synthesis washing solution used on particle diameter of resultant MCM-41 were investigated. It was found that MCM-41 produced at room temperature condition yield particles with smaller diameter, higher specific surface area and enhanced mesopore structure. Increase of stirring rate up to 500 rpm during synthesis also reduced the particle diameter. In addition, replacing water with methanol as the post-synthesis washing solution to remove bromide ions from the precipitate was able to further reduce the particle size by inhibiting polycondensation reaction.

  6. Polyethylenimine-modified curcumin-loaded mesoporus silica nanoparticle (MCM-41) induces cell death in MCF-7 cell line.

    Science.gov (United States)

    Harini, Lakshminarasimhan; Karthikeyan, Bose; Srivastava, Sweta; Suresh, Srinag Bangalore; Ross, Cecil; Gnanakumar, Georgepeter; Rajagopal, Srinivasan; Sundar, Krishnan; Kathiresan, Thandavarayan

    2017-02-01

    Breast cancer accounts for the first highest mortality rate in India and second in world. Though current treatment strategies are effectively killing cancer cells, they also end in causing severe side effects and drug resistance. Curcumin is a nutraceutical with multipotent activity but its insolubility in water limits its therapeutic potential as an anti-cancer drug. The hydrophilicity of curcumin could be increased by nanoformulation or changing its functional groups. In this study, curcumin is loaded on mesoporous silica nanoparticle and its anti-cancer activity is elucidated with MCF-7 cell death. Structural characteristics of Mobil Composition of Matter - 41(MCM-41) as determined by high-resolution transmission electron microscopy (HR-TEM) shows that MCM-41 size ranges from 100 to 200 nm diameters with pore size 2-10 nm for drug adsorption. The authors found 80-90% of curcumin is loaded on MCM-41 and curcumin is released efficiently at pH 3.0. The 50 µM curcumin-loaded MCM-41 induced 50% mortality of MCF-7 cells. Altogether, their results suggested that increased curcumin loading and sustained release from MCM-41 effectively decreased cell survival of MCF-7 cells in vitro.

  7. The study of methanol transformation over Cu-modified ZSM-5, Beta zeolite and MCM-41 mesoporous silica using 11C-radioisotope labeling

    International Nuclear Information System (INIS)

    Sarkadi-Priboczki, E.; Kovacs, Z.

    2004-01-01

    Complete text of publication follows. The copper-containing zeolites and mesoporous silica, among other metals, are suitable for dehydrogenation of methanol. The Cu transition metal determines the route of methanol conversion on supports of ZSM-5 and Beta zeolite as well as MCM-41 mesoporous silica. The catalysis mechanism and the catalytic property are concluded from the composition of methanol derivates over Cu-modified catalysts. The Cu ion-exchanged ZSM-5 and Beta zeolite and MCM-41 mesoporous silica were synthesized and characterized using X-ray power diffraction, scanning electron microscope, nitrogen and pyridine adsorption, X-ray fluorescency and FTIR spectroscopy. The 11 C-radioactive labeling method ( 11 C radioisotope, T 1/2 = 20 min, is a gamma emitter by annihilation of its positron) is suitable for following the process of 11 C-methanol con- version i.e. adsorption, desorption and catalytic transformation as well as for investigation of small amounts of molecules over catalysts by very sensitive radioactivity detectors.The 11 C radioisotope was produced at cyclotron and the 11 C-methanol was synthesized by a classical radiochemical method. After catalysis the 11 C-radioactive and non radioactive volatile products were identified by radiogas chromatography hereby radiolabeled compound and -derivates were distinguished from other participant natural, nonradioactive carbon compounds. Along radioactive products dimethyl ether and small hydrocarbons products were formed by Bronsted acid sites of catalysts while formaldehyde and small methyl formate were formed by Cu metal over bifunctional Cu-ZSM-5, Cu-Beta zeolite and mesoporous Cu-MCM-41 silica at 240 deg C. The detection of methoxy methanol and dimethoxy methane confirmed the simultaneous presence of acid and basic sites of catalysts. At higher temperature (400 deg C) the CO and CO 2 final products were dominated. In our previous works, methanol conversion to hydrocarbons was observed by dehydration

  8. Lysine-Grafted MCM-41 Silica as an Antibacterial Biomaterial.

    Science.gov (United States)

    Villegas, María F; Garcia-Uriostegui, Lorena; Rodríguez, Ofelia; Izquierdo-Barba, Isabel; Salinas, Antonio J; Toriz, Guillermo; Vallet-Regí, María; Delgado, Ezequiel

    2017-09-26

    This paper proposes a facile strategy for the zwitterionization of bioceramics that is based on the direct incorporation of l-lysine amino acid via the ε-amino group onto mesoporous MCM-41 materials. Fourier transform infrared (FTIR) studies of lysine-grafted MCM-41 (MCM-LYS) simultaneously showed bands at 3080 and 1540 cm -1 and bands at 1625 and 1415 cm -1 corresponding to -NH 3+ /COO - pairs, which demonstrate the incorporation of the amino acid on the material surface keeping its zwitterionic character. Both elemental and thermogravimetric analyses showed that the amount of grafted lysine was 8 wt. % based on the bioceramic total weight. Moreover, MCM-LYS exhibited a reduction of adhesion of S. aureus and E. coli bacteria in 33% and 50%, respectively at physiological pH, as compared with pristine MCM-41. Biofilm studies onto surfaces showed that lysine functionalization elicited a reduction of the area covered by S. aureus biofilm from 42% to only 5% (88%). This research shows a simple and effective approach to chemically modify bioceramics using single amino acids that provides zwitterionic functionality, which is useful to develop new biomaterials that are able to resist bacterial adhesion.

  9. Lysine-Grafted MCM-41 Silica as an Antibacterial Biomaterial

    Directory of Open Access Journals (Sweden)

    María F. Villegas

    2017-09-01

    Full Text Available This paper proposes a facile strategy for the zwitterionization of bioceramics that is based on the direct incorporation of l-lysine amino acid via the ε-amino group onto mesoporous MCM-41 materials. Fourier transform infrared (FTIR studies of lysine-grafted MCM-41 (MCM-LYS simultaneously showed bands at 3080 and 1540 cm−1 and bands at 1625 and 1415 cm−1 corresponding to -NH3+/COO− pairs, which demonstrate the incorporation of the amino acid on the material surface keeping its zwitterionic character. Both elemental and thermogravimetric analyses showed that the amount of grafted lysine was 8 wt. % based on the bioceramic total weight. Moreover, MCM-LYS exhibited a reduction of adhesion of S. aureus and E. coli bacteria in 33% and 50%, respectively at physiological pH, as compared with pristine MCM-41. Biofilm studies onto surfaces showed that lysine functionalization elicited a reduction of the area covered by S. aureus biofilm from 42% to only 5% (88%. This research shows a simple and effective approach to chemically modify bioceramics using single amino acids that provides zwitterionic functionality, which is useful to develop new biomaterials that are able to resist bacterial adhesion.

  10. Synthesis and characterization of bulky mesoporous silica Pd-MCM-41

    International Nuclear Information System (INIS)

    Nagata, Hidezumi; Nakahira, Atsushi; Hirao, Norie; Baba, Yuji; Onoki, Takamasa; Yamasaki, Yuki

    2008-01-01

    Bulky palladium catalyst supported on mesoporous silica MCM-41 (Pd-MCM-41) was successfully synthesized by hydrothermal hot-pressing method. In this study, the structure of the palladium species in Pd-MCM-41 bulk before and after heat-treatment process was revealed by X-ray diffraction (XRD), X-ray absorption near edge structure (XANES) and transmission electron microscopy (TEM). Also, the microstructure and mesoporous property of Pd-MCM-41 bulk was discussed. As a result, it was revealed that these dense Pd-MCM-41 bulks possessed a high surface area of over 1000 m 2 /g and the structure of palladium of Pd-MCM-41 bulk is almost equal to palladium (0) metal. (author)

  11. Pore radius fine tuning of a silica matrix (MCM-41) based on the synthesis of alumina nanolayers with different thicknesses by atomic layer deposition

    International Nuclear Information System (INIS)

    Zemtsova, Elena G.; Arbenin, Andrei Yu.; Plotnikov, Alexander F.; Smirnov, Vladimir M.

    2015-01-01

    The authors investigated a new approach to modify the surface of the mesoporous silica matrix MCM-41. This approach is based on manipulating the chemical composition of the porous surface layer and also on fine tuning the pore radius by applying the atomic layer deposition (ALD) technique. The synthesis of alumina nanolayers was performed on the planar and the porous matrix (MCM-41) by the ALD technique using aluminum tri-sec-butoxide and water as precursors. The authors show that one cycle on silicon, using aluminum tri-sec-butoxide and water as precursors, results in a 1–1.2 Å increase in alumina nanolayer thickness. This is comparable to the increase in thickness per cycle for other precursors such as trimethylaluminum and aluminum chloride. The authors show that the synthesis of an Al 2 O 3 nanolayer on the pore surface of the mesoporous silica matrix MCM-41 by the ALD technique results in a regular change in the porous structure of the samples. The specific porosity (ml/g) of the MCM-41 was 0.95 and that of MCM-41 after 5 ALD cycles was 0.39. The pore diameter (nm) of MCM-41 was 3.3 and that of MCM-41 after 5 ALD cycles was 2.3

  12. Tetracycline-Containing MCM-41 Mesoporous Silica Nanoparticles for the Treatment of Escherichia coli.

    Science.gov (United States)

    Koneru, Bhuvaneswari; Shi, Yi; Wang, Yu-Chieh; Chavala, Sai H; Miller, Michael L; Holbert, Brittany; Conson, Maricar; Ni, Aiguo; Di Pasqua, Anthony J

    2015-10-30

    Tetracycline (TC) is a well-known broad spectrum antibiotic, which is effective against many Gram positive and Gram negative bacteria. Controlled release nanoparticle formulations of TC have been reported, and could be beneficial for application in the treatment of periodontitis and dental bone infections. Furthermore, TC-controlled transcriptional regulation systems (Tet-on and Tet-off) are useful for controlling transgene expression in vitro and in vivo for biomedical research purposes; controlled TC release systems could be useful here, as well. Mesoporous silica nanomaterials (MSNs) are widely studied for drug delivery applications; Mobile crystalline material 41 (MCM-41), a type of MSN, has a mesoporous structure with pores forming channels in a hexagonal fashion. We prepared 41 ± 4 and 406 ± 55 nm MCM-41 mesoporous silica nanoparticles and loaded TC for controlled dug release; TC content in the TC-MCM-41 nanoparticles was 18.7% and 17.7% w/w, respectively. Release of TC from TC-MCM-41 nanoparticles was then measured in phosphate-buffered saline (PBS), pH 7.2, at 37 °C over a period of 5 h. Most antibiotic was released from both over this observation period; however, the majority of TC was released over the first hour. Efficacy of the TC-MCM-41 nanoparticles was then shown to be superior to free TC against Escherichia coli (E. coli) in culture over a 24 h period, while blank nanoparticles had no effect.

  13. Steam stable mesoporous silica MCM-41 stabilized by trace amounts of Al.

    Science.gov (United States)

    Tompkins, Jordan T; Mokaya, Robert

    2014-02-12

    Evaluation of low and ultralow Al content (Si/Al between 50 and 412) aluminosilicate Al-MCM-41 materials synthesized via three contrasting alumination routes, namely, direct mixed-gel synthesis, post-synthesis wet grafting, and post-synthesis dry grafting, indicates that trace amounts of Al introduced via dry grafting can stabilize mesoporous silica MCM-41 to steaming at 900 °C for 4 h. It was found that trace amounts of Al (Si/Al > 400) introduced via so-called dry grafting of Al stabilize the virtually purely siliceous MCM-41 to steaming, whereas Al incorporated via other methods that involve aqueous media such as direct mixed gel synthesis or wet grafting of Al offer only limited protection at low Al content. It is particularly remarkable that a post-synthesis dry grafted Al-MCM-41 material possessing trace amounts of Al (i.e., Si/Al ratio of 412) and surface area and pore volume of 1112 m(2)/g and 1.20 cm(3)/g, respectively, retains 90% (998 m(2)/g) of the surface area and 85% (1.03 cm(3)/g) of the pore volume after exposure to steaming at 900 °C for 4 h. Under similar steam treatment conditions, the mesostructure of pure silica Si-MCM-41 is virtually destroyed and undergoes a 93% reduction in surface area (958 m(2)/g to 69 m(2)/g) and 88% decrease in pore volume (0.97 cm(3)/g to 0.12 cm(3)/g). The steam stable ultralow (i.e., trace) Al containing MCM-41 materials is found to be virtually similar to mesoporous pure silica Si-MCM-41 with hardly any detectable acidity. The improvement in steam stability arises from not only the presence of trace amounts of Al, but also from an apparent increase in the level of silica condensation that is specific to dry grafted alluminosilicate MCM-41 materials. The more highly condensed framework has fewer silanol groups and therefore is more resistant to hydrolysis under steaming conditions.

  14. A Thin Film Nanocomposite Membrane with MCM-41 Silica Nanoparticles for Brackish Water Purification

    Directory of Open Access Journals (Sweden)

    Mohammed Kadhom

    2016-12-01

    Full Text Available Thin film nanocomposite (TFN membranes containing MCM-41 silica nanoparticles (NPs were synthesized by the interfacial polymerization (IP process. An m-phenylenediamine (MPD aqueous solution and an organic phase with trimesoyl chloride (TMC dissolved in isooctane were used in the IP reaction, occurring on a nanoporous polysulfone (PSU support layer. Isooctane was introduced as the organic solvent for TMC in this work due to its intermediate boiling point. MCM-41 silica NPs were loaded in MPD and TMC solutions in separate experiments, in a concentration range from 0 to 0.04 wt %, and the membrane performance was assessed and compared based on salt rejection and water flux. The prepared membranes were characterized via scanning electron microscopy (SEM, transmission electron microscopy (TEM, contact angle measurement, and attenuated total reflection Fourier transform infrared (ATR FT-IR analysis. The results show that adding MCM-41 silica NPs into an MPD solution yields slightly improved and more stable results than adding them to a TMC solution. With 0.02% MCM-41 silica NPs in the MPD solution, the water flux was increased from 44.0 to 64.1 L/m2·h, while the rejection virtually remained the same at 95% (2000 ppm NaCl saline solution, 25 °C, 2068 kPa (300 psi.

  15. A Thin Film Nanocomposite Membrane with MCM-41 Silica Nanoparticles for Brackish Water Purification.

    Science.gov (United States)

    Kadhom, Mohammed; Yin, Jun; Deng, Baolin

    2016-12-06

    Thin film nanocomposite (TFN) membranes containing MCM-41 silica nanoparticles (NPs) were synthesized by the interfacial polymerization (IP) process. An m -phenylenediamine (MPD) aqueous solution and an organic phase with trimesoyl chloride (TMC) dissolved in isooctane were used in the IP reaction, occurring on a nanoporous polysulfone (PSU) support layer. Isooctane was introduced as the organic solvent for TMC in this work due to its intermediate boiling point. MCM-41 silica NPs were loaded in MPD and TMC solutions in separate experiments, in a concentration range from 0 to 0.04 wt %, and the membrane performance was assessed and compared based on salt rejection and water flux. The prepared membranes were characterized via scanning electron microscopy (SEM), transmission electron microscopy (TEM), contact angle measurement, and attenuated total reflection Fourier transform infrared (ATR FT-IR) analysis. The results show that adding MCM-41 silica NPs into an MPD solution yields slightly improved and more stable results than adding them to a TMC solution. With 0.02% MCM-41 silica NPs in the MPD solution, the water flux was increased from 44.0 to 64.1 L/m²·h, while the rejection virtually remained the same at 95% (2000 ppm NaCl saline solution, 25 °C, 2068 kPa (300 psi)).

  16. Modified Ta/MCM-41 catalysts for enantioselective oxidation of thioanisole

    OpenAIRE

    Fadhli, Marwa; Khedher, Ilyes; Fraile, José M.

    2015-01-01

    Ta-MCM41 catalysts have been prepared by grafting of Ta(OEt)5 on MCM41, pre-calcined at three different temperatures (550, 650 and 750 °C). These solids have been modified with two chiral ligands: R-(+)-diethyl l-tartrate (DET) and R-(+)-diisopropyl l-tartrate (DIPT). The formation of the chiral tantalum species and their influence on the structure of MCM41 have been studied by several characterization techniques, such as XRD, FTIR, N2 adsorption isotherms and MAS NMR. The grafted tantalum sp...

  17. Cumene cracking on modified mesoporous material type MCM-41

    African Journals Online (AJOL)

    AlMCM-41 materials, the method of its exchange mode and its grains form were investigated for the mesoporous catalytic activity in the cumene (i.e. isopropylbenzene) cracking reaction. Benzene, propylene and xylene derivatives are the main ...

  18. 11C-radioisotope study of methanol co-reaction with ethanol over Ni-MCM-41 silica-alumina and Ni-alumina

    International Nuclear Information System (INIS)

    Sarkadi-Priboczki, E.; Kovacs, Z.; Tsoncheva, T.; Kumar, N.; Murzin, D.Yu.

    2009-01-01

    Complete text of publication follows. The Ni modifies the properties of acidic alumina and light acidic MCM-41 silica-alumina supports. The radioisotopic method is a suitable tool for distinction of the 11 Cradioisotopic methanol and its co-derivates from derivates of non-radioactive ethanol on these catalysts. Experimental. The Ni/A l 2O 3 (5 wt % Ni) is commercially available while H-MCMN-41 (Si/Al=20) and Ni-ion-exchanged MCM-41 silica-alumina (5 wt % Ni) were prepared and characterized in previous works. Before catalysis the Ni/Al 2 O 3 and Ni-MCM-41 were pre-reduced. The 11 C-methanol was formed by a radiochemical process from 11 C-carbon dioxide produced at cyclotron (T 1/2 = 20.4 min). The mixture of equivalent volume of radioactive methanol and non-radioactive ethanol was introduced into glass tube micro-flow reactor at ambient temperature. After adsorption, the valves were closed and the catalyst was heated up to the required temperatures. The desorption rate of the remaining 11 C-derivatives on catalysts were continuously followed by radiodetectors and the derivatives of methanol with ethanol were analyzed by Radio/FID-gas chromatography (FID is coupled on-line with a radiodetector). The ethanol and its derivates were identified by FID while the 11 C-methanol and its co-derivates (with ethanol) were detected by both of FID and radiodetector. Results The 11 C-dimethyl ether was the common product of the single 11 C-methanol transformation on H-MCM-41, Ni-MCM-41 and Ni- Al 2 O 3 at low temperature (200-280 degC) due to middle strong acid sites. At higher temperature (280-350 degC), the dimethyl ether and hydrocarbons were the dominant products on H-MCM-41 while dimethyl ether selectivity decreased on Ni-alumina and Ni-MCM-41 in favor of methane. The selectivities of methanol to formaldehyde and methane were the highest on Ni-MCM-41. During co-reaction of 11 C-methanol with non-radioactive ethanol, the 11 C-labeled coethers, namely 11 C-methyl ethyl ether

  19. Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

    Energy Technology Data Exchange (ETDEWEB)

    Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A., E-mail: ivan_melendez380@hotmail.com [Centro de Investigacion en Quimica Aplicada, Bldv. Enrique Reyna Hermosillo No. 140, Saltillo 25294, Coahuila (Mexico)

    2013-08-01

    In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na{sub 2}SiO{sub 3}) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO{sub 2} molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO{sub 2} molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

  20. Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

    International Nuclear Information System (INIS)

    Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A.

    2013-01-01

    In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na 2 SiO 3 ) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO 2 molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO 2 molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

  1. FT-IR studies on the acidity of gallium-substituted mesoporous MCM-41 silica

    International Nuclear Information System (INIS)

    Turnes Palomino, Gemma; Jose Cuart Pascual, Juan; Rodriguez Delgado, Montserrat; Bernardo Parra, Jose; Otero Arean, Carlos

    2004-01-01

    Gallium-containing mesoporous MCM-41 silica was synthesized at a nominal Si:Ga ratio of 16:1. Synthesis was carried out from a parent gel containing no cations other than NH 4 + and cetyltrimethylammonium (template), so that following thermolysis of the template agent and ammonium ions the protonic form, H-GaMCM-41, was obtained. Powder X-ray diffraction showed the characteristic pattern of MCM-41-type materials, and nitrogen adsorption at 77 K lead to a value of 535 m 2 g -1 for the specific (BET) surface area. Infrared spectroscopy of carbon monoxide adsorbed at 77 K, and of pyridine and lutidine adsorbed at room temperature, showed the presence in H-GaMCM-41 of both Broensted and Lewis acid sites. Broensted acidity, assigned to structural Si(OH)Ga groups, was most distinctively proved by protonation of both pyridine and lutidine. Lewis acidity (coordinatively unsaturated Ga 3+ ions) showed up by formation of the characteristic Lewis-type adducts with both CO and pyridine

  2. Optical properties of (nanometer MCM-41)-(malachite green) composite materials

    International Nuclear Information System (INIS)

    Li Xiaodong; Zhai Qingzhou; Zou Mingqiang

    2010-01-01

    Nanosized materials loaded with organic dyes are of interest with respect to novel optical applications. The optical properties of malachite green (MG) in MCM-41 are considerably influenced by the limited nanoporous channels of nanometer MCM-41. Nanometer MCM-41 was synthesized by tetraethyl orthosilicate (TEOS) as the source of silica and cetyltrimethylammonium bromide (CTMAB) as the template. The liquid-phase grafting method has been employed for incorporation of the malachite green molecules into the channels of nanometer MCM-41. A comparative study has been carried out on the adsorption of the malachite green into modified MCM-41 and unmodified MCM-41. The modified MCM-41 was synthesized using a silylation reagent, trimethychlorosilane (TMSCl), which functionalized the surface of nanometer MCM-41 for proper host-guest interaction. The prepared (nanometer MCM-41)-MG samples have been studied by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, low-temperature nitrogen adsorption-desorption technique at 77 K, Raman spectra and luminescence studies. In the prepared (nanometer MCM-41)-MG composite materials, the frameworks of the host molecular sieve were kept intact and the MG located inside the pores of MCM-41. Compared with the MG, it is found that the prepared composite materials perform a considerable luminescence. The excitation and emission spectra of MG in both modified MCM-41 and unmodified MCM-41 were examined to explore the structural effects on the optical properties of MG. The results of luminescence spectra indicated that the MG molecules existed in monomer form within MCM-41. However, the luminescent intensity of MG incorporated in the modified MCM-41 are higher than that of MG encapsulated in unmodified MCM-41, which may be due to the anchored methyl groups on the channels of the nanometer MCM-41 and the strong host-guest interactions. The steric effect from the pore size of the host materials is significant. Raman

  3. Synthesis of AL-MCM-41 using gravel drilling the source of silica from wells drilling

    International Nuclear Information System (INIS)

    Fontes, M.S.B.; Costa, C.C.; Melo, D.M.A.; Viana, L.M.; Viana, S.O.; Santos, L.M.

    2016-01-01

    The aim of this study was to synthesize Al-MCM-41 using gravel drilling as alternative source of silica, aiming at sustainable production and low cost. For hydrothermal synthesis of Al-MCM-41 was used gravel and sodium silicate as source of silica and sodium, respectively. The structural driver used was cetyltrimethylammonium bromide (CTMABr) and solvent distilled water. The hydrothermal synthesis was conducted at 100 ° C in a Teflon autoclave 45 ml jacketed stainless steel for a period of 120 hours with daily correcting pH (range 9-10) using 30% acetic acid. The material obtained was filtered, washed, dried at 100 ° C for 3 hours and then calcined at 550 ° C for 2 hours. Then it was characterized by XRD, FTIR and TG. For the results of characterization has been observed that the use of the gravel drilling as a source of silica was promising alternative for producing a mesoporous material with a high degree of hexagonal ordering. (author)

  4. Structure and photocatalytic activity studies of TiO2-supported over Ce-modified Al-MCM-41

    International Nuclear Information System (INIS)

    Krishna Reddy, Jakkidi; Durgakumari, Valluri; Subrahmanyam, Machiraju; Sreedhar, Bojja

    2009-01-01

    Ce-Al-MCM-41, TiO 2 /Al-MCM-41 and TiO 2 /Ce-Al-MCM-41 materials with varying contents of Ce (by impregnation) and TiO 2 loaded (by solid-state dispersion) on Al-MCM-41 support are prepared. The Ce modified and TiO 2 loaded composite systems are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectra (DRS) and X-ray photoelectron spectroscopy (XPS) techniques. The DRS and XPS of low Ce content (0.2-0.5 wt.%) modified Al-MCM-41 samples are showing more characteristic of Ce 3+ species wherein cerium in interaction with Al-MCM-41 and that of high Ce (0.8, 3.0 wt.%) content modified samples are showing the characteristic of both Ce 4+ and Ce 3+ species. A series of Ce-modified Al-MCM-41 and TiO 2 loaded composite catalysts are evaluated for photocatalytic degradation of phenol under UV irradiation. Low Ce content in Ce 3+ state on Al-MCM-41 is showing good photoactivity in comparison with high Ce content samples and pure ceria. The composite TiO 2 /Ce-Al-MCM-41 is showing enhanced degradation activity due decreased rate of electron-hole recombination on TiO 2 surface by the redox properties of cerium. The photocatalyst TiO 2 /Ce-Al-MCM-41 with an optimum of 10 wt.% TiO 2 and 0.3 wt.% Ce is showing maximum phenol degradation activity. The possible mechanism of phenol degradation on the composite photocatalyst is proposed.

  5. Partial hydrogenation of alkynes on highly selective nano-structured mesoporous silica MCM-41 composite catalyst

    International Nuclear Information System (INIS)

    Kojoori, R.K.

    2016-01-01

    In this research, we have developed a silica MCM-41/Metformin/Pd (II) nano composite catalyst for the selective hydrogenation of alkynes to the corresponding (Z)-alkenes under a mild condition of atmospheric pressure and room temperature. Firstly, functionalized Si-MCM-41 metformin catalyst with the optimum performance was prepared. Then, the synthesized catalyst was elucidated by X-ray powder diffraction, BET surface area, FT-IR spectrophotometer, Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) and applied in partial hydrogenation of different alkynes, with high selectivity and high yield. The products were characterized by 1H-NMR, 13C-NMR, FT-IR, and Mass Spectrometry (MS) that strongly approved the (Z)-double bond configuration of produced alkenes. This prepared catalyst is competitive with the best palladium catalysts known for the selective liquid phase hydrogenation of alkynes and can be easily recovered and regenerated with keeping high activity and selectivity over at least three cycles with a simple regeneration procedure. (author)

  6. Improvement of surface acidity and structural regularity of Zr-modified mesoporous MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Chen, L.F. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: chenlf2001@yahoo.com; Norena, L.E. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico); Navarrete, J. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Wang, J.A. [Laboratorio de Catalisis y Materiales, SEPI-ESIQIE, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico)

    2006-06-10

    This work reports the synthesis and surface characterization of a Zr-modified mesoporous MCM-41 solid with an ordered hexagonal arrangement, prepared through a templated synthesis route, using cetyltrimethylammonium chloride as the template. The surface features, crystalline structure, textural properties and surface acidity of the materials were characterized by in situ Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), N{sub 2} physisorption isotherms, {sup 29}Si MAS-NMR and in situ FT-IR of pyridine adsorption. It is evident that the surfactant cations inserted into the network of the solids during the preparation could be removed by calcination of the sample above 500 deg. C. The resultant material showed a large surface area of 680.6 m{sup 2} g{sup -1} with a uniform pore diameter distribution in a very narrow range centered at approximately 2.5 nm. Zirconium incorporation into the Si-MCM-41 framework, confirmed by {sup 29}Si MAS-NMR analysis, increased not only the wall thickness of the mesopores but also the long-range order of the periodically hexagonal structure. Both, Lewis and Broensted acid sites, were formed on the surface of the Zr-modified MCM-41 solid. Compared to Si-MCM-41 on which only very weak Lewis acid sites were formed, the densities of both Lewis and Broensted acid sites and the strength of the acidity on the Zr-modified sample were significantly increased, indicating that the incorporation of zirconium greatly enhances the acidity of the material.

  7. Mesoporous silica (MCM-41)-Fe2O3 as a novel magnetic nanosensor for determination of trace amounts of amino acids.

    Science.gov (United States)

    Hasanzadeh, Mohammad; Shadjou, Nasrin; Omidinia, Eskandar

    2013-08-01

    Magnetic (Fe2O3) mobile crystalline material-41 (MCM-41) was prepared and characterized using transmission electron microscopy (TEM) and nitrogen adsorption-desorption techniques. Due to the large surface area (1213 m(2)g(-1)) and remarkable electrocatalytic properties of MCM-41-Fe2O3, the MCM-41-Fe2O3 modified glassy carbon electrode (MCM-41-Fe2O3/GCE) exhibits potent electrocatalytic activity toward the electro-oxidation of amino acids. MCM-41-Fe2O3/GCE brings new capabilities for electrochemical sensing by combining the advantages of Fe2O3 magnetic nanoparticles and MCM-41 with very large surface area. Cyclic voltammetry, hydrodynamic amperometry and flow injection analysis used to determination of amino acids at higher concentration range. Fast response time, excellent catalytic activity, and ease of preparation are the advantages of the proposed amino acid sensor. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Dynamic behaviour of tantalum hydride supported on silica or MCM-41 in the metathesis of alkanes

    KAUST Repository

    Soignier, Sophie

    2014-01-01

    The metathesis of ethane and propane catalysed by tantalum hydride supported on silica or MCM-41 was studied under static and dynamic conditions. During the reaction, the rate decreased over time, indicating deactivation of the catalyst. The evolution of the catalytic system and surface species over time was monitored by various physico-chemical methods: FTIR, 13C NMR spectroscopy, elemental analysis and chemical reactivity. A carbonaceous deposit composed of unsaturated hydrocarbyl species was observed by 13C NMR. This deposit was responsible for poisoning of the catalyst. The deactivation of the catalyst proved more severe at higher temperatures and under static rather than dynamic conditions. A partial regeneration of the catalyst could be achieved during a series of repeated runs. Mechanistically, the deconvolution of the products\\' distribution over time indicated the occurrence of hydrogenolysis in the early stages of the reaction, while pure metathesis dominated later on. The hydrogen was supplied by the dehydrogenation of hydrocarbyl surface species involved in the deactivation process. © 2014 The Royal Society of Chemistry.

  9. Dynamic behaviour of tantalum hydride supported on silica or MCM-41 in the metathesis of alkanes

    KAUST Repository

    Soignier, Sophie; Saggio, Guillaume; Taoufik, Mostafa; Basset, Jean-Marie; Thivolle-Cazat, Jean

    2014-01-01

    The metathesis of ethane and propane catalysed by tantalum hydride supported on silica or MCM-41 was studied under static and dynamic conditions. During the reaction, the rate decreased over time, indicating deactivation of the catalyst. The evolution of the catalytic system and surface species over time was monitored by various physico-chemical methods: FTIR, 13C NMR spectroscopy, elemental analysis and chemical reactivity. A carbonaceous deposit composed of unsaturated hydrocarbyl species was observed by 13C NMR. This deposit was responsible for poisoning of the catalyst. The deactivation of the catalyst proved more severe at higher temperatures and under static rather than dynamic conditions. A partial regeneration of the catalyst could be achieved during a series of repeated runs. Mechanistically, the deconvolution of the products' distribution over time indicated the occurrence of hydrogenolysis in the early stages of the reaction, while pure metathesis dominated later on. The hydrogen was supplied by the dehydrogenation of hydrocarbyl surface species involved in the deactivation process. © 2014 The Royal Society of Chemistry.

  10. Catalytic co-pyrolysis of cellulose and polypropylene over all-silica mesoporous catalyst MCM-41 and Al-MCM-41.

    Science.gov (United States)

    Chi, Yongchao; Xue, Junjie; Zhuo, Jiankun; Zhang, Dahu; Liu, Mi; Yao, Qiang

    2018-08-15

    Fast pyrolysis is one of the most economical and efficient technologies to convert biomass to bio-oil and valuable chemical products. Co-pyrolysis with hydrogen rich materials such as plastics over zeolite catalysts is one of the significant solutions to various problems of bio-oil such as high oxygen content, low heat value and high acid content. This paper studied pyrolysis of cellulose and polypropylene (PP) separately and co-pyrolysis of cellulose and PP over MCM-41 and Al-MCM-41. The pyrolysis over different heating rates (10K/min, 20K/min, 30K/min) was studied by Thermogravimetry Analysis (TGA) and kinetic parameters were obtained by Coats-Redfern method and isoconversion method. TG and DTG data shows that the two catalysts advance the pyrolysis reaction of PP significantly and reduce its peak temperature of DTG curve from 458°C to 341°C. The activation energy of pyrolysis of PP also has a remarkable reduction over the two catalysts. Py-GC/MS method was used to obtain the product distribution of pyrolysis of cellulose and PP separately and co-pyrolysis of cellulose and PP over MCM-41 and Al-MCM-41 at constant temperature of 650°C. Experiment results proved that co-pyrolysis with PP bring significant changes to the product distribution of cellulose. Oxygenated compounds such as furans are decreased, while yields of olefins and aromatics increase greatly. The yield of furans increases with the catalysis of MCM-41 as for the pyrolysis of cellulose and co-pyrolysis, while the yield of olefins and aromatics both experience significant growth over Al-MCM-41, which can be explained by the abundant acid centers in Al-MCM-41. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica

    International Nuclear Information System (INIS)

    Gaydhankar, T.R.; Samuel, V.; Jha, R.K.; Kumar, R.; Joshi, P.N.

    2007-01-01

    Synthesis of mesoporous MCM-41 materials at room temperature using less expensive polymeric version of ethyl silicate (40 wt% SiO 2 ) as a source of silica was established. The influence of crucial synthesis parameters such as molar ratios of H 2 O/NH 4 OH, NH 4 OH/SiO 2 and CTMABr/SiO 2 in gel on the quality of the phase formed was investigated. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and low temperature N 2 adsorption-desorption isotherms have been employed to characterize the products. The magnitude of orderness, textural properties and thermal stability of the Si-MCM-41 samples prepared under identical judiciously pre-controlled synthesis conditions using ethyl silicate and conventional tetraethyl orthosilicate (TEOS) were assessed. Even though, ethyl silicate has proved to be suitable source for the preparation of MCM-41 at room temperature, there exists an optimum value of H 2 O/NH 4 OH for different NH 4 OH/SiO 2 molar ratios in the gel. Changes in the morphology were observed when NH 4 OH/SiO 2 , H 2 O/NH 4 OH molar ratios in the gels were changed

  12. Thermodynamic characteristics of the adsorption of organic molecules on modified MCM-41 adsorbents

    Science.gov (United States)

    Gus'kov, V. Yu.; Sukhareva, D. A.; Salikhova, G. R.; Karpov, S. I.; Kudasheva, F. Kh.; Roessner, F.; Borodina, E. V.

    2017-07-01

    The adsorption of a number of organic molecules on samples of MCM-41 adsorbent modified with dichloromethylphenylsilane and subsequently treated with sulfuric acid (MDCS) and N-trimethoxysilylpropyl- N, N, N-trimethylammonium chloride (MNM) is studied. Specific retention volumes equal to the Henry constant are determined by means of inverse gas chromatography at infinite dilution. The thermodynamic characteristics of adsorption, the dispersive and specific components of the Helmholtz energy of adsorption, and the increment of the methyl group to the heat of adsorption are calculated. It is shown that the grafting of aminosilane and phenylsilane groups enhances the forces of dispersion and reduces specific interactions. A greater drop in polarity is observed for MDCS than for MNM, due to the stronger polarity of amoinosilane; the enthalpy factor makes the main contribution to the adsorption of organic compounds on the investigated adsorbents. It is found that the MNM sample is capable of the irreversible adsorption of alcohols.

  13. Response to Extreme Temperatures of Mesoporous Silica MCM-41: Porous Structure Transformation Simulation and Modification of Gas Adsorption Properties.

    Science.gov (United States)

    Zhang, Shenli; Perez-Page, Maria; Guan, Kelly; Yu, Erick; Tringe, Joseph; Castro, Ricardo H R; Faller, Roland; Stroeve, Pieter

    2016-11-08

    Molecular dynamics (MD) and Monte Carlo (MC) simulations were applied together for the first time to reveal the porous structure transformation mechanisms of mesoporous silica MCM-41 subjected to temperatures up to 2885 K. Silica was experimentally characterized to inform the models and enable prediction of changes in gas adsorption/separation properties. MD simulations suggest that the pore closure process is activated by a collective diffusion of matrix atoms into the porous region, accompanied by bond reformation at the surface. Degradation is kinetically limited, such that complete pore closure is postponed at high heating rates. We experimentally observe decreased gas adsorption with increasing temperature in mesoporous silica heated at fixed rates, due to pore closure and structural degradation consistent with simulation predictions. Applying the Kissinger equation, we find a strong correlation between the simulated pore collapse temperatures and the experimental values which implies an activation energy of 416 ± 17 kJ/mol for pore closure. MC simulations give the adsorption and selectivity for thermally treated MCM-41, for N 2 , Ar, Kr, and Xe at room temperature within the 1-10 000 kPa pressure range. Relative to pristine MCM-41, we observe that increased surface roughness due to decreasing pore size amplifies the difference of the absolute adsorption amount differently for different adsorbate molecules. In particular, we find that adsorption of strongly interacting molecules can be enhanced in the low-pressure region while adsorption of weakly interacting molecules is inhibited. This then results in higher selectivity in binary mixture adsorption in mesoporous silica.

  14. Synthesis of AL-MCM-41 using gravel drilling the source of silica from wells drilling; Sintese do AL-MCM-41 usando como fonte de silica o cascalho de perfuracao de pocos de petroleo

    Energy Technology Data Exchange (ETDEWEB)

    Fontes, M.S.B.; Costa, C.C.; Melo, D.M.A.; Viana, L.M.; Viana, S.O.; Santos, L.M., E-mail: socorro.fontes@Yahoo.com.br [Universidade Federal do Rio grande do Norte (UFRN), Natal, RN (Brazil)

    2016-07-01

    The aim of this study was to synthesize Al-MCM-41 using gravel drilling as alternative source of silica, aiming at sustainable production and low cost. For hydrothermal synthesis of Al-MCM-41 was used gravel and sodium silicate as source of silica and sodium, respectively. The structural driver used was cetyltrimethylammonium bromide (CTMABr) and solvent distilled water. The hydrothermal synthesis was conducted at 100 ° C in a Teflon autoclave 45 ml jacketed stainless steel for a period of 120 hours with daily correcting pH (range 9-10) using 30% acetic acid. The material obtained was filtered, washed, dried at 100 ° C for 3 hours and then calcined at 550 ° C for 2 hours. Then it was characterized by XRD, FTIR and TG. For the results of characterization has been observed that the use of the gravel drilling as a source of silica was promising alternative for producing a mesoporous material with a high degree of hexagonal ordering. (author)

  15. Characterization of 12-molybdophosphoric acid supported on mesoporous silica MCM-41 and its catalytic performance in the synthesis of hydroquinone diacetate

    International Nuclear Information System (INIS)

    Ahmed, Awad I.; Samra, S.E.; El-Hakam, S.A.; Khder, A.S.; El-Shenawy, H.Z.; El-Yazeed, W.S. Abo

    2013-01-01

    12-molybdophosphoric acid (PMA) was supported on mesoporous molecular sieves MCM-41 by impregnation of 12-molybdophosphoric acid followed by calcination. The nanochannels of MCM-41 provide a large surface area for the solid state dispersion of 12-molybdophosphoric acid. The samples have been characterized by N 2 adsorption–desorption at −196 °C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and FT-IR measurements. The acidity and catalytic activity have been, respectively, examined by nonaqueous titration of n-butylamine in acetonitrile and synthesis of hydroquinone diacetate. The results showed that ordered hexagonal pore structure was observed in the synthesized MCM-41. Also the results indicate that PMA are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles while PMA retains its Keggin structure. On the other hand, with increasing the introduced PMA amount, the specific surface area decreases, and the mesoporous ordering of the samples become poor. Both the surface acidity and the catalytic activity sharply increase with the modification of MCM-41 by PMA but decrease by increasing the calcination temperature. The sample with 55 wt% PMA/MCM-41 calcined at 350 °C shows the highest acidity and catalytic activity.

  16. Amino-functionalized mesoporous MCM-41 silica as an efficient adsorbent for water treatment: batch and fixed-bed column adsorption of the nitrate anion

    Science.gov (United States)

    Ebrahimi-Gatkash, Mehdi; Younesi, Habibollah; Shahbazi, Afsaneh; Heidari, Ava

    2017-07-01

    In the present study, amino-functionalized Mobil Composite Material No. 41 (MCM-41) was used as an adsorbent to remove nitrate anions from aqueous solutions. Mono-, di- and tri-amino functioned silicas (N-MCM-41, NN-MCM-41 and NNN-MCM-41) were prepared by post-synthesis grafting method. The samples were characterized by means of X-ray powder diffraction, FTIR spectroscopy, thermogravimetric analysis, scanning electron microscopy and nitrogen adsorption-desorption. The effects of pH, initial concentration of anions, and adsorbent loading were examined in batch adsorption system. Results of adsorption experiments showed that the adsorption capacity increased with increasing adsorbent loading and initial anion concentration. It was found that the Langmuir mathematical model indicated better fit to the experimental data than the Freundlich. According to the constants of the Langmuir equation, the maximum adsorption capacity for nitrate anion by N-MCM-41, NN-MCM-41 and NNN-MCM-41 was found to be 31.68, 38.58 and 36.81 mg/g, respectively. The adsorption kinetics were investigated with pseudo-first-order and pseudo-second-order model. Adsorption followed the pseudo-second-order rate kinetics. The coefficients of determination for pseudo-second-order kinetic model are >0.99. For continuous adsorption experiments, NNN-MCM-41 adsorbent was used for the removal of nitrate anion from solutions. Breakthrough curves were investigated at different bed heights, flow rates and initial nitrate anion concentrations. The Thomas and Yan models were utilized to calculate the kinetic parameters and to predict the breakthrough curves of different bed height. Results from this study illustrated the potential utility of these adsorbents for nitrate removal from water solution.

  17. Magnetic behavior of iron-modified MCM-41 correlated with clustering processes from the wet impregnation method

    Energy Technology Data Exchange (ETDEWEB)

    Cuello, Natalia I.; Elías, Verónica R. [Centro de Investigación y Tecnología Química (CITeQ) (UTN-CONICET), Facultad Regional Córdoba. Maestro López y Cruz Roja Argentina, Ciudad Universitaria, Córdoba 5016 (Argentina); Winkler, Elin [Centro Atómico Bariloche, Comisión Nacional de Energía Atómica – CONICET, Avenue Bustillo 9500, San Carlos de Bariloche 8400 (Argentina); Pozo-López, Gabriela; Oliva, Marcos I. [Facultad de Matemática, Astronomía y Física, Universidad Nacional de Córdoba – IFEG, CONICET, Ciudad Universitaria, Córdoba 5000 (Argentina); Eimer, Griselda A., E-mail: geimer@frc.utn.edu.ar [Centro de Investigación y Tecnología Química (CITeQ) (UTN-CONICET), Facultad Regional Córdoba. Maestro López y Cruz Roja Argentina, Ciudad Universitaria, Córdoba 5016 (Argentina)

    2016-06-01

    Magnetic MCM-41 type mesoporous silica materials were synthetized and modified with different iron loadings by the wet impregnation method. The evolution of iron speciation, depending on the metal loading and associated with a particular magnetic behavior was investigated by M vs. H curves, FC–ZFC curves, EPR spectroscopy and other complementary techniques such as SEM, TEM, and chemisorption of pyridine followed by FT-IR studies. A superparamagnetic contribution was larger for the lower loadings suggesting the high dispersion of very small sized iron nanospecies. However, this contribution decreased with increasing metal loading due to the growth of magnetically blocked nanoparticles (hematite) on the outer surface. Finally, a bimodal size distribution for the superparamagnetic nanospecies could be inferred; then the anisotropy constant for this phase and the corresponding nanospecies sizes were estimated. - Highlights: • All samples showed a main superparamagnetic contribution. • The oxide particles grow at expense of superparamagnetic nanospecies. • Bimodal distribution of nanospecies in superparamagnetic regime was determined. • The anisotropy constant for superparamagnetic nanospecies was calculated.

  18. Grafting of [(64)Cu]-TPPF20 porphyrin complex on Functionalized nano-porous MCM-41 silica as a potential cancer imaging agent.

    Science.gov (United States)

    Fazaeli, Yousef; Feizi, Shahzad; Jalilian, Amir R; Hejrani, Ali

    2016-06-01

    Mesoporous silica, MCM-41, functionalized with 3-aminopropyltriethoxysilane (APTES) was investigated as a potential drug delivery system, using [(64)Cu]-5, 10, 15, 20-tetrakis penta fluorophenyl porphyrin complex. [(64)Cu]-TPPF20 complex was grafted on functionalized MCM-41. The product was characterized by paper chromatography, FTIR spectroscopy, low angle X-ray diffraction, CHN and TGA/DTA analyses and atomic force microscopy. The biological evaluations of the grafted complex, [(64)Cu]-TPPF20@NH2-MCM-41, were done in Fibrosarcoma tumor-bearing Sprague-Dawley rats using scarification studies and Sopha DST-XL Dual-Head SPECT system. The actual loading amount of aminopropyl groups was found about 1.6mmol per gram of final silica. The specific activity of the final compound was found to be 3Ci/g. Amine functionalized MCM-41 was found to be a good platform for theranostic radiopharmaceuticals such as copper-64 complexes. Considering the accumulation of the tracer in tumor cells, fast wash-out from normal tissues, the short half-life copper-64 and less imposed radiation doses to patients, [(64)Cu]-TPPF20@NH2-MCM-41 can potentially be a suitable candidate for tumor imaging applications and future PET studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Enhancement of Catalytic Performance of MCM-41 Synthesized with Rice Husk Silica by Addition of Titanium Dioxide for Photodegradation of Alachlor

    Directory of Open Access Journals (Sweden)

    Surachai Artkla

    2009-01-01

    Full Text Available Photocatalytic degradation of alachlor, a herbicide, in water on both bare TiO2 and TiO2 supported on mesoporous material, marked as TiO2/RH-MCM-41 were studied. The RH-MCM-41 support was synthesized from rice husk silica and other reagents by hydrothermal method. The required amount of titanium precursor (TiO2 P25 Degussa to give 10-60% was mixed with RH-MCM-41 and calcined at 300 °C for 6 h. The catalytic activities of TiO2 and TiO2/RH-MCM-41 for alachlor degradation were performed under UV radiation with wavelength of 300 nm. The ratio of catalyst weight to volume of alachlor solution was 1 g/L and all products were characterized by high performance liquid chromatograph. The reaction equilibrium was established in 30 min. in deionized water without adjusting the solution pH. The TiO2/RH-MCM-41 could adsorb alachlor more than the bare TiO2 (namely, 17% vs. 5% and the photocatalytic activity of alachlor degration on all TiO2/RH-MCM-41s was higher than that on the bare TiO2. By comparison per weight of TiO2, the 10%TiO2/RH-MCM-41 gave the highest alachlor conversion of 100% after 20 min. while 1% bare TiO2 showed conversion of 95%.

  20. Catalytic properties and acidity of modified MCM-41 mesoporous materials with low Si/Al ratio: heptane isomerisation

    Directory of Open Access Journals (Sweden)

    Ahmed Belhakem

    2006-06-01

    Full Text Available The catalytic properties and acidity of modified MCM-41 with a low Si/Al ratio and 0-95% NH4+ exchange were investigated. The samples were characterised by X-ray diffraction, scanning and transmission electron microscopy, and nitrogen adsorption. The acidity was studied by pyridine adsorption, temperature programmed desorption (TPD of ammonia, and infrared (IR spectroscopy. Adsorption of pyridine and IR spectroscopy indicated various types of Lewis and Brönsted acid sites. The density distribution of acid sites was determined by TPD. Both Lewis and Brönsted acid sites were found to be active in the heptane isomerisation. The presence of aluminium (low Si/Al combined to the ionic exchange between Na+ and NH4+ increases the acidity of MCM-41 materials. A close correlation between acidity and isomerisation was observed. Coke deposition, which reduces the activity, was also studied.

  1. Metal-Chelate Immobilization of Lipase onto Polyethylenimine Coated MCM-41 for Apple Flavor Synthesis.

    Science.gov (United States)

    Sadighi, Armin; Motevalizadeh, Seyed Farshad; Hosseini, Morteza; Ramazani, Ali; Gorgannezhad, Lena; Nadri, Hamid; Deiham, Behnaz; Ganjali, Mohammad Reza; Shafiee, Abbas; Faramarzi, Mohammad Ali; Khoobi, Mehdi

    2017-08-01

    An enzyme immobilized on a mesoporous silica nanoparticle can serve as a multiple catalyst for the synthesis of industrially useful chemicals. In this work, MCM-41 nanoparticles were coated with polyethylenimine (MCM-41@PEI) and further modified by chelation of divalent metal ions (M = Co 2+ , Cu 2+ , or Pd 2+ ) to produce metal-chelated silica nanoparticles (MCM-41@PEI-M). Thermomyces lanuginosa lipase (TLL) was immobilized onto MCM-41, MCM-41@PEI, and MCM-41@PEI-M by physical adsorption. Maximum immobilization yield and efficiency of 75 ± 3.5 and 65 ± 2.7% were obtained for MCM@PEI-Co, respectively. The highest biocatalytic activity at extremely acidic and basic pH (pH = 3 and 10) values were achieved for MCM-PEI-Co and MCM-PEI-Cu, respectively. Optimum enzymatic activity was observed for MCM-41@PEI-Co at 75 °C, while immobilized lipase on the Co-chelated support retained 70% of its initial activity after 14 days of storage at room temperature. Due to its efficient catalytic performance, MCM-41@PEI-Co was selected for the synthesis of ethyl valerate in the presence of valeric acid and ethanol. The enzymatic esterification yield for immobilized lipase onto MCM-41@PEI-Co was 60 and 53%, respectively, after 24 h of incubation in n-hexane and dimethyl sulfoxide media. Graphical Abstract Divalent metal chelated polyethylenimine coated MCM-41 (MCM-41@PEI-M) was used for immobilization of Thermomyces lanuginosa lipase catalyzing green apple flavor preparation.

  2. The investigation of MCM-48-type and MCM-41-type mesoporous silica as oral solid dispersion carriers for water insoluble cilostazol.

    Science.gov (United States)

    Wang, Yanzhu; Sun, Lizhang; Jiang, Tongying; Zhang, Jinghai; Zhang, Chen; Sun, Changshan; Deng, Yihui; Sun, Jin; Wang, Siling

    2014-06-01

    To explore the suitable application of MCM-41 (Mobil Composition of Matter number forty-one)-type and MCM-48-type mesoporous silica in the oral water insoluble drug delivery system. Cilostazol (CLT) as a model drug was loaded into synthesized MCM-48 (Mobil Composition of Matter number forty-eight) and commercial MCM-41 by three common methods. The obtained MCM-41, MCM-48 and CLT-loaded samples were characterized by means of nitrogen adsorption, thermogravimetric analysis, ultraviolet-visible spectrophotometry, scanning electron microscopy, transmission electron microscopy, differential scanning calorimetry and powder X-ray diffractometer. It was found that solvent evaporation method was preferred according to the drug loading efficiency and the maximum percent cumulative drug dissolution. MCM-48 with 3D cubic pore structure and MCM-41 with 2D long tubular structure are nearly spherical particles in 300-500 nm. Nevertheless, the silica carriers with similar large specific surface areas and concentrating pore size distributions (978.66 m(2)/g, 3.8 nm for MCM-41 and 1108.04 m(2)/g, 3.6 nm for MCM-48) exhibited different adsorption behaviors for CLT. The maximum percent cumulative drug release of the two CLT/silica solid dispersion (CLT-MCM-48 and CLT-MCM-41) was 63.41% and 85.78% within 60 min, respectively; while in the subsequent 12 h release experiment, almost 100% cumulative drug release were both obtained. In the pharmacokinetics aspect, the maximum plasma concentrations of CLT-MCM-48 reached 3.63 mg/L by 0.92 h. The AUC0-∞ values of the CLT-MCM-41 and CLT-MCM-48 were 1.14-fold and 1.73-fold, respectively, compared with the commercial preparation. Our findings suggest that MCM-41-type and MCM-48-type mesoporous silica have great promise as solid dispersion carriers for sustained and immediate release separately.

  3. Translational and rotational dynamics of water in mesoporous silica materials: MCM-41-S and MCM-48-S

    International Nuclear Information System (INIS)

    Faraone, Antonio; Liu Li; Mou, C.-Y.; Shih, P.-C.; Copley, John R.D.; Chen, S.-H.

    2003-01-01

    We investigated the translational and rotational dynamics of water molecules in mesoporous silica materials MCM-41-S and MCM-48-S using the incoherent quasielastic neutron scattering technique. The range of wave vector transfers Q covered in the measurements was from 0.27 to 1.93 Aa -1 broad enough to detect both the translational and rotational contributions to the scattering. We used the relaxing-cage models for both translational and rotational motions which we developed earlier, to analyze the QENS spectra and investigated water dynamics in a supercooled range from 250 to 280 K. The results show a marked slowing down of both the translational and rotational relaxation times, and an increasing effect of confinement on the translational motion, as the temperature is lowered

  4. Structure and thermal performance of poly(ethylene glycol) alkyl ether (Brij)/porous silica (MCM-41) composites as shape-stabilized phase change materials

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lingjian; Shi, Haifeng, E-mail: haifeng.shi@gmail.com; Li, Weiwei; Han, Xu; Zhang, Xingxiang, E-mail: zhangpolyu@gmail.com

    2013-10-20

    Graphical abstract: The maximum 50 wt% Brij58 is loaded into the porous MCM-41 networks, and a new peak at 18.8° in XRD patterns confirmed the changes of crystallization behavior of Brij58 against the bulk one. - Highlights: • Poly(ethylene glycol) hexadecyl ether and poly(ethylene glycol) octadecyl ether have the good thermal storage ability. • New peak at 18.8° proved the coexisted confined crystallization and nucleation-induced crystallization. • Poly(ethylene glycol) alkyl ether/MCM-41 PCMs exhibits the good thermal stability. - Abstract: A series of shape-stabilized phase change materials (PCMs), composed of poly(ethylene glycol) hexadecyl ether (Brij58) or poly(ethylene glycol) octadecyl ether (Brij76) and porous silica (MCM-41), were prepared by the physical mixing method. The structure, thermal stability, energy storage ability and crystallization behavior of these composites are deeply investigated and characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), wide-angle X-ray diffraction (WAXD) and thermogravimetric analysis (TGA). Obvious phase transition behavior and energy storage capability are observed for these Brij/MCM-41 composites, and the heat storage efficiency increased with the weight of Brij component. New peak at 18.8° demonstrated that the pore size and the surface adsorption ability of MCM-41 affect the crystallization behavior of Brij molecule. The crystalline structure and energy storage ability of these Brij/MCM-41 composites are discussed based on the crystallization process.

  5. A study of some fundamental physicochemical variables on the morphology of mesoporous silica nanoparticles MCM-41 type

    Science.gov (United States)

    Beltrán-Osuna, Ángela A.; Gómez Ribelles, José L.; Perilla, Jairo E.

    2017-12-01

    All variables affecting the morphology of mesoporous silica nanoparticles (MSN) should be carefully analyzed in order to truly tailored design their mesoporous structure according to their final use. Although complete control on MCM-41 synthesis has been already claimed, reproducibility and repeatability of results remain a big issue due to the lack of information reported in literature. Stirring rate, reaction volume, and system configuration (i.e., opened or closed reactor) are three variables that are usually omitted, making the comparison of product characteristics difficult. Specifically, the rate of solvent evaporation is seldom disclosed, and its influence has not been previously analyzed. These variables were systematically studied in this work, and they were proven to have a fundamental impact on final particle morphology. Hence, a high degree of circularity ( C = 0.97) and monodispersed particle size distributions were only achieved when a stirring speed of 500 rpm and a reaction scale of 500 mL were used in a partially opened system, for a 2 h reaction at 80 °C. Well-shaped spherical mesoporous silica nanoparticles with a diameter of 95 nm, a pore size of 2.8 nm, and a total surface area of 954 m2 g-1 were obtained. Final characteristics made this product suitable to be used in biomedicine and nanopharmaceutics, especially for the design of drug delivery systems.

  6. Uranium adsorption studies on aminopropyl modified mesoporous sorbent (NH{sub 2}-MCM-41) using statistical design method

    Energy Technology Data Exchange (ETDEWEB)

    Sert, Senol, E-mail: senol.sert@ege.edu.t [Ege University, Institute of Nuclear Sciences, 35100 Bornova-Izmir (Turkey); Eral, Meral [Ege University, Institute of Nuclear Sciences, 35100 Bornova-Izmir (Turkey)

    2010-11-30

    MCM-41 has been synthesized and modified in order to graft amine groups on its surface. The modified NH{sub 2}-MCM-41 adsorbent was characterized by using XRD, SEM, surface area and porosity analyzer, and FT-IR. This characterized adsorbent was investigated for uranium adsorption using the batch method. The central composite design (CCD) combined with the response surface methodology (RSM) was selected to determine the effects of parameters and their interactions for the removal of UO{sub 2}{sup 2+} ions. The optimum values of the parameters determined were 4.2 for the initial pH, 60 {sup o}C for the temperature, 90 mg L{sup -1} for the initial concentration and 173 min for the shaking time using the response surface methodology. {Delta}H{sup o} and {Delta}S{sup o} were calculated from the slope and the intercept of plots of ln K{sub d} versus 1/T. The isotherm models, Langmuir, Freundlich, Dubinin-Radushkevich (D-R) have been studied to explain the adsorption characteristics.

  7. Miniaturized solid-phase extraction of macrolide antibiotics in honey and bovine milk using mesoporous MCM-41 silica as sorbent.

    Science.gov (United States)

    Du, Li-Jing; Yi, Ling; Ye, Li-Hong; Chen, Yu-Bo; Cao, Jun; Peng, Li-Qing; Shi, Yu-Ting; Wang, Qiu-Yan; Hu, Yu-Han

    2018-02-16

    A simple and effective method of miniaturized solid-phase extraction (mini-SPE) was developed for the simultaneous purification and enrichment of macrolide antibiotics (MACs) (i.e. azithromycin, clarithromycin, erythromycin, lincomycin and roxithromycin) from honey and skim milk. Mesoporous MCM-41 silica was synthesized and used as sorbent in mini-SPE. Several key parameters affecting the performance of mini-SPE procedure were thoroughly investigated, including sorbent materials, amount of sorbent and elution solvents. Under the optimized condition, satisfactory linearity (r 2  > 0.99), acceptable precision (RSDs, 0.3-7.1%), high sensitivity (limit of detection in the range of 0.01-0.76 μg/kg), and good recoveries (83.21-105.34%) were obtained. With distinct advantages of simplicity, reliability and minimal sample requirement, the proposed mini-SPE procedure coupled with ultrahigh performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry could become an alternative tool to analyze the residues of MACs in complex food matrixes. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Ultrasonic-assisted synthesis of novel nanocomposite of poly(vinyl alcohol) and amino-modified MCM-41: A green adsorbent for Cd(II) removal.

    Science.gov (United States)

    Soltani, Roozbeh; Dinari, Mohammad; Mohammadnezhad, Gholamhossein

    2018-01-01

    Amino-modified MCM-41/poly(vinyl alcohol) nanocomposite (M-MCM-41/PVOH NC) was developed for the adsorption of Cd(II) from aqueous media. M-MCM-41/PVOH NC was prepared through ultrasonic-assisted and simple blending procedure with economical and environmentally friendly polymer. The as-prepared adsorbent was characterized by FT-IR, TEM, FE-SEM and TGA. The contact time, solution pH and initial concentration of Cd(II) were found to affect the adsorption of Cd(II) from aqueous media. Kinetic studies were carried out and pseudo-first-order (PFO), pseudo-second-order (PSO), Elovich, and intra-particle diffusion (IPD) reaction kinetic models were examined. The kinetic results revealed that the adsorption of Cd(II) onto M-MCM-41/PVOH NC followed PSO kinetic model and is a chemical adsorption. The equilibrium adsorption data were evaluated by different isotherms viz. Langmuir, Freundlich, and Dubinin Radushkevich (D-R) equations. The equilibrium data fitted better with the Langmuir isotherm and the maximum adsorption capacity of M-MCM-41/PVOH NC at 298K was calculated to be 46.73mgg -1 for Cd(II) on a typical saturated monomolecular layer with a fixed number of localized adsorption sites. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Uniform Surface Modification of 3D Bioglass®-Based Scaffolds with Mesoporous Silica Particles (MCM-41) for Enhancing Drug Delivery Capability

    Science.gov (United States)

    Boccardi, Elena; Philippart, Anahí; Juhasz-Bortuzzo, Judith A.; Beltrán, Ana M.; Novajra, Giorgia; Vitale-Brovarone, Chiara; Spiecker, Erdmann; Boccaccini, Aldo R.

    2015-01-01

    The design and characterization of a new family of multifunctional scaffolds based on bioactive glass (BG) of 45S5 composition for bone tissue engineering and drug delivery applications are presented. These BG-based scaffolds are developed via a replication method of polyurethane packaging foam. In order to increase the therapeutic functionality, the scaffolds were coated with mesoporous silica particles (MCM-41), which act as an in situ drug delivery system. These sub-micron spheres are characterized by large surface area and pore volume with a narrow pore diameter distribution. The solution used for the synthesis of the silica mesoporous particles was designed to obtain a high-ordered mesoporous structure and spherical shape – both are key factors for achieving the desired controlled drug release. The MCM-41 particles were synthesized directly inside the BG-based scaffolds, and the drug-release capability of this combined system was evaluated. Moreover, the effect of MCM-41 particle coating on the bioactivity of the BG-based scaffolds was assessed. The results indicate that it is possible to obtain a multifunctional scaffold system characterized by high and interconnected porosity, high bioactivity, and sustained drug delivery capability. PMID:26594642

  10. Zinc(II) phthalocyanines immobilized in mesoporous silica Al-MCM-41 and their applications in photocatalytic degradation of pesticides

    International Nuclear Information System (INIS)

    Silva, M.; Calvete, M.J.F.; Gonçalves, N.P.F.; Burrows, H.D.; Sarakha, M.; Fernandes, A.; Ribeiro, M.F.; Azenha, M.E.; Pereira, M.M.

    2012-01-01

    Highlights: ► Complete immobilization of zinc(II) phthalocyanines accomplished in Al-MCM-41. ► Efficient photodegradation of model pesticides achieved using 365 nm irradiation. ► Sodium azide experiments showed the involvement of singlet oxygen ( 1 O 2 ). - Abstract: In the present study the authors investigated a set of three new zinc(II) phthalocyanines (zinc(II) tetranitrophthalocyanine (ZnTNPc), zinc(II) tetra(phenyloxy)phthalocyanine (ZnTPhOPc) and the tetraiodide salt of zinc(II)tetra(N,N,N-trimethylaminoethyloxy) phthalocyaninate (ZnTTMAEOPcI)) immobilized into Al-MCM-41 prepared via ship-in-a-bottle methodology. The samples were fully characterized by diffuse reflectance-UV–vis spectroscopy (DRS-UV–vis), luminescence, thermogravimetric analysis (TG/DSC), N 2 adsorption techniques and elemental analysis. A comparative study was made on the photocatalytic performance upon irradiation within the wavelength range 320–460 nm of these three systems in the degradation of pesticides fenamiphos and pentachlorophenol. ZnTNPc-Al-MCM-41 and ZnTTMAEOPcI-Al-MCM-41 were found to be the most active systems, with the best performance observed with the immobilized cationic phthalocyanine, ZnTTMAEOPcI-Al-MCM-41. This system showed high activity even after three photocatalytic cycles. LC–MS product characterization and mechanistic studies indicate that singlet oxygen ( 1 O 2 ), produced by excitation of these immobilized photosensitizers, is a key intermediate in the photocatalytic degradation of both pesticides.

  11. Controlled drug release on amine functionalized spherical MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Szegedi, Agnes, E-mail: szegedi@chemres.hu [Institute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, Hungarian Academy of Sciences, 1025 Budapest, Pusztaszeri ut 59-67 (Hungary); Popova, Margarita; Goshev, Ivan [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, Sofia (Bulgaria); Klebert, Szilvia [Institute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, Hungarian Academy of Sciences, 1025 Budapest, Pusztaszeri ut 59-67 (Hungary); Mihaly, Judit [Institute of Molecular Pharmacology, Research Centre for Natural Sciences, Hungarian Academy of Sciences, 1025 Budapest, Pusztaszeri ut 59-67 (Hungary)

    2012-10-15

    MCM-41 silica with spherical morphology and small particle sizes (100 nm) was synthesized and modified by post-synthesis method with different amounts of 3-aminopropyltriethoxysilane (APTES). A comparative study of the adsorption and release of a model drug, ibuprofen, was carried out. The modified and drug loaded mesoporous materials were characterized by XRD, TEM, N{sub 2} physisorption, elemental analysis, thermal analysis and FT-IR spectroscopy. A new method was developed for the quantitative determination of amino groups in surface modified mesoporous materials by the ninhydrin reaction. Good correlation was found between the amino content of the MCM-41 materials determined by the ninhydrin method and their ibuprofen adsorption capacity. Amino modification resulted in high degree of ibuprofen loading and slow release rate in comparison to the parent non-modified MCM-41. - Graphical abstract: Determination of surface amino groups by ninhidrin method. Highlights: Black-Right-Pointing-Pointer Spherical MCM-41 modified by different amounts of APTES was studied. Black-Right-Pointing-Pointer Ibuprofen (IBU) adsorption and release characteristics was tested. Black-Right-Pointing-Pointer The ninhydrin reaction was used for the quantitative determination of amino groups. Black-Right-Pointing-Pointer Stoichiometric amount of APTES is enough for totally covering the surface with amino groups. Black-Right-Pointing-Pointer Good correlation was found between the amino content and IBU adsorption capacity.

  12. Controlled drug release on amine functionalized spherical MCM-41

    International Nuclear Information System (INIS)

    Szegedi, Agnes; Popova, Margarita; Goshev, Ivan; Klébert, Szilvia; Mihály, Judit

    2012-01-01

    MCM-41 silica with spherical morphology and small particle sizes (100 nm) was synthesized and modified by post-synthesis method with different amounts of 3-aminopropyltriethoxysilane (APTES). A comparative study of the adsorption and release of a model drug, ibuprofen, was carried out. The modified and drug loaded mesoporous materials were characterized by XRD, TEM, N 2 physisorption, elemental analysis, thermal analysis and FT-IR spectroscopy. A new method was developed for the quantitative determination of amino groups in surface modified mesoporous materials by the ninhydrin reaction. Good correlation was found between the amino content of the MCM-41 materials determined by the ninhydrin method and their ibuprofen adsorption capacity. Amino modification resulted in high degree of ibuprofen loading and slow release rate in comparison to the parent non-modified MCM-41. - Graphical abstract: Determination of surface amino groups by ninhidrin method. Highlights: ► Spherical MCM-41 modified by different amounts of APTES was studied. ► Ibuprofen (IBU) adsorption and release characteristics was tested. ► The ninhydrin reaction was used for the quantitative determination of amino groups. ► Stoichiometric amount of APTES is enough for totally covering the surface with amino groups. ► Good correlation was found between the amino content and IBU adsorption capacity.

  13. Zero-valent Fe confined mesoporous silica nanocarriers (Fe(0) @ MCM-41) for targeting experimental orthotopic glioma in rats

    Science.gov (United States)

    Shevtsov, M. A.; Parr, M. A.; Ryzhov, V. A.; Zemtsova, E. G.; Arbenin, A. Yu; Ponomareva, A. N.; Smirnov, V. M.; Multhoff, G.

    2016-01-01

    Mesoporous silica nanoparticles (MSNs) impregnated with zero-valent Fe (Fe(0) @ MCM-41) represent an attractive nanocarrier system for drug delivery into tumor cells. The major goal of this work was to assess whether MSNs can penetrate the blood-brain barrier in a glioblastoma rat model. Synthesized MSNs nanomaterials were characterized by energy dispersive X-ray spectroscopy, measurements of X-ray diffraction, scanning electron microscopy and Mössbauer spectroscopy. For the detection of the MSNs by MR and for biodistribution studies MSNs were labeled with zero-valent Fe. Subsequent magnetometry and nonlinear-longitudinal-response-M2 (NLR-M2) measurements confirmed the MR negative contrast enhancement properties of the nanoparticles. After incubation of different tumor (C6 glioma, U87 glioma, K562 erythroleukemia, HeLa cervix carcinoma) and normal cells such as fibroblasts and peripheral blood mononuclear cells (PBMCs) MSNs rapidly get internalized into the cytosol. Intracellular residing MSNs result in an enhanced cytotoxicity as Fe(0) @ MCM-41 promote the reactive oxygen species production. MRI and histological studies indicated an accumulation of intravenously injected Fe(0) @ MCM-41 MSNs in orthotopic C6 glioma model. Biodistribution studies with measurements of second harmonic of magnetization demonstrated an increased and dose-dependent retention of MSNs in tumor tissues. Taken together, this study demonstrates that MSNs can enter the blood-brain barrier and accumulate in tumorous tissues. PMID:27386761

  14. Analysis of nitrogen and carbon tetrachloride adsorption isotherms and pore size distribution for siliceous MCM-41 synthesized from rice husk silica

    Directory of Open Access Journals (Sweden)

    Siriluk Chiarakorn

    2004-02-01

    Full Text Available RH-MCM-41 particles were synthesized using sodium silicate prepared from rice husk as a silica source and hexadecyltrimethylammonium bromide (CTAB as a surfactant. The molar compositions were 1.0SiO2: 1.1NaOH: 0.13CTAB: 0.12H2O. This material was used for adsorption isotherm studies of carbon tetrachloride (CT at 25 oC using a magnetically coupled microbalance, and compared with adsorption isotherms using nitrogen at 77 K. The CT isotherms were classified as reversible Type V isotherms, and the nitrogen adsorption isotherm was Type IVc. Capillary condensation was found in a very narrow pressure range, indicating the presence of nearly uniform pores in the RH-MCM-41 particles, which agrees very well with TEM results. The surface area estimated by using the BET method was (800 ± 8 m2 g-1. Pore size distributions (PSD of nitrogen and CT adsorption isotherms for a series of MCM-41 were calculated by using method recommended by Naono and Hakuman (1997. The pore size distributions from the nitrogen isotherm using the BJH and Naono methods showed quite narrow pore diameter distributions, centered around 27 and 29 Å, respectively. Similarly, the peak pore diameters calculated from CT isotherms using the BJH and Naono methods were 24 and 28 Å. It was found that the PSDs analyzed by the BJH method were underestimated compared to that from Naono method.

  15. Modified silica-based heterogeneous catalysts for etherification of glycerol

    Energy Technology Data Exchange (ETDEWEB)

    Gholami, Zahra, E-mail: zahra.gholami@petronas.com.my [Centralized Analytical Laboratory, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750 Tronoh, Perak (Malaysia); Abdullah, Ahmad Zuhairi, E-mail: chzuhairi@usm.my; Gholami, Fatemeh, E-mail: fgholami59@gmail.com [School of Chemical Engineering, Universiti Sains Malaysia, Engineering Campus,14300 Nibong Tebal, Penang (Malaysia); Vakili, Mohammadtaghi, E-mail: farshid3601@gmail.com [School of Industrial Technology, Universiti Sains Malaysia, 11800 Penang (Malaysia)

    2015-07-22

    The advent of mesoporous silicas such as MCM-41 has provided new opportunities for research into supported metal catalysis. The loading of metals into framework structures and particularly into the pores of porous molecular sieves, has long been of interest because of their potential catalytic activity. Stable heterogeneous mesoporous basic catalysts were synthesized by wet impregnation of MCM-41 with calcium nitrate and lanthanum nitrate. The surface and structural properties of the prepared catalysts were characterized using BET surface analysis, SEM and TEM. MCM-41 and modified MCM-41 were used in the solventless etherification of glycerol to produce diglycerol as the desired product. The reaction was performed at 250 °C for 8 h, and catalyst activity was evaluated. Catalytic etherification over the 20%Ca{sub 1.6}La{sub 0.6}/MCM-41 catalyst resulted in the highest glycerol conversion of 91% and diglycerol yield of 43%.

  16. Modified silica-based heterogeneous catalysts for etherification of glycerol

    International Nuclear Information System (INIS)

    Gholami, Zahra; Abdullah, Ahmad Zuhairi; Gholami, Fatemeh; Vakili, Mohammadtaghi

    2015-01-01

    The advent of mesoporous silicas such as MCM-41 has provided new opportunities for research into supported metal catalysis. The loading of metals into framework structures and particularly into the pores of porous molecular sieves, has long been of interest because of their potential catalytic activity. Stable heterogeneous mesoporous basic catalysts were synthesized by wet impregnation of MCM-41 with calcium nitrate and lanthanum nitrate. The surface and structural properties of the prepared catalysts were characterized using BET surface analysis, SEM and TEM. MCM-41 and modified MCM-41 were used in the solventless etherification of glycerol to produce diglycerol as the desired product. The reaction was performed at 250 °C for 8 h, and catalyst activity was evaluated. Catalytic etherification over the 20%Ca 1.6 La 0.6 /MCM-41 catalyst resulted in the highest glycerol conversion of 91% and diglycerol yield of 43%

  17. Improving structural stability of water-dispersed MCM-41 silica nanoparticles through post-synthesis pH aging process

    Energy Technology Data Exchange (ETDEWEB)

    Varache, Mathieu; Bezverkhyy, Igor [UMR 6303 CNRS-Université Bourgogne Franche-Comté, Laboratoire Interdisciplinaire Carnot de Bourgogne (France); Bouyer, Florence [Inserm U866, Equipe Chimiothérapie, métabolisme des lipides et réponse immunitaire anti-tumorale (France); Chassagnon, Rémi; Baras, Florence; Bouyer, Frédéric, E-mail: frederic.bouyer@u-bourgogne.fr [UMR 6303 CNRS-Université Bourgogne Franche-Comté, Laboratoire Interdisciplinaire Carnot de Bourgogne (France)

    2015-09-15

    The colloidal and structural stabilities of MCM-41 mesoporous silica nanoparticles (MSNs) are of great importance in order to prepare optimal nanovectors. In this paper, MSNs (approximatively 160 nm in diameter) were synthesized using n-cetyltrimethylammonium bromide as a template and tetraethyl orthosilicate as a silica source under high N{sub 2} flow (MSN/N{sub 2}) to obtain stable dispersions in water. The degradation of the porous nanoparticles was investigated by immersion in water. The morphology and the porous structure were studied by TEM, XRD, N{sub 2} sorption, and {sup 29}Si MAS NMR and were compared to that of MSNs prepared in ambient air (MSN/air). The volumetric properties of the MSN/N{sub 2} after 1 day in water were drastically more decreased than MSN/air (a pore volume decrease of 85 % for MSN/N{sub 2} and 59 % for MSN/air) and the 2D-hexagonal porous structure was totally lost. Furthermore, synthesizing MSNs under a high N{sub 2} flow leads to a decrease in the synthesis yield (45 % MSN/N{sub 2} and 75 % for MSN/air). The lower structural stability of the MSN/N{sub 2} is explained by the lower polycondensation degree of the MSN/N{sub 2} observed by {sup 29}Si MAS NMR (Q{sup 4}/Q{sup 3} = 0.86 for MSN/N{sub 2} and 1.61 for MSN/air) and the lower silica molar ratio in the nanomaterials (SiO{sub 2}/CTA = 3.9 for MSN/N{sub 2} 7.1 for MSN/air). This allows for enhanced solubilization of silica in water. Four strategies were hence evaluated in order to reinforce the porous structure of the MSNs. Among them, the most efficient route was based on a pH adjustment of the colloidal suspension (pH 7.5) after 2 h of synthesis without any purification and while keeping a N{sub 2} static atmosphere (called MSN/N{sub 2}/7.5). After 1 day in water, the volumetric and structural properties of MSN/N{sub 2}/7.5 were similar to that obtained for MSN/air. The improvement of the stability arose as a result of the increase in the silica condensation (Q{sup 4

  18. Zinc(II) phthalocyanines immobilized in mesoporous silica Al-MCM-41 and their applications in photocatalytic degradation of pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Silva, M. [Departamento de Quimica, Universidade de Coimbra, Rua Larga, 3004-535 Coimbra (Portugal); Laboratoire de Photochimie Moleculaire et Macromoleculaire, UMR CNRS 6505, Universite Blaise Pascal, F-63177 Aubiere cedex (France); Calvete, M.J.F.; Goncalves, N.P.F.; Burrows, H.D. [Departamento de Quimica, Universidade de Coimbra, Rua Larga, 3004-535 Coimbra (Portugal); Sarakha, M. [Laboratoire de Photochimie Moleculaire et Macromoleculaire, UMR CNRS 6505, Universite Blaise Pascal, F-63177 Aubiere cedex (France); Fernandes, A.; Ribeiro, M.F. [Instituto para a Biotecnologia e Bioengenharia, Centro para a Engenharia Biologica e Quimica, Instituto Superior Tecnico - Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Azenha, M.E., E-mail: meazenha@ci.uc.pt [Departamento de Quimica, Universidade de Coimbra, Rua Larga, 3004-535 Coimbra (Portugal); Pereira, M.M., E-mail: mmpereira@qui.uc.pt [Departamento de Quimica, Universidade de Coimbra, Rua Larga, 3004-535 Coimbra (Portugal)

    2012-09-30

    Highlights: Black-Right-Pointing-Pointer Complete immobilization of zinc(II) phthalocyanines accomplished in Al-MCM-41. Black-Right-Pointing-Pointer Efficient photodegradation of model pesticides achieved using 365 nm irradiation. Black-Right-Pointing-Pointer Sodium azide experiments showed the involvement of singlet oxygen ({sup 1}O{sub 2}). - Abstract: In the present study the authors investigated a set of three new zinc(II) phthalocyanines (zinc(II) tetranitrophthalocyanine (ZnTNPc), zinc(II) tetra(phenyloxy)phthalocyanine (ZnTPhOPc) and the tetraiodide salt of zinc(II)tetra(N,N,N-trimethylaminoethyloxy) phthalocyaninate (ZnTTMAEOPcI)) immobilized into Al-MCM-41 prepared via ship-in-a-bottle methodology. The samples were fully characterized by diffuse reflectance-UV-vis spectroscopy (DRS-UV-vis), luminescence, thermogravimetric analysis (TG/DSC), N{sub 2} adsorption techniques and elemental analysis. A comparative study was made on the photocatalytic performance upon irradiation within the wavelength range 320-460 nm of these three systems in the degradation of pesticides fenamiphos and pentachlorophenol. ZnTNPc-Al-MCM-41 and ZnTTMAEOPcI-Al-MCM-41 were found to be the most active systems, with the best performance observed with the immobilized cationic phthalocyanine, ZnTTMAEOPcI-Al-MCM-41. This system showed high activity even after three photocatalytic cycles. LC-MS product characterization and mechanistic studies indicate that singlet oxygen ({sup 1}O{sub 2}), produced by excitation of these immobilized photosensitizers, is a key intermediate in the photocatalytic degradation of both pesticides.

  19. 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

  20. Amino-functionalized MCM-41 and MCM-48 for the removal of chromate and arsenate.

    Science.gov (United States)

    Benhamou, A; Basly, J P; Baudu, M; Derriche, Z; Hamacha, R

    2013-08-15

    The aim of the present work was to investigate the efficiency of three amino-functionalized (hexadecylamine, dodecylamine, and dimethyldodecylamine) mesoporous silicas (MCM-41 and MCM-48) toward the adsorption of arsenate and chromate. Hexadecylamine-functionalized materials were characterized; BET surface areas, pore volumes, and sizes decreased with the functionalization, whereas XRD patterns show that the hexagonal structure of MCM-41 and the cubic structure of MCM-48 were not modified. The zeta potential decreases with pH and the highest arsenate and chromate removal was observed at the lowest pHs. Adsorption of chromium and arsenate was significantly enhanced after functionalization and amino-functionalized MCM-41 adsorb larger amounts of arsenate when compared to expanded MCM-48 materials. Chromate sorption capacities increased with the chain length and the larger capacities were obtained with hexadecylamine-functionalized mesoporous silicas. Mesoporous silicas modified by dimethyldodecylamine exhibited the higher arsenate sorption capacities. Copyright © 2013 Elsevier Inc. All rights reserved.

  1. Elimination of ketone vapors by adsorption on spherical MCM-41 and MCM-48 silicas decorated with thermally activated poly(furfuryl alcohol)

    International Nuclear Information System (INIS)

    Machowski, Kamil; Kuśtrowski, Piotr; Dudek, Barbara; Michalik, Marek

    2015-01-01

    Spherical MCM-41 and MCM-48 silicas with different arrangements of mesopores were synthesized in a water–alcohol solution of surfactant by the hard-templating method. The pore structure and morphology of the obtained materials were confirmed by powder X-ray diffraction (XRD), low-temperature adsorption of nitrogen and scanning electron microscopy (SEM). The surface of mesoporous silicas was decorated with small amounts of poly(furfuryl alcohol) (PFA), which was introduced by the precipitation polymerization and subsequently thermally activated at 523 K to form stable C=O surface species detected by FTIR spectroscopy. The adsorption capacity of the PFA/silica composites in the elimination of various ketone (acetone, methyl-ethyl ketone and methyl-isobutyl ketone) vapors was compared to the effectiveness of pristine silicas. It was found that the modification of silicas by thermally degraded PFA enhanced their adsorption capacity. This effect was attributed to the appearance of another type of surface centers (namely carbonyl groups), which beside silanols interact with ketone molecules via hydrogen bonds. DRIFT spectra showed that a ketone molecule is bonded on silanol species in its keto form, whereas on carbonyl functionalities in enol one. - Highlights: • Surface of spherical MCM-type silicas was decorated with poly(furfuryl alcohol). • Thermal degradation of deposited polymer resulted in formation of C=O species. • Carbonyl groups enhanced adsorption capacity of MCM-41 and MCM-48 silicas. • Adsorption of ketones in enol or keto forms was revealed by DRIFT measurements.

  2. Elimination of ketone vapors by adsorption on spherical MCM-41 and MCM-48 silicas decorated with thermally activated poly(furfuryl alcohol)

    Energy Technology Data Exchange (ETDEWEB)

    Machowski, Kamil [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków (Poland); Kuśtrowski, Piotr, E-mail: kustrows@chemia.uj.edu.pl [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków (Poland); Dudek, Barbara [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków (Poland); Michalik, Marek [Institute of Geological Sciences, Jagiellonian University, Oleandry 2a, 30-063 Kraków (Poland)

    2015-09-01

    Spherical MCM-41 and MCM-48 silicas with different arrangements of mesopores were synthesized in a water–alcohol solution of surfactant by the hard-templating method. The pore structure and morphology of the obtained materials were confirmed by powder X-ray diffraction (XRD), low-temperature adsorption of nitrogen and scanning electron microscopy (SEM). The surface of mesoporous silicas was decorated with small amounts of poly(furfuryl alcohol) (PFA), which was introduced by the precipitation polymerization and subsequently thermally activated at 523 K to form stable C=O surface species detected by FTIR spectroscopy. The adsorption capacity of the PFA/silica composites in the elimination of various ketone (acetone, methyl-ethyl ketone and methyl-isobutyl ketone) vapors was compared to the effectiveness of pristine silicas. It was found that the modification of silicas by thermally degraded PFA enhanced their adsorption capacity. This effect was attributed to the appearance of another type of surface centers (namely carbonyl groups), which beside silanols interact with ketone molecules via hydrogen bonds. DRIFT spectra showed that a ketone molecule is bonded on silanol species in its keto form, whereas on carbonyl functionalities in enol one. - Highlights: • Surface of spherical MCM-type silicas was decorated with poly(furfuryl alcohol). • Thermal degradation of deposited polymer resulted in formation of C=O species. • Carbonyl groups enhanced adsorption capacity of MCM-41 and MCM-48 silicas. • Adsorption of ketones in enol or keto forms was revealed by DRIFT measurements.

  3. Promotion effect of palladium on Co{sub 3}O{sub 4} incorporated within mesoporous MCM-41 silica for CO Oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Hassan, Hassan M.A., E-mail: hassan.hassan@suezuniv.edu.eg [Department of Chemistry, Faculty of Science, Suez University, Suez (Egypt); Institut fur Anorganische Chemie und Strukturchemie, Heinrich-Heine Universitat, Dusseldorf (Germany); Betiha, Mohamed A. [Egyptian Petroleum Research Institute, Cairo 11727, Nasr City, Cairo (Egypt); Elshaarawy, Reda F.M. [Department of Chemistry, Faculty of Science, Suez University, Suez (Egypt); Institut fur Anorganische Chemie und Strukturchemie, Heinrich-Heine Universitat, Dusseldorf (Germany); Samy El-Shall, M. [Department of Chemistry, Virginia Commonwealth University Richmond, VA 23284-2006 (United States)

    2017-04-30

    Highlights: • Co{sub 3}O{sub 4} incorporated MCM-41 materials were successfully synthesized using MWI direct approach. • Co3{sup +} cation is considered as favorable site for CO adsorption resulted in promote the CO oxidation. • The loading of Pd species resulted in enhancement of activity for CO oxidation. - Abstract: Co{sub 3}O{sub 4} incorporated within mesoporous MCM-41 silica have been successfully synthesized and promoted with Pd nanoparticles through a microwave irradiation (MWI) approach. Powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), N{sub 2}-physisorped, X-ray photoelectron spectroscopy (XPS), temperature program reduction of hydrogen (H{sub 2}-TPR), temperature program desorption of oxygen (O{sub 2}-TPD) and high resolution transmission electron microscopy (HRTEM) were adapted to characterize these prepared catalysts. Carbon monoxide oxidation as a model reaction was then used to assess the catalytic performance of these materials. In the light of H{sub 2}-TPR and XPS results, revealed that the coexisting of Co{sup 3+} and Co{sup 2+} species as well as surface Co{sup 3+}/Co{sup 2+} ratio within the hexagonal mesoporous of MCM-41, could create an ideal environment to accomplish most extreme catalytic activity. On the other hand, the enhanced CO oxidation by Pd nanoparticles deposition has been explained in the light of the enhancement of the redox ability and tuning the electronic structure of Co{sub 3}O{sub 4}, which improved the O{sub 2} activation and reduced the adsorption ability of CO simultaneously, which significantly boosted the catalytic performance of CO oxidation. This work provides insights into factors that could lead to improved low temperature CO oxidation performance in Pd-based catalysts.

  4. Co-modified MCM-41 as an effective adsorbent for levofloxacin removal from aqueous solution: optimization of process parameters, isotherm, and thermodynamic studies.

    Science.gov (United States)

    Jin, Ting; Yuan, Wenhua; Xue, Yujie; Wei, Hong; Zhang, Chaoying; Li, Kebin

    2017-02-01

    Antibiotics are emerging contaminants due to their potential risks to human health and ecosystems. Poor biodegradability makes it necessary to develop effective physical-chemical methods to eliminate these contaminants from water. The cobalt-modified MCM-41 was prepared by a one-pot hydrothermal method and characterized by SAXRD, N 2 adsorption-desorption, SEM, UV-Vis DR, and FTIR spectroscopy. The results revealed that the prepared 3% Co-MCM-41 possessed mesoporous structure with BET surface areas at around 898.5 m 2 g -1 . The adsorption performance of 3% Co-MCM-41 toward levofloxacin (LVF) was investigated by batch experiments. The adsorption of LVF on 3% Co-MCM-41 was very fast and reached equilibrium within 2 h. The adsorption kinetics followed the pseudo-second-order kinetic model with the second-order rate constants in the range of 0.00198-0.00391 g mg -1  min -1 . The adsorption isotherms could be well represented by the Langmuir, Freundlich, and Dubinin-Radushkevich (D-R) isotherm equations. Nevertheless, D-R isotherm provided the best fit based on the coefficient of determination and average relative error values. The mean free energy of adsorption (E) calculated from D-R model was about 11 kJ mol -1 , indicating that the adsorption was mainly governed by a chemisorption process. Moreover, the adsorption capacity was investigated as a function of pH, adsorbent dosage, LVF concentration, and temperature with help of respond surface methodology (RSM). A quadratic model was established, and an optimal condition was obtained as follows: pH 8.5, adsorbent dosage of 1 g L -1 , initial LVF concentration of 119.8 mg L -1 , and temperature of 31.6 °C. Under the optimal condition, the adsorption capacity of 3% Co-MCM-41 to LVF could reach about 108.1 mg g -1 . The solution pH, adsorbent dosage, LVF concentration, and a combination of adsorbent dose and LVF concentration were significant factors affecting the adsorption process. The adsorption

  5. Effects of surface acidities of MCM-41 modified with MoO{sub 3} on adsorptive desulfurization of gasoline

    Energy Technology Data Exchange (ETDEWEB)

    Shao Xinchao, E-mail: sxc86@yahoo.cn [Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning ShiHua University, Fushun 113001 (China); Zhang Xiaotong; Yu Wenguang; Wu Yuye [Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning ShiHua University, Fushun 113001 (China); Qin Yucai [Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning ShiHua University, Fushun 113001 (China); College of Chemistry and Chemical Engineering, China University of Petroleum (East China), Qingdao, Shandong 257061 (China); Sun Zhaolin [Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning ShiHua University, Fushun 113001 (China); School of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China); Song Lijuan, E-mail: lsong56@263.net [Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning ShiHua University, Fushun 113001 (China) and College of Chemistry and Chemical Engineering, China University of Petroleum (East China), Qingdao, Shandong 257061 (China)

    2012-12-15

    Highlights: Black-Right-Pointing-Pointer The MoO{sub 3}-MCM-41 samples prepared by spontaneous monolayer dispersion and impregnation with a different MoO{sub 3} filling have been studied. Black-Right-Pointing-Pointer The relative concentration of hydroxyl groups present on before and after containing MoO{sub 3} samples was monitored by in situ FTIR to speculate the bonding style of MoO{sub 3} and MCM-41. Black-Right-Pointing-Pointer The surface acidities of the MoO{sub 3}-MCM-41 adsorbents were investigated systematically and correlated with the desulfurization performance. - Abstract: A series of MCM-41 samples containing molybdenum oxide as active species in the mesoporous channels loaded by spontaneous monolayer dispersion (SMD) and impregnation (IM) have been prepared and characterized using XRD, N{sub 2} adsorption-desorption analysis, Fourier transform infrared spectroscopy (FTIR) and intelligent gravimetric analyzer (IGA). The relative number of hydroxy on the adsorbents was investigated by in situ FTIR. Surface acidities of the adsorbents were studied by infrared spectroscopy of adsorbed pyridine and correlated with reactivity for adsorptive desulfurization. The IGA technique was employed to investigate adsorption behavior of thiophene and benzene on the adsorbents at 303 K. It is shown that MoO{sub 3} can be highly dispersed up to 0.2 g g{sup -1} in the MCM-41 channels by the SMD strategy with the ordered mesoporous structure of the MoMM samples remaining intact. The ordered mesostructure of MCM-41 is, however, destroyed at higher MoO{sub 3} contents of 0.26 and 0.32 g g{sup -1} with particle sizes of 1.2 nm and 3.6 nm, respectively, observed. For the MoMI(0.2) sample prepared by the IM method, the aggregation of the MoO{sub 3} particles takes place with a particle size of 6.5 nm obtained. The results are also revealed that the dispersion extent of the MoO{sub 3} species is related to the abundant surface hydroxy of MCM-41. The host species and guest

  6. Effects of surface acidities of MCM-41 modified with MoO3 on adsorptive desulfurization of gasoline

    International Nuclear Information System (INIS)

    Shao Xinchao; Zhang Xiaotong; Yu Wenguang; Wu Yuye; Qin Yucai; Sun Zhaolin; Song Lijuan

    2012-01-01

    Highlights: ► The MoO 3 -MCM-41 samples prepared by spontaneous monolayer dispersion and impregnation with a different MoO 3 filling have been studied. ► The relative concentration of hydroxyl groups present on before and after containing MoO 3 samples was monitored by in situ FTIR to speculate the bonding style of MoO 3 and MCM-41. ► The surface acidities of the MoO 3 -MCM-41 adsorbents were investigated systematically and correlated with the desulfurization performance. - Abstract: A series of MCM-41 samples containing molybdenum oxide as active species in the mesoporous channels loaded by spontaneous monolayer dispersion (SMD) and impregnation (IM) have been prepared and characterized using XRD, N 2 adsorption–desorption analysis, Fourier transform infrared spectroscopy (FTIR) and intelligent gravimetric analyzer (IGA). The relative number of hydroxy on the adsorbents was investigated by in situ FTIR. Surface acidities of the adsorbents were studied by infrared spectroscopy of adsorbed pyridine and correlated with reactivity for adsorptive desulfurization. The IGA technique was employed to investigate adsorption behavior of thiophene and benzene on the adsorbents at 303 K. It is shown that MoO 3 can be highly dispersed up to 0.2 g g −1 in the MCM-41 channels by the SMD strategy with the ordered mesoporous structure of the MoMM samples remaining intact. The ordered mesostructure of MCM-41 is, however, destroyed at higher MoO 3 contents of 0.26 and 0.32 g g −1 with particle sizes of 1.2 nm and 3.6 nm, respectively, observed. For the MoMI(0.2) sample prepared by the IM method, the aggregation of the MoO 3 particles takes place with a particle size of 6.5 nm obtained. The results are also revealed that the dispersion extent of the MoO 3 species is related to the abundant surface hydroxy of MCM-41. The host species and guest species undergo solid-state reaction to form Si-O-Mo bonds in the mixtures which enhance both the Lewis acid and Brönsted acid of

  7. Synthesis and physicochemical properties of Zr-MCM-41 mesoporous molecular sieves and Pt/H3PW12O40/Zr-MCM-41 catalysts

    International Nuclear Information System (INIS)

    Chen, L.F.; Wang, J.A.; Norena, L.E.; Aguilar, J.; Navarrete, J.; Salas, P.; Montoya, J.A.; Del Angel, P.

    2007-01-01

    For the first time, modifications of the surface and framework of Si-MCM-41 by depositing a heteropolyacid on the surface and by introducing foreign Zr 4+ ions into the framework are investigated. The Zr-modified Si-MCM-41 mesoporous materials (hereafter referred as WSZn, n=Si/Zr=25, 15, 8, 4) were synthesized through a surfactant-templated preparation approach, using low-cost fumed silica as the Si precursor. After impregnation with 25 wt% of H 3 PW 12 O 40 , the surface Broensted acidity of the Pt/H 3 PW 12 O 40 /WSZn catalysts was greatly enhanced by 2-10 times relative to the bare WSZn support. Two kinds of supported heteropolyacids were formed: (i) bulk-like heteropolyacid crystals with unchanged Keggin structures, and (ii) highly dispersed heteropolyacid with distorted Keggin units. The formation of various kinds of heteropolyacid structures is closely related to the interaction between the heteropolyanions and the hydroxyl groups in the host support. - Graphical abstract: Modifications of the surface and framework of Si-MCM-41 by depositing a heteropolyacid on the surface and by introducing foreign Zr 4+ ions into the framework are investigated. Broensted acidity of the Pt/H 3 PW 12 O 40 /Zr-MCM-41 catalysts was greatly enhanced by 2-10 times relative to the bare Zr-MCM-41 support

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

    Science.gov (United States)

    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.

  9. 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.

  10. Solid-state (49/47)Ti NMR of titanium-based MCM-41 hybrid materials.

    Science.gov (United States)

    Ballesteros, Ruth; Fajardo, Mariano; Sierra, Isabel; Force, Carmen; del Hierro, Isabel

    2009-11-03

    Titanium solid-state NMR spectroscopy data for a series of organic-inorganic titanium MCM-41 based materials have been collected. These materials have been synthesized by first modifying the mesoporous silica MCM-41 in one step with a mixture of silanes: a triazine propyl triethoxysilane acting as functional linker and methyltrimethoxysilane or hexamethyldisilizane as capped agents to mask the remaining silanol groups. Second, the appropiate titanium precursor Ti(OPr(i))(4), [{Ti(OPr(i))(3)(OMent)}(2)] (OMent = 1R,2S,5R-(-)-menthoxo), Ti(OPr(i))(4), or [Ti(eta(5)-C(5)HMe(4))Cl(3)], has been immobilized by reaction with the modified MCM-41. Finally, after Ti(OPr(i))(4) immobilization onto the organomodified support the reaction with the chiral (+)-diethyl-l-tartrate was accomplished. The materials without functional linker have been also prepared by reaction in one step of the capped agent and the titanium precursor with the mesoporous silica. Relevant correlations of titanium NMR resonance chemical shifts and line widths can be inferred depending on different factors. The immobilization procedure used to prepare titanium-based MCM-41 hybrid materials and the choice of the silylating reagents employed to mask the silanol groups present on the silica surfaces produce significant differences in the Ti NMR spectra. Furthermore, depending on the electronic and sterical influence of the substituents directly attached to the titanium center, chemical shifts and line widths are modified providing novel information about titanium structure.

  11. MCM-41 mesoporous silica nanoparticles functionalized with aptamer and radiolabelled with 90Y and 159Gd as a potential therapeutic agent against colorectal cancer

    International Nuclear Information System (INIS)

    Ferreira, Carolina de Aguiar

    2014-01-01

    Colorectal cancer (CRC) is a malignancy that affects large intestine and rectum, and it is the most common malignancy of the gastrointestinal tract, the third most commonly diagnosed type of cancer in the world and the second leading cause of cancer-related death in the United States. Nowadays, available therapeutic procedures for this type of cancer are limited and ineffective. Conventional radiotherapy is not an often used approach in the treatment of CRC due to the fact that peristaltic movements hamper the targeting of ionizing radiation and this type of treatment is used as adjuvant and palliative to control symptoms. Therefore, surgical intervention is the primary therapeutic choice against this disease. Researches based on the combination of radioisotopes and nanostructured carriers systems have demonstrated significant results in improving the selectivity action as well as reducing the radiation dose into healthy tissues. MCM-41 mesoporous silica nanoparticles have unique characteristics such as high surface area and well-defined pore diameters making these nanoparticles an ideal candidate of therapeutic agent carrier. Thus, the objective of this work is to synthesize and characterize MCM-41 mesoporous silica nanoparticles conjugated with yttrium-90 and gadolinium-159 and evaluate this system as a potential therapeutic agent. The nanoparticles were synthesized via sol-gel method. The sample was characterized using FTIR, SAXS, PCS, Zeta Potential analysis, Thermal analysis, CHN elemental analysis, nitrogen adsorption, scanning and transmission electron microscopy. The ability to incorporate Y +3 and Gd +3 ion was determined in vitro using different ratios (1:1, 1:3, 1:5 v/v) of YCL 3 and Gd 2 O 3 and silica nanoparticles dispersed in saline, pH 7.4. The non-incorporated Y +3 and Gd +3 ions were removed by ultracentrifugation procedure and the concentration of ions in the supernatant was determined by ICP-AES. Cell viability was assessed by colorimetric MTT

  12. Mesoporous silica based MCM-41 as solid-phase extraction sorbent combined with micro-liquid chromatography-quadrupole-mass spectrometry for the analysis of pharmaceuticals in waters.

    Science.gov (United States)

    Dahane, S; Martínez Galera, M; Marchionni, M E; Socías Viciana, M M; Derdour, A; Gil García, M D

    2016-05-15

    This paper reports the first application of the silica based mesoporous material MCM-41 as a sorbent in solid phase extraction, to pre-concentrate pharmaceuticals of very different polarity (atenolol, nadolol, pindolol, timolol, bisoprolol, metoprolol, betaxolol, ketoprofen, naproxen, ibuprofen, diclofenac, tolfenamic acid, flufenamic acid and meclofenamic acid) in surface waters. The analytes were extracted from 100mL water samples at pH 2.0 (containing 10(-3) mol/L of sodium chloride) by passing the solution through a cartridge filled with 100 mg of MCM-41. Following elution, the pharmaceuticals were determined by micro-liquid chromatography and triple quadrupole-mass spectrometry. Two selected reaction monitoring transitions were monitored per compound, the most intense one being used for quantification and the second one for confirmation. Matrix effect was found in real waters for most analytes and was overcome using the standard addition method, which compared favorably with the matrix matched calibration method. The detection limits in solvent (acetonitrile:water 10:90, v/v) ranged from 0.01 to 1.48 μg/L and in real water extracts from 0.10 to 3.85 μg/L (0.001-0.0385 μg/L in the water samples). The quantitation limits in solvent were in the range 0.02-4.93 μg/L, whereas in real water extracts were between 0.45 and 10.00 μg/L (0.0045 and 0.1000 μg/L in the water samples). When ultrapure water samples were spiked at two concentration levels of each pharmaceutical (0.1 and 0.2 μg/L) and quantified using solvent based calibration graphs, recoveries were near 100%. However, recoveries for most pharmaceuticals were comparable or better than de described above, when river water samples (spiked at the same concentration levels) were quantified by the standard addition method and slightly worse using the matrix matched calibration method. Five real samples (two rivers, one dam and two fountain water samples) were analyzed by the developed method, atenolol

  13. Free-radical sensing by using naphthalimide based mesoporous silica (MCM-41) nanoparticles: A combined fluorescence and cellular imaging study

    Science.gov (United States)

    Jha, Gaurav; Roy, Subhasis; Sahu, Prabhat Kumar; Banerjee, Somnath; Anoop, N.; Rahaman, Abdur; Sarkar, Moloy

    2018-01-01

    Keeping in mind the advantages of material-based systems over simple molecule-based systems, we have designed and developed three inorganic-organic hybrid systems by anchoring 1,8-naphthalimide derivatives to mesoporous silica nanoparticles for detection of free radicals. Prior to photophysical study, systems are characterized by spectroscopic, microscopic and thermo-gravimetric techniques. Steady state and time-resolved fluorescence studies demonstrate that the hydrazine based system is senstive towards detection of various free radicals. Cellular imaging study reveals cell permeability and toxicity study demonstrates the non-toxic nature of the material. These studies have suggested that present system has the potential to be used in various biological applications.

  14. MCM-41 mesoporous silica nanoparticles functionalized with aptamer and radiolabelled with {sup 90}Y and {sup 159}Gd as a potential therapeutic agent against colorectal cancer; Nanoparticulas de silica mesoporosa MCM-41 funcionalizadas com aptamero e radiomarcadas com {sup 90}Y e {sup 159}Gd como um potencial agente terapeutico contra cancer colorretal

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Carolina de Aguiar

    2014-06-01

    Colorectal cancer (CRC) is a malignancy that affects large intestine and rectum, and it is the most common malignancy of the gastrointestinal tract, the third most commonly diagnosed type of cancer in the world and the second leading cause of cancer-related death in the United States. Nowadays, available therapeutic procedures for this type of cancer are limited and ineffective. Conventional radiotherapy is not an often used approach in the treatment of CRC due to the fact that peristaltic movements hamper the targeting of ionizing radiation and this type of treatment is used as adjuvant and palliative to control symptoms. Therefore, surgical intervention is the primary therapeutic choice against this disease. Researches based on the combination of radioisotopes and nanostructured carriers systems have demonstrated significant results in improving the selectivity action as well as reducing the radiation dose into healthy tissues. MCM-41 mesoporous silica nanoparticles have unique characteristics such as high surface area and well-defined pore diameters making these nanoparticles an ideal candidate of therapeutic agent carrier. Thus, the objective of this work is to synthesize and characterize MCM-41 mesoporous silica nanoparticles conjugated with yttrium-90 and gadolinium-159 and evaluate this system as a potential therapeutic agent. The nanoparticles were synthesized via sol-gel method. The sample was characterized using FTIR, SAXS, PCS, Zeta Potential analysis, Thermal analysis, CHN elemental analysis, nitrogen adsorption, scanning and transmission electron microscopy. The ability to incorporate Y{sup +3} and Gd{sup +3} ion was determined in vitro using different ratios (1:1, 1:3, 1:5 v/v) of YCL{sub 3} and Gd{sub 2}O{sub 3} and silica nanoparticles dispersed in saline, pH 7.4. The non-incorporated Y{sup +3} and Gd{sup +3} ions were removed by ultracentrifugation procedure and the concentration of ions in the supernatant was determined by ICP-AES. Cell viability

  15. Multifunctional materials such as MCM-41÷Fe3O4÷folic acid as drug delivery system.

    Science.gov (United States)

    Popescu, Simona; Ardelean, Ioana Lavinia; Gudovan, Dragoş; Rădulescu, Marius; Ficai, Denisa; Ficai, Anton; Vasile, Bogdan Ştefan; Andronescu, Ecaterina

    2016-01-01

    In this study, MCM-41 mesoporous silica nanoparticles (NPs) and MCM-41÷Fe3O4 mesoporous silica NPs were prepared by sol-gel method using CTAB (cetyltrimethylammonium bromide) as template and TEOS (tetraethyl orthosilicate) as silica precursor in order to use these materials as drug delivery system (DDS) for different biologically active agents. The MCM-41 and MCM-41÷Fe3O4 mesoporous silica NPs were characterized using specific physico-chemical methods [transmission electron microscopy (TEM), scanning electron microscopy (SEM), nitrogen adsorption and desorption studies - BET (Brunauer-Emmett-Teller) method, X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy], while the release studies were done by a high-performance liquid chromatography (HPLC)-modified method. The pH dependence of the delivery of folic acid from the mesoporous structures was analyzed and found that the release is pH sensitive. The lower delivery at strongly acid pH comparing with neutral/slightly alkaline pH could be beneficial because in stomach the folic acid can be destroyed.

  16. Synthesis and characterization of mesoporous Mn-MCM-41 materials

    International Nuclear Information System (INIS)

    Saladino, Maria Luisa; Kraleva, Elka; Todorova, Silvia; Spinella, Alberto; Nasillo, Giorgio; Caponetti, Eugenio

    2011-01-01

    Highlights: · Manganese MCM-41 as catalyst. · Influence of pH on the structure of MCM-41. · Influence of manganese on the structure and activity of Mn-MCM-41. - Abstract: MCM-41 has been synthesized at two different pH using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 deg. C for 4 h. Mn-MCM-41 powders with different Mn/Si molar ratios were prepared using the incipient wetness method, followed by calcination at 550 deg. C for 5 h. At the end of the impregnation process the powders colour changed from white to brown whose intensity depends on manganese quantity. The materials characterization was performed by X-ray diffraction, N 2 adsorption, 29 Si Cross Polarization-Magic Angle Spinning NMR, and X-ray Photoelectron Spectroscopy. The effects of the manganese quantity and of the structural characteristic of the MCM-41 support were studied. The catalytic activity of the prepared systems was evaluated in a complete n-hexane oxidation.

  17. Fabrication of MCM-41 fibers with well-ordered hexagonal mesostructure controlled in acidic and alkaline media

    International Nuclear Information System (INIS)

    Jafarzadeh, A.; Sohrabnezhad, Sh.; Zanjanchi, M.A.; Arvand, M.

    2016-01-01

    In this paper, synthesis and characterization of two type morphologies of the MCM-41mesoporous material, nano and microfibers, were investigated by electrospinning technique. The synthesis was performed in acidic and alkaline media, separately. The MCM-41 morphologies were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethylorthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) were used as silica and template sources for the synthesis of MCM-41 morphologies, respectively. The SEM results showed that MCM-41 nanofibers were spun in acidic media and microfibers of MCM-41 were produced in alkaline media. The XRD study revealed a long range structural ordering of mesoporous materials. The TEM results indicated rough surfaces with uniform average diameter 200 nm for nanofibers and 2 µm for microfibers. The pore diameter and surface area of calcined MCM-41 nanofibers were 2.2 nm and 970 m 2 /g, respectively. For the MCM-41 microfibers, pore sizes of 2.7 nm and surface areas 420 m 2 /g was measured. - Graphical abstract: Electrospinning method was used for fabricating of MCM-41 microfibers from TEOS in alkaline media (top) and MCM-41 nanofibers in acidic media (bottom). - Highlights: • Synthesis of MCM-41 nanofibers and microfibers by electrospinning technique. • MCM-41 nanofibers were synthesized in acidic media. • MCM-41 manofibers spun in alkaline media. • Electrospinning was a simple method for preparing of fibers with respect to chemical method.

  18. Study on thermal, mechanical and adsorption properties of amine-functionalized MCM-41/PMMA and MCM-41/PS nanocomposites prepared by ultrasonic irradiation.

    Science.gov (United States)

    Mohammadnezhad, Gholamhossein; Abad, Saeed; Soltani, Roozbeh; Dinari, Mohammad

    2017-11-01

    In this study, two common industrial polymers, poly(methyl methacrylate) (PMMA) and polystyrene (PS), were incorporated into amine-functionalized MCM-41 mesoporous silica as reinforcement agents via an ultrasonic assisted method as a facile, fast, eco-friendly, and versatile synthetic tool. Amino functionalization of MCM-41 were performed by 3-aminopropyl triethoxysilane as a coupling agent and it is denoted as APTS-MCM-41. The obtained nanocomposites (NCs), APTS-MCM-41/PMMA and APTS-MCM-41/PS, were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning and transmission electron microscopies (SEM and TEM), and thermogravimetric analysis (TGA). Their mechanical properties were also probed via stress-strain curves and improved tensile properties were observed in the NCs relative to the neat polymers. Additionally, APTS-MCM-41/PMMA exhibited better mechanical properties than APTS-MCM-41/PS. Sorption studies were carried out on the two NCs and the effect of different process parameters, namely, pH, contact time, and initial Cd(II) concentration investigated in batch mode. Pseudo-second order and intraparticle diffusion models explain the Cd(II) kinetics more effectively for APTS-MCM-41/PMMA and APTS-MCM-41/PS, respectively. The adsorption isotherm data fitted well to Langmuir isotherm for both NCs and the maximum monolayer adsorption capacities were found to be 24.75mg/g and 10.42mg/g for APTS-MCM-41/PMMA and APTS-MCM-41/PS, respectively. The results demonstrate that the NCs show potential for use in adsorption of heavy metal ion such as Cd(II) from aqueous media. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Synthesis, Characterizations, and Applications of Metal-Ions Incorporated High Quality MCM-41 Catalysts

    International Nuclear Information System (INIS)

    Lim, Steven S.; Haller, Gary L.

    2013-01-01

    Various metal ions (transition and base metals) incorporated MCM-41 catalysts can be synthesized using colloidal and soluble silica with non-sodium involved process. Transition metal ion-typically V 5+ , Co 2+ , and Ni 2+ -incorporated MCM-41 catalysts were synthesized by isomorphous substitution of Si ions in the framework. Each incorporated metal ion created a single species in the silica framework, single-site solid catalyst, showing a substantial stability in reduction and catalytic activity. Radius of pore curvature effect was investigated with Co-MCM-41 by temperature programmed reduction (TPR). The size of metallic Co clusters, sub-nanometer, could be controlled by a proper reduction treatment of Co-MCM-41 having different pore size and the initial pH adjustment of the Co-MCM-41 synthesis solution. These small metallic clusters showed a high stability under a harsh reaction condition without serious migration, resulting from a direct anchoring of small metallic clusters to the partially or unreduced metal ions on the surface. After a complete reduction, partial occlusion of the metallic cluster surface by amorphous silica stabilized the particles against aggregations. As a probe reaction of particle size sensitivity, carbon single wall nanotubes (SWNT) were synthesized using Co-MCM-41. A metallic cluster stability test was performed by CO methanation using Co- and Ni-MCM-41. Methanol and methane partial oxidations were carried out with V-MCM-41, and the radius of pore curvature effect on the catalytic activity was investigated

  20. Synthesis of MCM-41 nanomaterial from Algerian bentonite ...

    African Journals Online (AJOL)

    Mesoporous materials of the MCM-41 type were synthesized from Algerian bentonite as an aluminosilicate source without the addition of pure silica and aluminum reagents. The samples were synthesized under hydrothermal condition using cetyltrimithylammonium bromide (CTAB) as surfactant. The influence of initial ...

  1. Recycling of surfactant template in mesoporous MCM-41 synthesis

    Science.gov (United States)

    Lai, J. Y.; Twaiq, F.; Ngu, L. H.

    2017-06-01

    The recycling of surfactant template is investigated through the reuse of the surfactant template in the mesoporous MCM-41 synthesis process. In the synthesis of MCM-41, tetraethylorthosilicate (TEOS) solution in water was utilized as the silica source while hexadecyltrimethylammonium bromide (CTAB) solution in ethyl alcohol was used as a surfactant template. The synthesized gel is formed thoroughly by mixing the two solutions under acid conditions with a pH value of 0.5 for 1 hour and kept for crystallization for 48 hours. The as-synthesized MCM-41 powder is recovered by filtration while the filtrate (mother liquor) was then reused for the second synthesis cycle. The synthesis procedure was repeated till no further solid product was formed. The synthesized gel was not produced in the unifying solution in the fifth cycle of MCM-41 synthesis. The quality of the calcined MCM-41 powder produced in each synthesis cycle was evaluated by calculating the amount of MCM-41 produced and the surface area of the powder product. The result showed that 1.28, 0.37, 1.64, 1.90 and 0.037 g were obtained in the 1st, 2nd, 3rd, 4th and 5th synthesis cycle, respectively. The surface area of the powder produced was found to be 1170, 916, 728, and 508 m2/g for 1st, 2nd, 3rd and 4th respectively. The concentration of the surfactant template has reached value lower than the critical micelle concentration (CMC) and remained constant after the 4th cycle. There was no further formation of gel due to low availability in the interaction between silicate anions and surfactant cations when the amount of TEOS was fixed for every synthesis cycle.

  2. Paraquat adsorption on NaX and Al-MCM-41.

    Science.gov (United States)

    Rongchapo, Wina; Deekamwong, Krittanun; Loiha, Sirinuch; Prayoonpokarach, Sanchai; Wittayakun, Jatuporn

    2015-01-01

    The aim of this work is to determine paraquat adsorption capacity of zeolite NaX and Al-MCM-41. All adsorbents were synthesized by hydrothermal method using rice husk silica. For Al-MCM-41, aluminum (Al) was added to the synthesis gel of MCM-41 with Al content of 10, 15, 20 and 25 wt%. The faujasite framework type of NaX and mesoporous characteristic of Al-MCM-41 were confirmed by X-ray diffraction. Surface area of all adsorbents determined by N2 adsorption-desorption analysis was higher than 650 m2/g. Al content and geometry were determined by X-ray fluorescence and 27Al nuclear magnetic resonance, respectively. Morphology of Al-MCM-41 were studied by transmission electron microscopy; macropores and defects were observed. The paraquat adsorption experiments were conducted using a concentration range of 80-720 mg/L for NaX and 80-560 mg/L for Al-MCM-41. The paraquat adsorption isotherms from all adsorbents fit well with the Langmuir model. The adsorption capacity of NaX was 120 mg/g-adsorbent. Regarding Al-MCM-41, the 10% Al-MCM-41 exhibited the lowest capacity of 52 mg/g-adsorbent while the other samples had adsorption capacity of 66 mg/g-adsorbent.

  3. Grafting of a novel gold(III) complex on nanoporous MCM-41 and evaluation of its toxicity in Saccharomyces cerevisiae.

    Science.gov (United States)

    Fazaeli, Yousef; Amini, Mostafa M; Ashourion, Hamed; Heydari, Homayoun; Majdabadi, Abbas; Jalilian, Amir Reza; Abolmaali, Shamsozoha

    2011-01-01

    The goal of this research was to investigate the potential of newly synthesized gold complex trichloro(2,4,6-trimethylpyridine)Au(III) as an anticancer agent. The gold(III) complex was synthesized and grafted on nanoporous silica, MCM-41, to produce AuCl(3)@PF-MCM- 41 (AuCl(3) grafted on pyridine-functionalized MCM-41). The toxicity of trichloro(2,4,6- trimethylpyridine)Au(III) and AuCl(3)@PF-MCM-41 in Saccharomyces cerevisiae (as a model system) was studied. The gold(III) complex showed a mid cytotoxic effect on yeast viability. Using the drug delivery system, nanoporous MCM-41, the gold(III) complex became a strong inhibitor for growth of yeast cells at a very low concentration. Furthermore, the animal tests revealed a high uptake of AuCl(3)@PF-MCM-41 in tumor cells. The stability of the compound was confirmed in human serum.

  4. MCM-41 impregnated with A zeolite precursor: Synthesis, characterization and tetracycline antibiotics removal from aqueous solution.

    Science.gov (United States)

    Liu, Minmin; Hou, Li-An; Yu, Shuili; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

    2013-05-01

    In this paper, the MCM-41 has been modified by impregnation with zeolite A to prepare a kind of new adsorbent. The adsorption of TC from aqueous solutions onto modified MCM-41 has been studied. It was discovered that the adsorption capability of zeolite A modified MCM-41 (A-MCM-41) increased dramatically after modification. The modified MCM-41 was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier Transform Infrared (FTIR) analysis, Transmission electron microscopy (TEM) images, and 29 Si and 27 Al Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR) spectra. The modified MCM-41 structure was still retained after impregnated with zeolite A but the surface area and pore diameter decreased due to pore blockage. The adsorption of TC on modified MCM-41 was discussed regarding various parameters such as pH, initial TC concentration, and the reaction time. The pH effects on TC adsorption indicated that the adsorbents had better adsorption performances in acidic and neutral conditions. The adsorption isotherms were fitted well by the Langmuir model. The adsorption kinetics was well described by both pseudo-second order equation and the intra-particle diffusion model. The adsorption behavior in a fixed-bed column system followed Thomas model. The adsorption behavior of TC was the chemical adsorption with an ion exchange process and electrostatic adsorption.

  5. Preparation, characterization and optical properties of Lanthanum-(nanometer MCM-41) composite materials

    International Nuclear Information System (INIS)

    Zhai, Q. Z.; Wang, P.

    2008-01-01

    Nanometer MCM-41 molecular sieve was prepared under a base condition by using cetyltrimethylammonium bromide as template and tetraethyl orthosilicate as silica source by means of hydrothermal method. Lanthanum(III) was incorporated into the nanometer MCM-41 by a liquid phase grafting method. The prepared nano composite materials were characterized by means of powder X-ray diffraction, spectrophotometric analysis, Fourier transform infrared spectroscopy, low temperature nitrogen adsorption-desorption technique, solid diffuse reflectance absorption spectra and luminescence. The powder X-ray diffraction studies show that the nanometer MCM-41 molecular sieve is successfully prepared. The highly ordered meso porous two-dimensional hexagonal channel structure and framework of the support MCM-41 is retained intact in the prepared composite material La-(nanometer MCM-41). The spectrophotometric analysis indicates that lanthanum exists in the prepared nano composite materials. The Fourier transform infrared spectra indicate that the framework of the MCM-41 molecular sieve still remains in the prepared nano composite materials and some framework vibration peaks show blue shifts relative to those of the MCM-41 molecular sieve. The low temperature nitrogen adsorption-desorption indicates that the guest locales in the channel of the molecular sieve. Compared with bulk lanthanum oxide, the guest in the channel of the molecular sieve has smaller particle size and shows a significant blue shift of optical absorption band in solid diffuse reflectance absorption spectra. The observed blue shift in the solid state diffuse reflectance absorption spectra of the lanthanum-(nanometer MCM-41) sample show the obvious stereoscopic confinement effect of the channel of the host on the guest, which further indicates the successful encapsulation of the guest in the host. The La-(nanometer MCM-41) sample shows luminescence

  6. Ultrasonic-assisted synthesis and magnetic studies of iron oxide/MCM-41 nanocomposite

    International Nuclear Information System (INIS)

    Ursachi, Irina; Vasile, Aurelia; Ianculescu, Adelina; Vasile, Eugeniu; Stancu, Alexandru

    2011-01-01

    Highlights: → A quick and facile route for the synthesis of iron oxide/MCM-41 nanocomposite. → Magnetic nanoparticles were stabilized inside the pores of mesoporous silica MCM-41. → The pore size of MCM-41 dictates the properties of iron oxide nanoparticles. → The procedure provides a narrow size distribution of magnetic nanoparticles. - Abstract: Iron oxide nanoparticles were stabilized within the pores of mesoporous silica MCM-41 amino-functionalized by a sonochemical method. Formation of iron oxide nanoparticles inside the mesoporous channels of amino-functionalized MCM-41 was realized by wet impregnation using iron nitrate, followed by calcinations at 550 deg. C in air. The effect of functionalization level on structural and magnetic properties of obtained nanocomposites was studied. The resulting materials were characterized by powder X-ray diffraction (XRD), high-resolution transmission electron microscopy and selected area electron diffraction (HRTEM and SAED), vibrating sample and superconducting quantum interface magnetometers (VSM and SQUID) and nitrogen adsorption-desorption isotherms measurements. The HRTEM images reveal that the most of the iron oxide nanoparticles were dispersed inside the mesopores of silica matrix and the pore diameter of the amino-functionalized MCM-41 matrix dictates the particle size of iron oxide nanoparticles. The obtained material possesses mesoporous structure and interesting magnetic properties. Saturation magnetization value of magnetic iron oxide nanopatricles stabilized in MCM-41 amino-functionalized by in situ sonochemical synthesis was 1.84 emu g -1 . An important finding is that obtained magnetic nanocomposite materials exhibit enhanced magnetic properties than those of iron oxide/MCM-41 nanocomposite obtained by conventional method. The described method is providing a rather short preparation time and a narrow size distribution of iron oxide nanoparticles.

  7. 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.

  8. Photocatalytic Properties of Nb/MCM-41 Molecular Sieves: Effect of the Synthesis Conditions

    Directory of Open Access Journals (Sweden)

    Caterine Daza Gomez

    2015-08-01

    Full Text Available The effect of synthesis conditions and niobium incorporation levels on the photocatalytic properties of Nb/MCM-41 molecular sieves was assessed. Niobium pentoxide supported on MCM-41 mesoporous silica was obtained using two methods: sol-gel and incipient impregnation, in each case also varying the percentage of niobium incorporation. The synthesized Nb-MCM-41 ceramic powders were characterized using the spectroscopic techniques of infrared spectroscopy (IR, Raman spectroscopy, X-ray diffraction (XRD, and transmission electron microscopy (TEM. The photodegradation capacity of the powders was studied using the organic molecule, methylene blue. The effect of both the method of synthesis and the percentage of niobium present in the sample on the photodegradation action of the solids was determined. The mesoporous Nb-MCM-41 that produced the greatest photodegradation response was obtained using the sol-gel method and 20% niobium incorporation.

  9. Surface Properties of Al-Functionalized Mesoporous MCM-41 and the Melting Behavior of Water in Al-MCM-41 Nanopores.

    Science.gov (United States)

    Sterczyńska, Angelina; Deryło-Marczewska, Anna; Zienkiewicz-Strzałka, Małgorzata; Śliwińska-Bartkowiak, Małgorzata; Domin, Kamila

    2017-10-24

    We report an experimental investigation of structural and adhesive properties for Al-containing mesoporous MCM-41 and MCM-41 surfaces. In this work, highly ordered hexagonal mesoporous structures of aluminosilica with two different Si/Al molar ratios equal to 50 and 80 and silica samples were studied; Al was incorporated into the MCM-41 structures using the direct synthesis method, with CTAB as a surfactant. The incorporation of aluminum was evidenced simultaneously without any change in the hexagonal arrangement of cylindrical mesopores. The porous materials were examined by techniques such as low-temperature nitrogen sorption, energy-dispersive spectroscopy, and scanning and transmission electron microscopy. Surface properties were determined through X-ray photoelectron spectroscopy, potentiometric titration, and static contact angle measurements. It was shown that an increase in surface acidity leads to an increase in the wetting energy of the surface. To investigate the influence of acidity on the confinement effects, the melting behavior of water in Al-MCM-41 and MCM-41 with the same pore size was determined by using dielectric relaxation spectroscopy and differential scanning calorimetry methods. We found that the melting-point depression of water in pores is larger in the functionalized pores than in pure silica pores of the same pore diameter.

  10. A secondary, coplanar design Ni/MCM-41/Zn microbattery

    Science.gov (United States)

    Meskon, S. R.; Othman, R.; Ani, M. H.

    2018-01-01

    A secondary Ni/Zn microbattery (∼200 µm thick) has been developed in a coplanar electrode configuration. The cell is essentially of a circular shape (∼30 mm in diameter) consisting of a fine circular ring (cathode) and a circle (anode) split apart (~800 µm). Unlike the stacking cell architecture, coplanar configuration offers simple design, ease of fabrication and eventually cost saving. The use of MCM-41 mesoporous silica as the membrane separator cum electrolyte reservoir enables the successful implementation of coplanar configuration. The fabrication of Ni/Zn microbattery first begins with electrodeposition of zinc (Zn) and nickel hydroxide (Ni(OH)2) thin films onto patterned FR4 printed circuit board, followed by deposition of zinc oxide (ZnO) slurry onto the zinc active layer, and finally ends by multiple drop-coating procedures of MCM-41 from its precursor solution at ambient temperature. Once a potassium hydroxide (6 M KOH)/MCM-41 electrolyte-separator mixture is incorporated, the cell is sealed with an acrylic sheet and epoxy adhesive. The fabricated microbatteries were capable to sustain around 130 deep charge-discharge cycles. When rated at 0.1 mA, the energy density of the microbattery was around 3.82 Wh l-1 which is suitable for low rate applications and storage for micro energy harvesters such as piezoelectric generators.

  11. Metal Nanoparticles Supported on Al-MCM-41 via In Situ Aqueous Synthesis

    International Nuclear Information System (INIS)

    Alonso-Lemus, I.; Aguilar-Elguezabal, A.; Alvarez-Contreras, L.; Verde-Gomez, Y.

    2010-01-01

    MCM-41 have been used to custom synthesize catalysts in because of the controllable properties, such as pore size, active phase incorporation, crystal size, and morphology, among others. In this paper, a simple and versatile method for the incorporation of platinum, ruthenium, and palladium onto Al-MCM-41 mesoporous silica by direct inclusion of various precursors was studied. M/Al-MCM-41 structure, textural properties, morphology, and elemental composition were analyzed. The results obtained indicate that the Al-MCM-41 mesoporous-ordered structure was not affected by metallic particle incorporation. High-surface areas were obtained (1131 m2/g). Metallic nanoparticles dispersion on Al-MCM-41 was homogeneous for all samples and its particles sizes were between 6?nm to 20 nm. Microscopy results show round shape particles in platinum and palladium samples; however, ruthenium catalysts exhibit a spherical and rod shapes. Electrochemical testing for Pt/Al-MCM-41 showed electrocatalytic activity for H2 oxidation which indicates that these materials can be used as a catalyst in electrochemical devices.

  12. Functionalized bimodal mesoporous silicas as carriers for controlled aspirin delivery

    International Nuclear Information System (INIS)

    Gao Lin; Sun Jihong; Li Yuzhen

    2011-01-01

    The bimodal mesoporous silica modified with 3-aminopropyltriethoxysilane was performed as the aspirin carrier. The samples' structure, drug loading and release profiles were characterized with X-ray diffraction, scanning electron microscopy, N 2 adsorption and desorption, Fourier transform infrared spectroscopy, TG analysis, elemental analysis and UV-spectrophotometer. For further exploring the effects of the bimodal mesopores on the drug delivery behavior, the unimodal mesoporous material MCM-41 was also modified as the aspirin carrier. Meantime, Korsmeyer-Peppas equation f t =kt n was employed to analyze the dissolution data in details. It is indicated that the bimodal mesopores are beneficial for unrestricted drug molecules diffusing and therefore lead to a higher loading and faster releasing than that of MCM-41. The results show that the aspirin delivery properties are influenced considerably by the mesoporous matrix, whereas the large pore of bimodal mesoporous silica is the key point for the improved controlled-release properties. - Graphical abstract: Loading (A) and release profiles (B) of aspirin in N-BMMs and N-MCM-41 indicated that BMMs have more drug loading capacity and faster release rate than that MCM-41. Highlights: → Bimodal mesoporous silicas (BMMs) and MCM-41 modified with amino group via post-treatment procedure. → Loading and release profiles of aspirin in modified BMMs and MCM-41. → Modified BMMs have more drug loading capacity and faster release rate than that modified MCM-41.

  13. SYNTHESIS OF MCM-41 NANOMATERIAL FROM ALGERIAN ...

    African Journals Online (AJOL)

    T. Ali-Dahmane

    1 mai 2017 ... Journal of Fundamental and Applied Sciences is licensed under a Creative Commons Attribution-NonCommercial 4.0. International License. Libraries Resource Directory. We are listed under Research Associations category. SYNTHESIS OF MCM-41 NANOMATERIAL FROM ALGERIAN BENTONITE:.

  14. Synthesis and characterization of mesoporous Si-MCM-41 materials ...

    Indian Academy of Sciences (India)

    Administrator

    The poten- tial use of Al-MCM-41 and 12TPA-MCM-41 as solid acid catalysts has been explored and compared by study- ... such as difficulty in handling, causing an acidic waste water ... been supported onto MCM-41 by process of anchoring.

  15. Bimetallic iron and cobalt incorporated MFI/MCM-41 composite and its catalytic properties

    International Nuclear Information System (INIS)

    Li, Baoshan; Xu, Junqing; Li, Xiao; Liu, Jianjun; Zuo, Shengli; Pan, Zhiyun; Wu, Ziyu

    2012-01-01

    Graphical abstract: The formation of FeCo-MFI/MCM-41 composite is based on two steps, the first step of synthesizing the MFI-type proto-zeolite unites under hydrothermal conditions. The second step of assembling these zeolite fragment together new silica and heteroatom source on the CTAB surfactant micelle to synthesize the mesoporous product with hexagonal structure. Highlights: ► Bimetallic iron and cobalt incorporated MFI/MCM-41 composite was prepared using templating method. ► FeCo-MFI/MCM-41 composite simultaneously possessed two kinds of meso- and micro-porous structures. ► Iron and cobalt ions incorporated into the silica framework with tetrahedral coordination. -- Abstract: The MFI/MCM-41 composite material with bimetallic Fe and Co incorporation was prepared using templating method via a two-step hydrothermal crystallization procedure. The obtained products were characterized by a series of techniques including powder X-ray diffraction, N 2 sorption, transmission electron microscopy, scanning electron microscope, H 2 temperature programmed reduction, thermal analyses, and X-ray absorption fine structure spectroscopy of the Fe and Co K-edge. The catalytic properties of the products were investigated by residual oil hydrocracking reactions. Characterization results showed that the FeCo-MFI/MCM-41 composite simultaneously possessed two kinds of stable meso- and micro-porous structures. Iron and cobalt ions were incorporated into the silicon framework, which was confirmed by H 2 temperature programmed reduction and X-ray absorption fine structure spectroscopy. This composite presented excellent activities in hydrocracking of residual oil, which was superior to the pure materials of silicate-1/MCM-41.

  16. Fe_3O_4@B-MCM-41: A new magnetically recoverable nanostructured catalyst for the synthesis of polyhydroquinolines

    International Nuclear Information System (INIS)

    Abdollahi-Alibeik, Mohammad; Rezaeipoor-Anari, Ali

    2016-01-01

    Boron modified MCM-41 with magnetite core (Fe_3O_4@B-MCM-41) as a new magnetically recoverable heterogeneous catalyst was prepared and characterized by SEM, TEM, BET, XRD, VSM and FT-IR techniques. The catalytic activity of Fe_3O_4@B-MCM-41 was investigated in the four-component reaction of aldehyde, dimedone, active methylene compounds and ammonium acetate for the synthesis of polyhydroquinolines. According to optimization and characterization results the catalyst with Si:B:Fe_3O_4 mole composition of 40:4:1 has the best activity. The catalyst could be recovered easily by external magnet and has excellent reusability many times without significant decrease of activity. - Highlights: • Core–shell Fe_3O_4@MCM-41 nanoparticles modified by boron (Fe_3O_4@B-MCM-41). • Fe_3O_4@B-MCM-41 as reusable catalyst for the synthesis of polyhydroquinolines. • Characterization of Fe_3O_4@B-MCM-41 using SEM, TEM, BET, XRD and FT-IR techniques.

  17. Spectral studies on the interaction of acetylacetone with aluminum-containing MCM-41 mesoporous materials

    International Nuclear Information System (INIS)

    Zanjanchi, M.A.; Vaziri, M.

    2008-01-01

    Diffuse reflectance spectroscopy (DRS) was used to study the interaction of acetylacetone (acac) with the mesoporous aluminum-containing MCM-41 materials. A room temperature synthesis method was used for preparation of purely siliceous MCM-41 and for aluminum-containing MCM-41 materials. Samples with Si/Al ratios of 50, 20, 10 and 5 were synthesized. The synthesized mesoporous materials possess highly ordered structure and high surface area as evidenced from X-ray diffraction and nitrogen physisorption measurements, respectively. The treatment of the as-synthesized aluminum-containing MCM-41 samples with acac shows a distinct band at ∼290 nm. This band is assigned to six coordinated aluminum atoms in the structure which is produced by diffusion of acac molecules through surfactant micelles and their interaction with aluminum atoms. The 290-nm band disappears upon several successive washing of the sample with ethanol. The treatment of the calcined aluminum-containing MCM-41 sample with acac produces the same 290-nm band where its intensity increases with the aluminum content of the sample. The intensity of this band is reduced upon successive ethanol washing, but remains nearly constant after three times washing. This irremovable aluminum species can be assigned to framework aluminum. The measured acidity for our aluminum-containing MCM-41 samples correlates linearly with the intensity of 290-nm band for the ethanol treated samples. This supports the idea that the Bronsted acidity in aluminum-modified MCM-41 samples is a function of the amount of tetrahedral framework aluminum in the structure

  18. Density profile of nitrogen in cylindrical pores of MCM-41

    Science.gov (United States)

    Soper, Alan K.; Bowron, Daniel T.

    2017-09-01

    A straightforward approach using radiation scattering (X-ray or neutron) combined with atomistic modelling is used to accurately assess the pore dimensions in the porous silica, MCM-41. The method is used to calculate the density profile of nitrogen absorbed in this material at a variety of fractional pressures, p/p0, where p0 is the saturated vapour pressure, up to p/p0 = 0.36 at T = 87 K in the present instance. At this pressure two distinct layers of liquid nitrogen occur on the silica surface, with a relatively sharp gas-liquid interface. It is suggested surface tension effects at this interface strongly influence the growth of further layers.

  19. Fuels by Waste Plastics Using Activated Carbon, MCM-41, HZSM-5 and Their Mixture

    Directory of Open Access Journals (Sweden)

    Miskolczi Norbert

    2016-01-01

    Full Text Available Waste material was pyrolyzed in a horizontal tubular reactor at 530-540°C using different catalysts, such as activated carbon, MCM-41, HZSM-5 and their mixtures. Products were investigated by gas-chromatography, EDXRFS and standardized methods. Catalysts significantly affected the yields of volatiles; e.g. HZSM-5 catalyst increased especially the yield of gaseous hydrocarbons, while MCM-41 catalyst was responsible for increasing the pyrolysis oil yield. Synergistic effects were found using mixtures of different catalysts. Furthermore the catalysts modified the main carbon frame of the products. Pyrolysis oil obtained over HZSM-5 catalyst contained large amounts of aromatics, while MCM-41 catalyst mainly isomerized the carbon frame. Regarding contaminants it was concluded, that the sulphur content could be significantly decreased by activated carbon, however it had only a slight effect to the other properties of the products.

  20. Steam-assisted crystallization of TPA+-exchanged MCM-41 type mesoporous materials with thick pore walls

    International Nuclear Information System (INIS)

    Chen, Hong Li; Zhang, Kun; Wang, Yi Meng

    2012-01-01

    Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, 1 H– 13 C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show that the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.

  1. Aluminum Doped MCM-41 Nanoparticles as Platforms for the Dual Encapsulation of a CO-Releasing Molecule and Cisplatin.

    Science.gov (United States)

    Carmona, Francisco J; Jiménez-Amezcua, Ignacio; Rojas, Sara; Romão, Carlos C; Navarro, Jorge A R; Maldonado, Carmen R; Barea, Elisa

    2017-09-05

    Mesoporous silica Al-MCM-41 nanoparticles have been used, for the first time, as vehicles for the single and dual encapsulation of the cationic CO-releasing molecule (CORM) [Mn(1,4,7-triazacyclononane)(CO) 3 ] + (ALF472 + ) and the well-known antineoplastic drug, cis-[PtCl 2 (NH 3 ) 2 ] (cisplatin). Thus, two new hybrid materials, namely, ALF472@Al-MCM-41 and ALF472-cisplatin@Al-MCM-41, have been isolated and fully characterized. The results reveal that the presence of CORM molecules enhances cisplatin loading 3-fold, yielding a cargo of 0.45 mmol g -1 of ALF472 + and 0.12 mmol g -1 of the platinum complex for ALF472-cisplatin@Al-MCM-41. It is worth noting that ALF472@Al-MCM-41 shows a good dispersion in phosphate buffered saline solution, while the dual hybrid material slightly aggregates in this simulated physiological medium (hydrodynamic size: 112 ± 23 and 336 ± 50 nm, respectively). In addition, both hybrid materials (ALF472@Al-MCM-41 and ALF472-cisplatin@Al-MCM-41) behave as photoactive CO-releasing materials, delivering 0.25 and 0.11 equiv of CO, respectively, after 24 h and exhibiting a more controlled CO delivery than that of the free CORM. Finally, metal leaching studies have confirmed the good retention capacity of Al-MCM-41 toward the potentially toxic manganese fragments (86% of retention after 72 h) as well as the low release of cisplatin (ca. 7% after 72 h).

  2. UTILIZATION OF RICE HUSK AS RAW MATERIAL IN SYNTHESIS OF MESOPOROUS SILICATES MCM-41

    Directory of Open Access Journals (Sweden)

    Suyanta Suyanta

    2011-12-01

    Full Text Available The research about synthesis and characterization of MCM-41 from rice husk has been done. Silica (SiO2 was extracted from rice husk by refluxing with 3M hydrochloric solution at 80 °C for 3 h. The acid-leached rice husk was filtered, washed, dried and calcined at 650 °C for 6 h lead the rough powder of rice husk silica with light brown in color. Characterization was carried out by X-ray diffraction (XRD and FTIR spectroscopy method. Rice husk silica was dissolved into the sodium hydroxide solution leading to the solution of sodium silicate, and used as silica source for the synthesis of MCM-41. MCM-41 was synthesized by hydrothermal process to the mixture prepared from 29 g of distilled water, 8.67 g of cetyltrimethyl ammonium bromide (CTMAB, 9.31 g of sodium silicate solution, and amount mL of 1 M H2SO4. Hydrothermal process was carried out at 100 °C in a teflon-lined stainless steel autoclave heated in the oven for 36 h. The solid phase was filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcination at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined crystals were characterized by using FTIR spectroscopy, X-ray diffraction and N2 physisorption methods. In order to investigate the effect of silica source, the same procedure was carried out by using pure sodium silicate as silica source. It was concluded that silica extracted from rice husk can be used as raw materials in the synthesis of MCM-41, there is no significant difference in crystallinity and pore properties when was compared to material produced from commercial sodium silicate.

  3. Response of Fibroblasts MRC-5 to Flufenamic Acid-Grafted MCM-41 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Giovanna Gomes Lara

    2018-01-01

    Full Text Available Recently, flufenamic acid (FFA was discovered among fenamates as a free radical scavenger and gap junction blocker; however, its effects have only been studied in cancer cells. Normal cells in the surroundings of a tumor also respond to radiation, although they are not hit by it directly. This phenomenon is known as the bystander effect, where response molecules pass from tumor cells to normal ones, through communication channels called gap junctions. The use of the enhanced permeability and retention effect, through which drug-loaded nanoparticles smaller than 200 nm may accumulate around a tumor, can prevent the local side effect upon controlled release of the drug. The present work, aimed at functionalizing MCM-41 (Mobil Composition of Matter No. 41 silica nanoparticles with FFA and determining its biocompatibility with human fibroblasts MRC-5 (Medical Research Council cell strain 5. MCM-41, was synthesized and characterized structurally and chemically, with multiple techniques. The biocompatibility assay was performed by Live/Dead technique, with calcein and propidium–iodide. MRC-5 cells were treated with FFA-grafted MCM-41 for 48 h, and 98% of cells remained viable, without signs of necrosis or morphological changes. The results show the feasibility of MCM-41 functionalization with FFA, and its potential protection of normal cells, in comparison to the role of FFA in cancerous ones.

  4. Response of Fibroblasts MRC-5 to Flufenamic Acid-Grafted MCM-41 Nanoparticles.

    Science.gov (United States)

    Lara, Giovanna Gomes; Cipreste, Marcelo Fernandes; Andrade, Gracielle Ferreira; Silva, Wellington Marcos da; Sousa, Edésia Martins Barros de

    2018-01-09

    Recently, flufenamic acid (FFA) was discovered among fenamates as a free radical scavenger and gap junction blocker; however, its effects have only been studied in cancer cells. Normal cells in the surroundings of a tumor also respond to radiation, although they are not hit by it directly. This phenomenon is known as the bystander effect, where response molecules pass from tumor cells to normal ones, through communication channels called gap junctions. The use of the enhanced permeability and retention effect, through which drug-loaded nanoparticles smaller than 200 nm may accumulate around a tumor, can prevent the local side effect upon controlled release of the drug. The present work, aimed at functionalizing MCM-41 (Mobil Composition of Matter No. 41) silica nanoparticles with FFA and determining its biocompatibility with human fibroblasts MRC-5 (Medical Research Council cell strain 5). MCM-41, was synthesized and characterized structurally and chemically, with multiple techniques. The biocompatibility assay was performed by Live/Dead technique, with calcein and propidium-iodide. MRC-5 cells were treated with FFA-grafted MCM-41 for 48 h, and 98% of cells remained viable, without signs of necrosis or morphological changes. The results show the feasibility of MCM-41 functionalization with FFA, and its potential protection of normal cells, in comparison to the role of FFA in cancerous ones.

  5. Composite hydrogel based on surface modified mesoporous silica and poly[(2-acryloyloxy)ethyl trimethylammonium chloride

    International Nuclear Information System (INIS)

    Torres, Cecilia C.; Urbano, Bruno F.; Campos, Cristian H.; Rivas, Bernabé L.; Reyes, Patricio

    2015-01-01

    This work focused on the synthesis, characterization and water absorbency of a composite hydrogel based on poly[(2-acryloyloxy)ethyl trimethylammonium chloride] and mesoporous silica, MCM-41. The MCM-41 was synthesized and later surface functionalized with triethoxyvinylsilane (VTES) and 3-trimethoxysilylpropylmethacrylate (TMSPM) by a post-grafting procedure. The composite hydrogels were obtained by in-situ polymerization using a mixture of monomer, crosslinker and initiator in the presence of functionalized MCM-41. Diverse characterization techniques were used at the different stages of synthesis, namely, FT-IR, TEM, SEM, DRX, 29 Si and 13 C solid state NMR, and N 2 adsorption isotherms at 77 K. Finally, the water uptake performance of the composites was tested as a function of time, mesoporous silica loading and coupling agent used at the functionalization. The composites using non-functionalized MCM-41 reached the highest water uptake, whereas those composite with MCM-41 TMSPM exhibited the lowest sorption. - Highlights: • Hydrophilic crosslinked polymer-mesoporous silica was obtained. • Mesoporous silica MCM-41 was synthesized and functionalized with organosilane. • Functionalization of MCM-41 affects the water uptake of composite. • Mesoporous silica is covalently bound to the polymer acting as crosslinked point

  6. Composite hydrogel based on surface modified mesoporous silica and poly[(2-acryloyloxy)ethyl trimethylammonium chloride

    Energy Technology Data Exchange (ETDEWEB)

    Torres, Cecilia C. [Department of Organic Chemistry, Faculty of Chemical Science, University of Concepción (Chile); Urbano, Bruno F., E-mail: burbano@udec.cl [Department of Polymer Chemistry, Faculty of Chemical Science, University of Concepción (Chile); Campos, Cristian H. [Department of Organic Chemistry, Faculty of Chemical Science, University of Concepción (Chile); Rivas, Bernabé L. [Department of Polymer Chemistry, Faculty of Chemical Science, University of Concepción (Chile); Reyes, Patricio [Department of Physical Chemistry, Faculty of Chemical Science, University of Concepción (Chile)

    2015-02-15

    This work focused on the synthesis, characterization and water absorbency of a composite hydrogel based on poly[(2-acryloyloxy)ethyl trimethylammonium chloride] and mesoporous silica, MCM-41. The MCM-41 was synthesized and later surface functionalized with triethoxyvinylsilane (VTES) and 3-trimethoxysilylpropylmethacrylate (TMSPM) by a post-grafting procedure. The composite hydrogels were obtained by in-situ polymerization using a mixture of monomer, crosslinker and initiator in the presence of functionalized MCM-41. Diverse characterization techniques were used at the different stages of synthesis, namely, FT-IR, TEM, SEM, DRX, {sup 29}Si and {sup 13}C solid state NMR, and N{sub 2} adsorption isotherms at 77 K. Finally, the water uptake performance of the composites was tested as a function of time, mesoporous silica loading and coupling agent used at the functionalization. The composites using non-functionalized MCM-41 reached the highest water uptake, whereas those composite with MCM-41 TMSPM exhibited the lowest sorption. - Highlights: • Hydrophilic crosslinked polymer-mesoporous silica was obtained. • Mesoporous silica MCM-41 was synthesized and functionalized with organosilane. • Functionalization of MCM-41 affects the water uptake of composite. • Mesoporous silica is covalently bound to the polymer acting as crosslinked point.

  7. Epoxidation of limonene over Ti MCM 41 and Ti BETA

    International Nuclear Information System (INIS)

    Cubillos Lobo, Jairo Antonio; Gonzalez Rodriguez, Lina Maria; Montes de Correa, Consuelo

    2002-01-01

    Ti MCM 41 were synthesized and evaluated in the epoxidation of limonene, using peroxide of hydrogen (H 2 O) as agent oxidizer. The characteristic hexagonal phase of Ti MCM 41 was obtained by heating the precursor gel during three days at 100 centigrade degrees. Further heating up to ten days leads to a decrease of this phase. The increase (Ti) in the synthesis gel also decreases that phase. The increase of Ti in the synthesis gel also decreases that phase UV VIS and FTIR spectroscopy indicates that Ti was incorporated in the lattice of Ti MCM 41 as well as, in Ti BETA. SEM micrographs of Ti MCM 41 show that the morphology changes with the Ti loading. Ti MCM 41 was most active than Ti BETA for limonene epoxidation even though both show high selectivity to epoxides

  8. Improvement of the Derjaguin-Broekhoff-de Boer theory for capillary condensation/evaporation of nitrogen in mesoporous systems and its implications for pore size analysis of MCM-41 silicas and related materials.

    Science.gov (United States)

    Kowalczyk, Piotr; Jaroniec, Mietek; Terzyk, Artur P; Kaneko, Katsumi; Do, Duong D

    2005-03-01

    In this work, we propose an improvement of the classical Derjaguin-Broekhoff-de Boer (DBdB) theory for capillary condensation/evaporation in mesoporous systems. The primary idea of this improvement is to employ the Gibbs-Tolman-Koenig-Buff equation to predict the surface tension changes in mesopores. In addition, the statistical film thickness (so-called t-curve) evaluated accurately on the basis of the adsorption isotherms measured for the MCM-41 materials is used instead of the originally proposed t-curve (to take into account the excess of the chemical potential due to the surface forces). It is shown that the aforementioned modifications of the original DBdB theory have significant implications for the pore size analysis of mesoporous solids. To verify our improvement of the DBdB pore size analysis method (IDBdB), a series of the calcined MCM-41 samples, which are well-defined materials with hexagonally ordered cylindrical mesopores, were used for the evaluation of the pore size distributions. The correlation of the IDBdB method with the empirically calibrated Kruk-Jaroniec-Sayari (KJS) relationship is very good in the range of small mesopores. So, a major advantage of the IDBdB method is its applicability for small mesopores as well as for the mesopore range beyond that established by the KJS calibration, i.e., for mesopore radii greater than approximately 4.5 nm. The comparison of the IDBdB results with experimental data reported by Kruk and Jaroniec for capillary condensation/evaporation as well as with the results from nonlocal density functional theory developed by Neimark et al. clearly justifies our approach. Note that the proposed improvement of the classical DBdB method preserves its original simplicity and simultaneously ensures a significant improvement of the pore size analysis, which is confirmed by the independent estimation of the mean pore size by the powder X-ray diffraction method.

  9. A potential bioactive wound dressing based on carboxymethyl cellulose/ZnO impregnated MCM-41 nanocomposite hydrogel

    Energy Technology Data Exchange (ETDEWEB)

    Rakhshaei, Rasul [Research Laboratory of Dendrimers and Nanopolymers, Faculty of Chemistry, University of Tabriz, P.O. Box 51666, Tabriz (Iran, Islamic Republic of); Namazi, Hassan, E-mail: namazi@tabrizu.ac.ir [Research Laboratory of Dendrimers and Nanopolymers, Faculty of Chemistry, University of Tabriz, P.O. Box 51666, Tabriz (Iran, Islamic Republic of); Research Center for Pharmaceutical Nanotechnology, Tabriz University of Medical Science, Tabriz (Iran, Islamic Republic of)

    2017-04-01

    Lack of antibacterial activity, deficient water vapor and oxygen permeability, and insufficient mechanical properties are disadvantages of existing wound dressings. Hydrogels could absorb wound exudates due to their strong swelling ratio and give a cooling sensation and a wet environment. To overcome these shortcomings, flexible nanocomposite hydrogel films was prepared through combination of zinc oxide impregnated mesoporous silica (ZnO-MCM-41) as a nano drug carrier with carboxymethyl cellulose (CMC) hydrogel. Citric acid was used as cross linker to avoid the cytotoxicity of conventional cross linkers. The prepared nanocomposite hydrogel was characterized using X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential and UV–vis spectroscopy. Results of swelling and erosion tests showed CMC/ZnO nanocomposite hydrogel disintegrated during the first hours of the test. Using MCM-41 as a substrate for ZnO nanoparticles solved this problem and the CMC/ZnO-MCM-41 showed a great improvement in tensile strength (12%), swelling (100%), erosion (53%) and gas permeability (500%) properties. Drug delivery and antibacterial properties of the nanocomposite hydrogel films studied using tetracycline (TC) as a broad spectrum antibiotic and showed a sustained TC release. This could efficiently decrease bandage exchange. Cytocompatibility of the nanocomposite hydrogel films has been analyzed in adipose tissue-derived stem cells (ADSCs) and results showed cytocompatibility of CMC/ZnO-MCM-41. Based on these results the prepared CMC nanocomposite hydrogel containing ZnO impregnated MCM-41, could serve as a kind of promising wound dressing with sustained drug delivery properties. - Highlights: • CMC nanocomposite hydrogel incorporated with TC loaded ZnO-MCM-41 nanoparticles have been prepared as active wound dressing. • Citric acid was used as cross linker to avoid conventional toxic crosslinkers. • CMC/ZnO-MCM-41

  10. Butanol Dehydration over V₂O₅-TiO₂/MCM-41 Catalysts Prepared via Liquid Phase Atomic Layer Deposition.

    Science.gov (United States)

    Choi, Hyeonhee; Bae, Jung-Hyun; Kim, Do Heui; Park, Young-Kwon; Jeon, Jong-Ki

    2013-04-29

    MCM-41 was used as a support and, by using atomic layer deposition (ALD) in the liquid phase, a catalyst was prepared by consecutively loading titanium oxide and vanadium oxide to the support. This research analyzes the effect of the loading amount of vanadium oxide on the acidic characteristics and catalytic performance in the dehydration of butanol. The physical and chemical characteristics of the TiO₂-V₂O₅/MCM-41 catalysts were analyzed using XRF, BET, NH₃-TPD, XRD, Py-IR, and XPS. The dehydration reaction of butanol was performed in a fixed bed reactor. For the samples with vanadium oxide loaded to TiO₂/MCM-41 sample using the liquid phase ALD method, it was possible to increase the loading amount until the amount of vanadium oxide reached 12.1 wt %. It was confirmed that the structural properties of the mesoporous silica were retained well after titanium oxide and vanadium loading. The NH₃-TPD and Py-IR results indicated that weak acid sites were produced over the TiO₂/MCM-41 samples, which is attributed to the generation of Lewis acid sites. The highest activity of the V₂O₅(12.1)-TiO₂/MCM-41 catalyst in 2-butanol dehydration is ascribed to it having the highest number of Lewis acid sites, as well as the highest vanadium dispersion.

  11. Enhanced adsorptive and photocatalytic achievements in removal of methylene blue by incorporating tungstophosphoric acid-TiO2 into MCM-41

    International Nuclear Information System (INIS)

    Zanjanchi, M.A.; Golmojdeh, H.; Arvand, M.

    2009-01-01

    The use of titania-dispersed materials in photocatalytic processes has been proposed as an alternative to the conventional bare TiO 2 , in order to modify the surface area and activity of the catalyst. A homogeneously dispersed Keggin unit into TiO 2 was synthesized using tungstophosphoric acid (TPA) and titanium tetraisopropoxide. This compound was then loaded into MCM-41 by dispersing it in a suspension containing the mesoporous phase. Two other titanium-containing MCM-41 catalysts, Ti-MCM-41 and TiO 2 /MCM-41 were also prepared using isomorphous substitution synthesis method and impregnation method, respectively, for the sake of comparison. The prepared photocatalysts were characterized by X-ray diffraction (XRD), nitrogen physisorption (BET) and chemical analysis. The catalysts were used to study degradation of methylene blue (MB) in aqueous solution. XRD result shows a pure anatase crystalline phase for TPA-containing TiO 2 indicating that there is good molecular distribution of tungstophosphoric acid into TiO 2 structure. Supported TPA-TiO 2 into MCM-41 shows both TPA-TiO 2 and MCM-41 characteristic X-ray reflections in the high-angle and low-angle parts of the XRD patterns, respectively. The experimental results show that adsorption is a major constituent in the elimination of MB from the dye solutions by the TPA-containing materials. Exploitation of both adsorption and photocatalytic processes speeds up the removal of the dye using the TPA-TiO 2 -loaded MCM-41 photocatalyst. The elimination of MB is completed within 15 min for a 30 mg l -1 MB solution containing a catalyst dose of 100 mg/100 ml. The efficiencies of the other photocatalysts such as commercial TiO 2 , Ti-MCM-41, TiO 2 /MCM-41 and TPA-TiO 2 for adsorption and degradation of MB were also studied and compared with that of the prepared catalyst.

  12. Hidrólise de celulose por catalisadores mesoestruturados NiO-MCM-41 e MoO3-MCM-41

    Directory of Open Access Journals (Sweden)

    Adriano Sant'Ana Silva

    2012-01-01

    Full Text Available This study was carried out to synthesize, characterize and evaluate the application of mesoestruturated catalysts MCM-41, 5%MoO3-MCM-41 and 5%NiO-MCM-41 in the hydrolysis of microcrystalline cellulose. XRD results indicate that the phase of mesoporous MCM-41 was obtained and that the introduction of metal oxides did not affect this mesoporous phase. About the heterogeneous hydrolysis reaction, it was observed that the increase in temperature results in a higher concentration of glucose and the catalyst 5%MoO3-MCM-41 provides the highest concentrations of glucose.

  13. Dehidroisomerización de n-butano sobre catalizadores bifuncionales tipo Al-MCM-41 y Ga-MCM-41 impregnados con Pt o Ga

    Directory of Open Access Journals (Sweden)

    Dino Brisigotti

    2006-05-01

    Full Text Available A series of bi-functional catalysts was prepared by using Al-MCM-41 and Ga-MCM-41 with Si/Me ratios of 15 and 50 impregnated with 0,5 Wt% of Pt or Ga. The n-butane dehydroisomerization was studied at 773 K. Catalysts based on Pt/Al-MCM-41 were less selective (more hydrogenolyzing than those based on Ga-MCM-41. For the latter, Ga species segregated to extra-framework positions might exercise a kind of geometric effect on the Pt clusters inhibiting hydrogenolysis. The catalyst Ga/Al-MCM-41 showed the closest approach to the ideal dehydroisomerization catalyst.

  14. Blue-green photoluminescence in MCM-41 mesoporous nanotubes

    CERN Document Server

    Shen, J L; Lui, Y L; Cheng, P W; Cheng, C F

    2003-01-01

    Different photoluminescence (PL) techniques have been used to study the blue-green emission from siliceous MCM-41 nanotubes. It was found that the intensity of the blue-green PL is enhanced by rapid thermal annealing (RTA). This enhancement is explained by the generation of twofold-coordinated Si centres and non-bridging oxygen hole centres, in line with the surface properties of MCM-41. On the basis of the analysis of the PL following RTA, polarized PL, and PL excitation, we suggest that the triplet-to-singlet transition of twofold-coordinated silicon centres is responsible for the blue-green PL in MCM-41 nanotubes. (letter to the editor)

  15. 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

  16. MCM-41 functionalized with YVO{sub 4}:Eu{sup 3+}: a novel drug delivery system

    Energy Technology Data Exchange (ETDEWEB)

    Yang Piaoping [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Quan Zewei [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Lu Lanlan [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Huang Shanshan [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Lin Jun [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Fu Honggang [School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080 (China)

    2007-06-13

    Luminescence functionalization of ordered mesoporous MCM-41 silica was realized by depositing a YVO{sub 4}:Eu{sup 3+} phosphor layer on its surface via the Pechini sol-gel process. This material, which combines the mesoporous structure of MCM-41 and the strong red luminescence property of YVO{sub 4}:Eu{sup 3+}, has been studied as a host carrier for drug delivery/release systems. The structure, morphology, texture and optical properties of Materials were well characterized by x-ray diffraction (XRD), Fourier infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), N{sub 2} adsorption and photoluminescence (PL) spectra. The results indicated that the specific surface area and pore volume of MCM-41, which were directly correlated to the drug-loading amount and ibuprofen (IBU) release rate, decreased in sequence after deposition of YVO{sub 4}:Eu{sup 3+} and loading of IBU as expected. The IBU-loaded YVO{sub 4}:Eu{sup 3+}MCM-41 system still showed red luminescence under UV irradiation (365 nm) and a controlled release property for IBU. In addition, the emission intensity of Eu{sup 3+} increases with an increase in the cumulative released amount of IBU, making the extent of drug release easily identified, tracked and monitored by the change of luminescence, which demonstrates its potential application in drug delivery/release systems.

  17. Adsorption of CO2 on amine-functionalised MCM-41: experimental and theoretical studies.

    Science.gov (United States)

    dos Santos, Thiago Custódio; Bourrelly, Sandrine; Llewellyn, Philip L; Carneiro, José Walkimar de M; Ronconi, Célia Machado

    2015-04-28

    Adsorption of CO2 on MCM-41 functionalised with [3-(2-aminoethylamino)propyl]trimethoxysilane (MCM-41-N2), N(1)-(3-trimethoxysilylpropyl)diethylenetriamine (MCM-41-N3), 4-aminopyridine (MCM-41-aminopyridine), 4-(methylamino)pyridine (MCM-41-methylaminopyridine) and 1,5,7-triazabicyclo[4.4.0]dec-5-ene (MCM-41-guanidine) was investigated. The amine-functionalised materials were characterised by (29)Si and (13)C solid-state nuclear magnetic resonance, N2 adsorption/desorption isotherms, X-ray diffraction and transmission electron microscopy. CO2 adsorption at 1.0 bar and 30 °C showed that the amount of CO2 (nads/mmol g(-1)) adsorbed on MCM-41-N2 and MCM-41-N3 is approximately twice the amount adsorbed on MCM-41. For MCM-41-aminopyridine, MCM-41-methylaminopyridine and MCM-41-guanidine, the CO2 adsorption capacity was smaller than that of MCM-41 at the same conditions. The proton affinity (computed with wB97x-D/6-311++G(d,p)) of the secondary amino groups is higher than that of the primary amino groups; however, the relative stabilities of the primary and secondary carbamates are similar. The differential heat of adsorption decreases as the number of secondary amino groups increases.

  18. Preparation of Organic-Inorganic Hybrid Materials Based on MCM-41 and Its Applications

    Directory of Open Access Journals (Sweden)

    Sana M. Alahmadi

    2013-01-01

    Full Text Available This work reports the covalent attachment of three different calix[4]arenes (calix[4]arene (C4, p-sulfonatocalix[4]arene (C4S, and p-tert-butyl-calix[4]arene (PC4 to MCM-41, using a three-step modification process. 3-Chloropropyltrimethoxysilane (ClPTS was first attached to the mesoporous silica surface and subsequently converted to amides via the reaction with toluene diisocyanate (TDI. Finally, calix[4]arene derivatives attached to the isocyanate ending remained available on toluene di-iso-cyanate. Changes in the surface properties of the mesoporous silica caused by the chemical modification were monitored using the Fourier transform infrared spectroscopy (FTIR, thermal analysis (TGA, and elemental analysis. The FTIR spectra and TGA analysis verify that the calix[4]arene derivatives are covalently attached to the mesoporous silica. The preservation of the MCM-41 channel system was checked by the X-ray diffraction and nitrogen adsorption analysis. These materials were then used to evaluate the sorption properties of some organotins compounds (Tributyltin (TBT, Triphenyltin (TPT, and Dibutyltin (DBT.

  19. A potential bioactive wound dressing based on carboxymethyl cellulose/ZnO impregnated MCM-41 nanocomposite hydrogel.

    Science.gov (United States)

    Rakhshaei, Rasul; Namazi, Hassan

    2017-04-01

    Lack of antibacterial activity, deficient water vapor and oxygen permeability, and insufficient mechanical properties are disadvantages of existing wound dressings. Hydrogels could absorb wound exudates due to their strong swelling ratio and give a cooling sensation and a wet environment. To overcome these shortcomings, flexible nanocomposite hydrogel films was prepared through combination of zinc oxide impregnated mesoporous silica (ZnO-MCM-41) as a nano drug carrier with carboxymethyl cellulose (CMC) hydrogel. Citric acid was used as cross linker to avoid the cytotoxicity of conventional cross linkers. The prepared nanocomposite hydrogel was characterized using X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential and UV-vis spectroscopy. Results of swelling and erosion tests showed CMC/ZnO nanocomposite hydrogel disintegrated during the first hours of the test. Using MCM-41 as a substrate for ZnO nanoparticles solved this problem and the CMC/ZnO-MCM-41 showed a great improvement in tensile strength (12%), swelling (100%), erosion (53%) and gas permeability (500%) properties. Drug delivery and antibacterial properties of the nanocomposite hydrogel films studied using tetracycline (TC) as a broad spectrum antibiotic and showed a sustained TC release. This could efficiently decrease bandage exchange. Cytocompatibility of the nanocomposite hydrogel films has been analyzed in adipose tissue-derived stem cells (ADSCs) and results showed cytocompatibility of CMC/ZnO-MCM-41. Based on these results the prepared CMC nanocomposite hydrogel containing ZnO impregnated MCM-41, could serve as a kind of promising wound dressing with sustained drug delivery properties. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Thermal and hydrothermal stability of ZrMCM-41 mesoporous ...

    Indian Academy of Sciences (India)

    Administrator

    The mesoporous structure of the ZrMCM-41 mesoporous molecular sieve still retains after calcination at 750°C for 3 h or ... adsorption, sensor and petrochemical industry. 2–5. However, the ... the pH value of the mixed solution was adjusted to.

  1. Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

    Energy Technology Data Exchange (ETDEWEB)

    Omidi, Fariborz [Department of Occupational Health Engineering, School of Public Health, Shahroud University of Medical Sciences, Shahroud (Iran, Islamic Republic of); Behbahani, Mohammad, E-mail: mohammadbehbahai89@yahoo.com [Department of Chemistry, Shahid Beheshti University, Evin, Tehran (Iran, Islamic Republic of); Kalate Bojdi, Majid [Faculty of Chemistry, Kharazmi (Tarbiat Moallem) University, Tehran (Iran, Islamic Republic of); Shahtaheri, Seyed Jamaleddin [Department of Occupational Health Engineering, School of Public Health and Institute for Environmental Research, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

    2015-12-01

    A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe{sub 3}O{sub 4}@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe{sub 3}O{sub 4}@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe{sub 3}O{sub 4}@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe{sub 3}O{sub 4}@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L{sup –1} and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g{sup −1}. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results. - Highlights: • The introducing of modified magnetic mesoporous silica as a novel magnetic sorbent. • Trace monitoring of cadmium ions. • The limit of detection (LOD) by the proposed solid phase extraction method was 0.04 ng mL{sup −1} for the cadmium ions. • High surface areas and magnetic characteristic of the sorbent. • Maximum adsorption capacity of the sorbent was 154 mg g{sup −1}.

  2. Dehydration of xylose to furfural over MCM-41-supported niobium-oxide catalysts.

    Science.gov (United States)

    García-Sancho, Cristina; Sádaba, Irantzu; Moreno-Tost, Ramón; Mérida-Robles, Josefa; Santamaría-González, José; López-Granados, Manuel; Maireles-Torres, Pedro

    2013-04-01

    A series of silica-based MCM-41-supported niobium-oxide catalysts are prepared, characterized by using XRD, N2 adsorption-desorption, X-ray photoelectron spectroscopy, Raman spectroscopy, and pyridine adsorption coupled to FTIR spectroscopy, and tested for the dehydration of D-xylose to furfural. Under the operating conditions used all materials are active in the dehydration of xylose to furfural (excluding the MCM-41 silica support). The xylose conversion increases with increasing Nb2 O5 content. At a loading of 16 wt % Nb2 O5 , 74.5 % conversion and a furfural yield of 36.5 % is achieved at 170 °C, after 180 min reaction time. Moreover, xylose conversion and furfural yield increase with the reaction time and temperature, attaining 82.8 and 46.2 %, respectively, at 190 °C and after 100 min reaction time. Notably, the presence of NaCl in the reaction medium further increases the furfural yield (59.9 % at 170 °C after 180 min reaction time). Moreover, catalyst reutilization is demonstrated by performing at least three runs with no loss of catalytic activity and without the requirement for an intermediate regeneration step. No significant niobium leaching is observed, and a relationship between the structure of the catalyst and the activity is proposed. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. A study on hydrogen-storage behaviors of nickel-loaded mesoporous MCM-41.

    Science.gov (United States)

    Park, Soo-Jin; Lee, Seul-Yi

    2010-06-01

    The objective of the present work was to investigate the possibility of improving the hydrogen-storage capacity of mesoporous MCM-41 containing nickel (Ni) oxides (Ni/MCM-41). The MCM-41 and Ni/MCM-41 were prepared using a hydrothermal process as a function of Ni content (2, 5, and 10 wt.% in the MCM-41). The surface functional groups of the Ni/MCM-41 were identified by Fourier transform infrared spectroscopy (FTIR). The structure and morphology of the Ni/MCM-41 were characterized by X-ray diffraction (XRD) and field emission transmission electron microscopy (FE-TEM). XRD results showed a well-ordered hexagonal pore structure; FE-TEM also revealed, as a complementary technique, the structure and pore size. The textural properties of the Ni/MCM-41 were analyzed using N(2) adsorption isotherms at 77 K. The hydrogen-storage capacity of the Ni/MCM-41 was evaluated at 298 K/100 bar. It was found that the presence of Ni on mesoporous MCM-41 created hydrogen-favorable sites that enhanced the hydrogen-storage capacity by a spillover effect. Furthermore, it was concluded that the hydrogen-storage capacity was greatly influenced by the amount of nickel oxide, resulting in a chemical reaction between Ni/MCM-41 and hydrogen molecules. Crown Copyright © 2010. Published by Elsevier Inc. All rights reserved.

  4. Synthesis and characterization of mesoporous Si–MCM-41 ...

    Indian Academy of Sciences (India)

    Administrator

    Table S1. MCM-41 synthesis strategies—parameters optimized. BET surface area at different temperature (m2/g). SiO2. Template Template H2O Temp. Aging. Parameters. No. source source mole mole. (°C) time (h) pH. 550 °C. 700 °C. 900 °C. Aging time. 1. Na2SiO3. CTABr. 0⋅25. 80. RT. 1. 10⋅5. 640. 490. 370. 2.

  5. MCM-41 ordered mesoporous molecular sieves synthesis and characterization

    Directory of Open Access Journals (Sweden)

    Rogério A.A. Melo

    1999-07-01

    Full Text Available The aim of this work was to study the hydrothermal synthesis of Si and SiAlMCM-41 performed under both autogenic pressure and refluxing conditions. XRD data showed that the MCM-41 phase may be formed by both processes and that the synthesized material in the presence of Al and/or under reflux presents the hexagonally arrangement of less ordered mesopores. However, as verified by XRD and physisorption data, the order was improved with higher synthesis times. 29Si and 1H - 29Si C/P MAS NMR spectra showed that a great part of the Si atoms exists as silanol groups which originate resonance peaks at -110, -100 and -91 ppm. The presence of Al atoms may generate Si(3Si, Al and Si(2Si, 2Al environments which might be contributing to resonance peaks at -100 and -91 ppm. The 27Al MAS NMR spectrum of the as synthesized AlSiMCM-41 showed a resonance peak of tetrahedral framework aluminum close to 53 ppm and two others, one close to 14 ppm attributed to Al(H2O6+3 species and the other a weak signal close to 32 ppm attributed to pentacoordinated Al. 27Al MAS NMR spectra of the calcined sample showed a peak at 0 ppm corresponding to an hexacoordinated extra-framework aluminum formed during calcination.

  6. o-Vanillin functionalized mesoporous silica - coated magnetite nanoparticles for efficient removal of Pb(II) from water

    Science.gov (United States)

    Culita, Daniela C.; Simonescu, Claudia Maria; Patescu, Rodica-Elena; Dragne, Mioara; Stanica, Nicolae; Oprea, Ovidiu

    2016-06-01

    o-Vanillin functionalized mesoporous silica - coated magnetite (Fe3O4@MCM-41-N-oVan) was synthesized and fully characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, N2 adsorption-desorption technique and magnetic measurements. The capacity of Fe3O4@MCM-41-N-oVan to adsorb Pb(II) from aqueous solutions was evaluated in comparison with raw mesoporous silica - coated magnetite (Fe3O4@MCM-41) and amino - modified mesoporous silica coated magnetite (Fe3O4@MCM-41-NH2). The effect of adsorption process parameters such us pH, contact time, initial Pb(II) concentration was also investigated. The adsorption data were successfully fitted with the Langmuir model, exhibiting a maximum adsorption capacity of 155.71 mg/g at pH=4.4 and T=298 K. The results revealed that the adsorption rate was very high at the beginning of the adsorption process, 80-90% of the total amount of Pb(II) being removed within the first 60 min, depending on the initial concentration. The results of the present work suggest that Fe3O4@MCM-41-N-oVan is a suitable candidate for the separation of Pb(II) from contaminated water.

  7. Sn-MCM-41 as Efficient Catalyst for the Conversion of Glucose into 5-Hydroxymethylfurfural in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Qing Xu

    2013-11-01

    Full Text Available Recently, much attention has been paid to the development of technologies that facilitate the conversion of biomass into platform chemicals such as 5-hydroxymethylfurfural (5-HMF. In this paper, a tin-containing silica molecular sieve (Sn-MCM-41 was found to act as a bifunctional heterogeneous catalyst for the efficient conversion of glucose into 5-HMF in ionic liquid. In the presence of [EMIM]Br, the yield of 5-HMF converted from glucose reached 70% at 110 °C after 4 h. During the reaction, the active center of the catalyst first catalyzed the isomerization of glucose into fructose and then the dehydration of fructose into 5-HMF. After the reaction, the heterogeneous catalyst Sn-MCM-41 could be easily recovered and reused without a significant loss in activity. The catalyst Sn-MCM-41 was also able to catalyze the conversion of fructose into 5-HMF at an 80% yield. Moreover, the low toxicity of the Sn-based catalyst makes the method a greener approach for the conversion of saccharides into 5-HMF.

  8. Preparation of chitosan/MCM-41-PAA nanocomposites and the adsorption behaviour of Hg(II) ions

    Science.gov (United States)

    Fu, Yong; Huang, Yue; Hu, Jianshe

    2018-03-01

    A novel functional hybrid mesoporous composite material (CMP) based on chitosan and MCM-41-PAA was reported and its application as an excellent adsorbent for Hg(II) ions was also investigated. Innovatively, MCM-41-PAA was prepared by using diatomite and polyacrylic acid (PAA) with integrated polymer-silica hybrid frameworks, and then CMP was fabricated by introducing MCM-41-PAA to chitosan using glutaraldehyde as a cross-linking agent. The structure and morphology of CMP were characterized by X-ray diffraction, Fourier transform infrared spectra, thermogravimetric analysis, scanning electron microscopy and Brunauer-Emmett-Teller measurements. The results showed that the CMP possessed multifunctional groups such as -OH, -COOH and -NH2 with large specific surface area. Adsorption behaviour of Hg(II) ions onto CMP was fitted better by the pseudo-second-order kinetic model and the Langmuir model when the initial Hg(II) concentration, pH, adsorption temperature and time were 200 mg l-1, 4, 298 K and 120 min, respectively, as the optimum conditions. The corresponding maximum adsorption capacity could reach 164 mg g-1. According to the thermodynamic parameters determined such as free energy, enthalpy and entropy, the adsorption process of Hg(II) ions was spontaneous endothermic adsorption.

  9. Preparation of chitosan/MCM-41-PAA nanocomposites and the adsorption behaviour of Hg(II) ions

    Science.gov (United States)

    Fu, Yong; Huang, Yue; Hu, Jianshe

    2018-01-01

    A novel functional hybrid mesoporous composite material (CMP) based on chitosan and MCM-41-PAA was reported and its application as an excellent adsorbent for Hg(II) ions was also investigated. Innovatively, MCM-41-PAA was prepared by using diatomite and polyacrylic acid (PAA) with integrated polymer–silica hybrid frameworks, and then CMP was fabricated by introducing MCM-41-PAA to chitosan using glutaraldehyde as a cross-linking agent. The structure and morphology of CMP were characterized by X-ray diffraction, Fourier transform infrared spectra, thermogravimetric analysis, scanning electron microscopy and Brunauer–Emmett–Teller measurements. The results showed that the CMP possessed multifunctional groups such as –OH, –COOH and –NH2 with large specific surface area. Adsorption behaviour of Hg(II) ions onto CMP was fitted better by the pseudo-second-order kinetic model and the Langmuir model when the initial Hg(II) concentration, pH, adsorption temperature and time were 200 mg l−1, 4, 298 K and 120 min, respectively, as the optimum conditions. The corresponding maximum adsorption capacity could reach 164 mg g−1. According to the thermodynamic parameters determined such as free energy, enthalpy and entropy, the adsorption process of Hg(II) ions was spontaneous endothermic adsorption. PMID:29657793

  10. Synthesis, characterization, and catalytic properties of stable mesoporous molecular sieve MCM-41 prepared from zeolite mordenite

    International Nuclear Information System (INIS)

    Wang Shan; Dou Tao; Li Yuping; Zhang Ying; Li Xiaofeng; Yan Zichun

    2004-01-01

    Mesoporous molecular sieves (denoted as M-MCM-41) with ordered hexagonal structure have been successfully synthesized from the assembly of precursors from preformed zeolite Mordenite with CTAB surfactant micelle in alkaline media. The samples were characterized by XRD, N 2 adsorption, IR and DTG. The materials exhibit highly hydrothermal stability, as compared with conventional MCM-41. Characterization results indicate that the mesoporous walls of M-MCM-41 contain the secondary building units similar to those in microporous crystal of zeolite Mordenite. In catalytic dealkylation of C10 + aromatic hydrocarbon, M-MCM-41 shows higher activities in comparison with Mordenite and MCM-41, which would be ascribed to the combination of advantages of both MCM-41 (large pores) and Mordenite (strong acidity). Furthermore, this synthesis strategy could be used as a new general method for the preparation of hydrothermally stable mesoporous aluminosilicate materials under alkaline conditions

  11. Synthesis and characterization of MCM-41-supported nano zirconia catalysts

    Directory of Open Access Journals (Sweden)

    Mohamed S. Abdel Salam

    2015-03-01

    Full Text Available Series of MCM-41 supported sulfated Zirconia (SZ catalysts with different loadings (2.5–7.5% wt. were prepared using direct impregnation method. The acquired solid catalysts were characterized structurally and chemically using X-RD, HRTEM, BET, FT-IR, Raman spectroscopy and TPD analysis. The acidity of the solid catalysts was investigated through cumene cracking and isopropanol dehydration at different temperatures. As the SZ loading increases, the surface acidity of the mesoporous catalysts was enhanced, this was reflected by the higher catalytic activity toward cumene cracking and isopropanol dehydration.

  12. Application of as-synthesised MCM-41 and MCM-41 wrapped with reduced graphene oxide/graphene oxide in the remediation of acetaminophen and aspirin from aqueous system.

    Science.gov (United States)

    Akpotu, Samson O; Moodley, Brenda

    2018-03-01

    In this study, ASM41 (as-synthesised MCM-41), MCM-41, MCM-41 encapsulated with graphene oxide (MCM-41-GO) and reduced graphene oxide (MCM-41-G) were fabricated and utilized in the remediation of acetaminophen and aspirin from water. A surfactant template (cetyltrimethylammonium bromide) was added to ASM41 to make it more hydrophobic and its effects on the remediation of acetaminophen and aspirin from wastewater was studied. To further improve the adsorption capacity of the adsorbent, MCM-41 was encapsulated with GO and G which also aided in easy separation of the adsorbent from the aqueous solution. Comparative studies of the adsorption of acetaminophen and aspirin on all four adsorbents were investigated. Batch adsorption studies of acetaminophen and aspirin were carried out to determine the effects of pH, initial concentration, time and adsorbent dose. Adsorption mechanism was through EDA, π-π interactions, and hydrophobic effects. Data from sorption kinetics showed ASM41 had the highest q m value for aspirin (909.1 mg/g) and MCM-41-G had the highest q m value for acetaminophen (555.6 mg/g). The significant adsorption by ASM41 can be attributed to increased hydrophobicity due to the retention of the surfactant template. Thermodynamic studies revealed the adsorption process as spontaneous and exothermic. Desorption studies revealed that adsorbents could be regenerated and reused for adsorption. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Application of Mn/MCM-41 as an adsorbent to remove methyl blue from aqueous solution.

    Science.gov (United States)

    Shao, Yimin; Wang, Xi; Kang, Yuan; Shu, Yuehong; Sun, Qiangqiang; Li, Laisheng

    2014-09-01

    In this study, the application of Mn loaded MCM-41 (Mn/MCM-41) was reported as a novel adsorbent for methyl blue (MB) from aqueous solution. The mesoporous structure of Mn/MCM-41 was confirmed by XRD technique. Surface area, pore size and wall thickness were calculated from BET equation and BJH method using nitrogen sorption technique. FT-IR studies showed that Mn were loaded on the hexagonal mesoporous structures of MCM-41. It is found that the MCM-41 structure retained after loading of Mn but its surface area and pore diameter decreased due to pore blockage. Adsorption of MB from aqueous solution was investigated by Mn/MCM-41 with changing Mn content, adsorbent dosage, initial MB concentration, contact time, pH and the temperature. Under the chosen condition (25°C, 0.02 g adsorbent dosage, 6.32 pH, 50 mg L(-1) MB, 1 wt.% Mn), a high MB adsorption capacity (45.38 mg g(-1)) was achieved by Mn/MCM-41 process at 120 min, 8.6 times higher than MCM-41. The electrostatic interaction was considered to be the main mechanism for the dye adsorption. The experimental data fitted well to Freundlich and Dubinin-Radushkevich isotherms. The adsorption of MB on Mn/MCM-41 followed pseudo-second-order kinetics. Thermodynamic parameters suggested that the adsorption process is endothermic and spontaneous. Copyright © 2014 Elsevier Inc. All rights reserved.

  14. Síntese do material mesoporoso MCM-41 usando esponja de água-doce como fonte de sílica

    Directory of Open Access Journals (Sweden)

    Orivaldo da Silva Lacerda Júnior

    2013-01-01

    Full Text Available Fresh water sponge was used as a silica source for the synthesis of MCM-41 via the hydrothermal process. The silica was extracted from the sponge by washing with nitric acid and piranha solution. Synthesis of MCM-41 was performed at 100 °C for 5 days and the procedure was optimized, with modifications made to the leaching temperature of the silica and the synthesis of mesoporous material, which was characterized by XRD, FT-IR, SEM and adsorption of N2. The optimal result was achieved at a temperature of 135 °C for 3 days, showing ordered mesoporous material with a surface area of 1080 m² g-1.

  15. Design of epoxy-functionalized Fe3O4@MCM-41 core-shell nanoparticles for enzyme immobilization.

    Science.gov (United States)

    Ulu, Ahmet; Ozcan, Imren; Koytepe, Suleyman; Ates, Burhan

    2018-05-01

    The scope of our research was to prepare the organosilane-modified Fe 3 O 4 @MCM-41 core-shell magnetic nanoparticles, used for L-ASNase immobilization and explored screening of immobilization conditions such as pH, temperature, thermal stability, kinetic parameters, reusability and storage stability. In this content, Fe 3 O 4 core-shell magnetic nanoparticles were prepared via co-precipitation method and coated with MCM-41. Then, Fe 3 O 4 @MCM-41 magnetic nanoparticles were functionalized by (3-glycidyloxypropyl) trimethoxysilane (GPTMS) as an organosilane compound. Subsequently, L-ASNase was covalently immobilized on epoxy-functionalized Fe 3 O 4 @MCM-41 magnetic nanoparticles. The immobilized L-ASNase had greater activity at high pH and temperature values. It also maintained >92% of the initial activity after incubation at 55 °C for 3 h. Regarding kinetic values, immobilized L-ASNase showed a higher Vmax and lower Km compared to native L-ASNase. In addition, it displayed excellent reusability for 12 successive cycles. After 30 days of storage at 4 °C and 25 °C, immobilized L-ASNase retained 54% and 26% of its initial activities while native L-ASNase lost about 68% and 84% of its initial activity, respectively. As a result, the immobilization of L-ASNase onto magnetic nanoparticles may provide an advantage in terms of removal of L-ASNase from reaction media. Copyright © 2018. Published by Elsevier B.V.

  16. CO2 methanation on the catalyst of Ni/MCM-41 promoted with CeO2.

    Science.gov (United States)

    Wang, Xiaoliu; Zhu, Lingjun; Liu, Yincong; Wang, Shurong

    2018-06-01

    CO 2 as a raw feed combined with renewable hydrogen for the production of useful chemicals and alternative energy products is one of the solutions to environmental and energy problems. In this study, a series of Ni-xCeO 2 /MCM-41 catalysts with a nickel content of 20wt% were prepared through deposition precipitation method for CO 2 methanation. Different characterization methods, including BET, XRD, TEM, SEM, H 2 -TPR and H 2 -TPD were applied to help explore the influence mechanism of CeO 2 on Ni/MCM-41 in CO 2 methanation. It was found that all CeO 2 -promoted catalysts exhibited enhanced catalytic activity when compared to Ni/MCM-41. The catalyst modified with 20wt% CeO 2 showed the best catalytic performance, with CO 2 conversion and CH 4 selectivity of 85.6% and 99.8%, respectively, at the temperature of 380°C under atmospheric pressure. The synergetic effects among Ni 0 active sites, the promoter and the support, including nickel dispersion improvement and increased CO 2 adsorption sites due to the addition of CeO 2 , were considered as important factors for high reactivity of the promoted catalysts. The stability test showed that the promoted catalyst maintained its high reactivity after 30h. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Mechanism insight of pollutant degradation and bromate inhibition by Fe-Cu-MCM-41 catalyzed ozonation.

    Science.gov (United States)

    Chen, Weirui; Li, Xukai; Tang, Yiming; Zhou, Jialu; Wu, Dan; Wu, Yin; Li, Laisheng

    2018-03-15

    A flexible catalyst, Fe-Cu-MCM-41, was employed to enhance diclofenac (DCF) mineralization and inhibit bromate formation in catalytic ozonation process. Greater TOC removal was achieved in Fe-Cu-MCM-41/O 3 process (78%) than those in Fe-MCM-41/O 3 (65%), Cu-MCM-41/O 3 (73%) and sole ozonation (42%). But it was interesting that both Cu-MCM-41/O 3 and Fe-MCM-41/O 3 achieved 93% bromate inhibition efficiency, only 71% inhibition efficiency was observed in Fe-Cu-MCM-41/O 3 . Influence of pH, TBA/NaHSO 3 and detection of by-products were conducted to explore the mechanism. By Pyridine adsorption-IR and XPS, a relationship was found among activity of catalysts, Lewis acid sites and electron transfer effect between Fe (II/III) and Cu (I/II). Fe-Cu-MCM-41 promoted ozone decomposition to generate OH, which accounted for enhanced DCF mineralization. The consumption of aqueous O 3 also suppressed the oxidative of Br - and HBrO/Br - . More HBrO/BrO - accumulated in catalytic ozonation process and less bromate generated. Bromate formation in Fe-Cu-MCM-41/O 3 process was sensitive with pH value, the acidic condition was not favor for bromate formation. Both DCF mineralization and bromate inhibition were influenced by surface reaction. Moreover, Fe-Cu-MCM-41 showed excellent catalytic performance in suppressing the accumulation of carboxylic acid, especially for oxalic acid. Nearly no oxalic acid was detected during Fe-Cu-MCM-41/O 3 process. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. SiC-dopped MCM-41 materials with enhanced thermal and hydrothermal stabilities

    International Nuclear Information System (INIS)

    Wang, Yingyong; Jin, Guoqiang; Tong, Xili; Guo, Xiangyun

    2011-01-01

    Graphical abstract: Novel SiC-dopped MCM-41 materials were synthesized by adding silicon carbide suspension in the molecular sieve precursor solvent followed by in situ hydrothermal synthesis. The dopped materials have a wormhole-like mesoporous structure and exhibit enhanced thermal and hydrothermal stabilities. Highlights: → SiC-dopped MCM-41 was synthesized by in situ hydrothermal synthesis of molecular sieve precursor combined with SiC. → The dopped MCM-41 materials show a wormhole-like mesoporous structure. → The thermal stability of the dopped materials have an increment of almost 100 o C compared with the pure MCM-41. → The hydrothermal stability of the dopped materials is also better than that of the pure MCM-41. -- Abstract: SiC-dopped MCM-41 mesoporous materials were synthesized by the in situ hydrothermal synthesis, in which a small amount of SiC was added in the precursor solvent of molecular sieve before the hydrothermal treatment. The materials were characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, N 2 physical adsorption and thermogravimetric analysis, respectively. The results show that the thermal and hydrothermal stabilities of MCM-41 materials can be improved obviously by incorporating a small amount of SiC. The structure collapse temperature of SiC-dopped MCM-41 materials is 100 o C higher than that of pure MCM-41 according to the differential scanning calorimetry analysis. Hydrothermal treatment experiments also show that the pure MCM-41 will losses it's ordered mesoporous structure in boiling water for 24 h while the SiC-dopped MCM-41 materials still keep partial porous structure.

  19. Ibuprofen in mesopores of Mobil Crystalline Material 41 (MCM-41): a deeper understanding.

    Science.gov (United States)

    Skorupska, Ewa; Jeziorna, Agata; Paluch, Piotr; Potrzebowski, Marek J

    2014-05-05

    In this work, we compared two methods (incipient wetness and melting) for the encapsulation of ibuprofen in the pores of Mobil Crystalline Material 41 (MCM-41) through NMR (nuclear magnetic resonance) spectroscopy. (1)H NMR spectra were recorded under very fast MAS (sample spinning 60 kHz) conditions in both 1D and 2D mode (NOESY sequence). We also performed (13)C cross-polarization magic angle spinning (CP/MAS) experiments, (13)C single pulse experiments (SPE), and (1)H-(13)C HSQC HR/MAS (heteronuclear single quantum coherence high resolution) HR/MAS correlations. Evaluation of the encapsulation methods included an analysis of the filling factor of the drug into the pores. The stability of Ibu/MCM in an environment of ethanol or water vapor was tested. Our study showed that melting a mixture of Ibu and MCM is a much more efficient method of confining the drug in the pores compared to incipient wetness. The optimal experiments for the former method achieved a filling factor of approximately 60%. We concluded that the major limitation to the applicability of the incipient wetness method (filling factor ca. 20%) is the high affinity of solvent (typically ethanol) for MCM-41. We found that even ethanol vapor can remove Ibu from the pores. When a sample of Ibu/MCM was stored for a few hours in a closed vessel with ethanol vapor, Ibu was transported from the pores to the outer walls of MCM. We observed a similar phenomenon with water vapor, although this process is slower compared to the analogous procedure using ethanol. Our study clearly demonstrates that existing methods used to encapsulate drugs in mesoporous silica nanoparticles (MSNs) require reevaluation.

  20. The viability of MCM-41 as separator in secondary alkaline cells

    Science.gov (United States)

    Meskon, S. R.; Othman, R.; Ani, M. H.

    2018-01-01

    The viability of MCM-41 membrane as a separator material in secondary alkaline cell is investigated. The inorganic membrane was employed in an alkaline nickel-zinc system. MCM-41 mesoporous material consists of arrays of hexagonal nano-pore channels. The membrane was synthesized using sol-gel route from parent solution comprising of quarternary ammonium surfactant, cethyltrimethylammonium bromide C16H33(CH3)3NBr (CTAB), hydrochloric acid (HCl), deionized water (H2O), ethanol (C2H5OH), and tetraethylortosilicate (TEOS). Both the anodic zinc/zinc oxide and cathodic nickel hydroxide electrodeposited film were coated with MCM-41 membrane. The Ni/MCM-41/Zn alkaline cell was then subjected to 100-cycle durability test and the structural stability of MCM-41 separator throughout the progression of the charge-discharge cycles is studied. X-ray diffraction (XRD) analysis on the dismantled cell shows that MCM-41 began to transform to lamellar MCM-50 on the 5th cycle and transformed almost completely on the 25th cycle. The phase transformation of MCM-41 hexagonal structure into gel-like MCM-50 prevents the mesoporous cell separator from diminished in the caustic alkaline surround. This work has hence demonstrated MCM-41 membrane is viable to be employed in secondary alkaline cells.

  1. Influence of MCM-41 particle on mechanical and morphological behavior of polypropylene

    International Nuclear Information System (INIS)

    Wang Na; Shao Yawei; Shi Zhaoxin; Zhang Jing; Li Hongwei

    2008-01-01

    This study investigates the effects of different types of nanoparticles and amount of nanoparticles on morphology and mechanical performance of polypropylene (PP) composites. Three different types of nanoparticles, namely mesoporous MCM-41 (without template), mesoporous MCM-41 (with template), and mesoporous MCM-41, whose pore channels were filled with different flexible polymer inside the pore channels with the aid of supercritical CO 2 are considered. PP composites containing (0.5-5 wt.%) mesoporous MCM-41 were prepared by compounding. The tensile properties of the composites determined as a function of the filler loading and the different types of nanoparticles are found to vary with the different interface between different fillers and the matrix. The results of tensile tests showed that different flexible polymer filled mesoporous MCM-41 nanoparticles could simultaneously provide PP with strengthening and toughening effects at rather low filler content (0.5 wt.%). Scanning electron microscopy studies revealed a good dispersion of the MCM-41-S-PMMA and MCM-41-S-PS particles in the PP matrix and the enhancement of the interface between PP and MCM-41 are obtained

  2. Evaluation of the influence of sulfur-based functional groups on the embedding of silver nanoparticles into the pores of MCM-41

    International Nuclear Information System (INIS)

    Oliveira, Roselaine da S.; Camilo, Fernanda F.; Bizeto, Marcos A.

    2016-01-01

    The incorporation of noble metals in the pores of mesoporous silicas might produce materials with interesting catalytic and sensing capabilities, but the proper control of pore filling and the avoidance of nanoparticles migration to outside the pores are processes not yet completely understood. In this work, we evaluated the role of –SH and –SO_3H groups post-grafted into MCM-41 on the production of silver nanoparticles by using 1-butanol as reducing agent. Thiol groups were the most efficient on promoting the formation of nanoparticles within the pores. Conversely, sulfonic groups establish electrostatic interactions with silver cations that preclude the formation of nanoparticle in yields comparable to thiol groups. MCM-41 without functional groups did not have good affinity to silver and the nanoparticles are produced outside the pores. This study showed the importance on selecting an adequate surface functional group in order to obtain silver nanoparticles filling the pores of MCM-41. - Graphical abstract: Silver nanoparticles formation inside the pores of sulfur-groups functionalized mesoporous silica. - Highlights: • Silver nanoparticles formation inside the pores of mesoporous silica. • n-butanol as reducing agent of impregnated silver cations. • Tuning the silica surface properties by grafting sulfur-based functional groups. • Influence on the loading and distribution of the nanoparticles through the pores.

  3. Evaluation of Optimal Pore Size of (3-Aminopropyltriethoxysilane Grafted MCM-41 for Improved CO2 Adsorption

    Directory of Open Access Journals (Sweden)

    Zhilin Liu

    2015-01-01

    Full Text Available An array of new MCM-41 with substantially larger average pore diameters was synthesized through adding 1,3,5-trimethylbenzene (TMB as the swelling agent to explore the effect of pore size on final adsorbent properties. The pore expanded MCM-41 was also grafted with (3-Aminopropyltriethoxysilane (APTES to determine the optimal pore size for CO2 adsorption. The pore-expanded mesoporous MCM-41s showed relatively less structural regularity but significant increments of pore diameter (4.64 to 7.50 nm; the fraction of mesopore volume also illustrated an increase. The adsorption heat values were correlated with the order of the adsorption capacities for pore expanded MCM-41s. After amine functionalization, the adsorption capacities and heat values showed a significant increase. APTES-grafted pore-expanded MCM-41s depicted a high potential for CO2 capture regardless of the major drawback of the high energy required for regeneration.

  4. An investigation into the Ti-grafting structure on MCM-41 and epoxidation catalysis

    DEFF Research Database (Denmark)

    Yuan, Q.C.; Hagen, A.; Roessner, F.

    2006-01-01

    The structure of titanium species grafted on a purely siliceous MCM-41 and their catalysis in the epoxidation of cyclohexene with tert-butyl hydroperoxide (TBHP) were investigated. FT-IR, XANES and UV-vis were used for the examination of the Ti-grafted MCM-41. The results indicated...... that the titanium atoms are grafted on the wall surface of the MCM-41 by four-fold coordination. The four-fold coordinated titanium species are mainly grafted by two or one -O-Si-O- bridges on the MCM-41, resulting in so-called bipodal or monopodal titanium centres in partially polymerised states. The ratio...... of monopodal to bipodal titanium increases with the increase in Ti-content. These partially polymerised titanium species considered as catalytic active centres have high activity and selectivity in the epoxidation reaction. The used Ti-grafted MCM-41 samples were regenerated by heating in nitrogen or air...

  5. Enhanced photocatalytic hydrogen production from an MCM-41-immobilized photosensitizer-[Fe-Fe] hydrogenase mimic dyad.

    Science.gov (United States)

    Wang, Wen; Yu, Tianjun; Zeng, Yi; Chen, Jinping; Yang, Guoqiang; Li, Yi

    2014-11-01

    A covalently linked photosensitizer-catalytic center dyad Ps-Hy, consisting of two bis(2-phenylpyridine)(2,2'-bipyridine)iridium(iii) chromophores (Ps) and a diiron hydrogenase mimic (Hy) was constructed by using click reaction. Ps-Hy was incorporated into K(+)-exchanged molecular sieve MCM-41 to form a composite (Ps-Hy@MCM-41), which has been successfully applied to the photochemical production of hydrogen. The catalytic activity of Ps-Hy@MCM-41 is ∼3-fold higher as compared with that of Ps-Hy in the absence of MCM-41. The incorporation of Ps-Hy into MCM-41 stabilizes the catalyst, and consequently, advances the photocatalysis. The present study provides a potential strategy for improving catalytic efficiency of artificial photosynthesis systems using mesoporous molecular sieves.

  6. Removal of tetracycline from aqueous solution by MCM-41-zeolite A loaded nano zero valent iron: Synthesis, characteristic, adsorption performance and mechanism.

    Science.gov (United States)

    Guo, Yige; Huang, Wenli; Chen, Bin; Zhao, Ying; Liu, Dongfang; Sun, Yu; Gong, Bin

    2017-10-05

    In this study, nano zero valent iron (NZVI) modified MCM-41-zeolite A (Fe-MCM-41-A) composite as a novel adsorbent was prepared by precipitation method and applied for tetracycline (TC) removal from aqueous solution. The adsorbent was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and N 2 -BET analysis. Hysteresis loops indicated that the sample has a desirable magnetic property and can be separated quickly. Adsorption studies were carried out to evaluate its potential for TC removal. Results showed that the optimal Fe-MCM-41-A dosage, initial pH and reaction time at initial TC concentration of 100mgL -1 solution are 1gL -1 , pH=5, and 60 min respectively, at which the removal efficiency of TC was 98.7%. The TC adsorption results fitted the Langmuir isotherm model very well and the adsorption process could be described by a pseudo-second-order kinetic model. A maximum TC adsorption capacity of 526.32mgg -1 was achieved. This study demonstrates that Fe-MCM-41-A is a promising and efficient material for TC adsorption from aqueous solution. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Comparative studies of Zr-based MCM-41 and MCM-48 mesoporous molecular sieves: Synthesis and physicochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Chen, L.F. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: chenlf2001@yahoo.com; Zhou, X.L. [Petroleum Processing Research Center, East China University of Science and Technology, 200237 Shanghai (China); Norena, L.E. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: lnf@correo.azc.uam.mx; Wang, J.A. [Laboratorio de Catalisis y Materiales, SEPI-ESIQIE, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico); Navarrete, J. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Salas, P. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Montoya, A. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Del Angel, P. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Llanos, M.E. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico)

    2006-12-30

    Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8 m{sup 2}/g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600 deg. C, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9 m{sup 2}/g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and {sup 29}Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Broensted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Broensted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface.

  8. Comparative studies of Zr-based MCM-41 and MCM-48 mesoporous molecular sieves: Synthesis and physicochemical properties

    International Nuclear Information System (INIS)

    Chen, L.F.; Zhou, X.L.; Norena, L.E.; Wang, J.A.; Navarrete, J.; Salas, P.; Montoya, A.; Del Angel, P.; Llanos, M.E.

    2006-01-01

    Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8 m 2 /g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600 deg. C, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9 m 2 /g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and 29 Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Broensted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Broensted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface

  9. Catalytic Oxidation of Vanillyl Alcohol Using FeMCM-41 Nanoporous Tubular Reactor

    Science.gov (United States)

    Elamathi, P.; Kolli, Murali Krishna; Chandrasekar, G.

    Iron containing nanoporous MCM-41 (FeMCM-41) with different Si/Fe ratios of 50, 100 and 150 was synthesized by hydrothermal synthesis process. The materials obtained from hydrothermal synthesis were characterized by various physico chemical techniques such as XRD, N2 adsorption, DR UV-vis, EPR and FTIR spectroscopy. XRD analyses of FeMCM-41 materials confirmed the presence of well-ordered crystalline structure. N2 isotherm of FeMCM-41 materials showed type IV adsorption isotherm. EPR and DR UV-vis analysis of FeMCM-41 samples indicates the presence of high tetrahedral coordination at the Si/Fe ratios of 100 and 150. The catalytic performance of FeMCM-41 nano tubular reactor was tested in the liquid phase oxidation of vanillyl alcohol into vanillin using H2O2 (50wt% in water). The reaction products were analyzed by gas chromatography in DB-5 capillary column with flame ionization detector. The products were confirmed by 1H NMR, 13C NMR and LC-Mass spectroscopy. The maximum conversion of vanillyl alcohol (85%) and selectivity towards vanillin (82%) were observed using the catalyst FeMCM-41(100) in 30min at 60∘C. The influence of reaction temperature, reaction time, reactants molar ratio, Si/Fe ratio and amount of catalyst were investigated.

  10. Effect of template in MCM-41 on the adsorption of aniline from aqueous solution.

    Science.gov (United States)

    Yang, Xinxin; Guan, Qingxin; Li, Wei

    2011-11-01

    The effect of the surfactant template cetyltrimethylammonium bromide (CTAB) in MCM-41 on the adsorption of aniline was investigated. Various MCM-41 samples were prepared by controlling template removal using an extraction method. The samples were then used as adsorbents for the removal of aniline from aqueous solution. The results showed that the MCM-41 samples with the template partially removed (denoted as C-MCM-41) exhibited better adsorption performance than MCM-41 with the template completely removed (denoted as MCM-41). The reason for this difference may be that the C-MCM-41 samples had stronger hydrophobic properties and selectivity for aniline because of the presence of the template. The porosity and cationic sites generated by the template play an important role in the adsorption process. The optimal adsorbent with moderate template was achieved by changing the ratio of extractant; it has the potential for promising applications in the field of water pollution control. Copyright © 2011 Elsevier Ltd. All rights reserved.

  11. Synthesis of Dicyclopentadiene Oligomer Over Nanoporous Al-MCM-41 Catalysts.

    Science.gov (United States)

    Park, Eunseo; Kim, Jinhan; Yim, Jin-Heong; Han, Jeongsik; Kwon, Tae Soo; Park, Y K; Jeon, Jong-Ki

    2016-05-01

    One step reaction composed of DCPD oligomerization and DCPD oligomer isomerization was investigated over nanoporous Al-MCM-41 catalysts. The effects of aluminum grafting over MCM-41 on the catalyst characteristics were studied with respect to the synthesis of TCPD isomer. Physical and chemical properties of the catalysts were analyzed by N2 adsorption, temperature-programmed desorption of ammonia, and infrared spectroscopy of adsorbed pyridine. The overall number of acid sites as well as the number of Lewis acid sites increased with increasing of aluminum content over MCM-41. When utilizing MCM-41 and Al-MCM-41 as the catalyst, DCPD oligomerization reaction activity greatly increased compared to the thermal reaction. The highest TCPD isomer selectivity over the Al-MCM-41 catalyst with the highest aluminum content could be ascribed to the largest amount of acid sites. This study showed an increased level of TCPD isomer selectivity by an increasing level of Lewis acid sites through aluminum addition over MCM-41.

  12. CATALYTIC PROPERTIES AND ACIDITY OF MODIFIED MCM-41 ...

    African Journals Online (AJOL)

    Adsorption of pyridine and IR spectroscopy indicated various types of Lewis and Brönsted acid sites. The density distribution of acid sites was determined by TPD. Both Lewis and Brönsted acid sites were found to be active in the heptane isomerisation. The presence of aluminium (low Si/Al) combined to the ionic exchange ...

  13. CATALYTIC PROPERTIES AND ACIDITY OF MODIFIED MCM-41 ...

    African Journals Online (AJOL)

    a

    obtain H-form catalysts, samples were heated to remove the NH3 gas. Catalytic tests .... Chem. Soc. Ethiop. 2006, 20(1). 102. 0. 50. 100. 150. 200. 250. 300. 350. 400. 450. 0. 0.2 ..... Zhao, X.S.; Lu, G.Q.; Millar, G.J.; Li, X.S. Catal. Lett. 1996, 38 ...

  14. The 11C-radioisotopic study of methanol conversion on V-MCM-41; the influence of methyl iodide on the transformation

    International Nuclear Information System (INIS)

    Sarkadi-Priboczki, E.; Szelecsenyi, F.; Kovacs, Z.; Solmaz, A.; Balci, S.; Dogu, T.

    2007-01-01

    Complete text of publication follows. The MCM-41 mesoporous material has Lewis and even Bronsted acid sites to produce dimethyl ether with some hydrocarbons, while over metal modified MCM-41 mostly formaldehyde and dimethoxy methane (i.e. methylal) or methyl formate are produced. In present experiments V incorporated basically mild acid sites of MCM-41 was prepared by low temperature direct synthesis. The V-MCM-41 has enough main active Lewis sites (by V-) to form formaldehyde and also light Bronsted acid sites to let the adsorbed formaldehyde eliminate and afterwards, with methanol, to form dimethoxy methane in nonoxidative environment. This V-MCM-41 has been tested by ethanol conversion in non-oxidative environments too and diethoxy methane as main product was detected. In present work the methanol conversion, as well as the methanol co-reaction with methyl iodide are studied from the same V-MCM-41 sample using 11 C-technique. The 11 C-labelled radioactive methanol has been already applied for determination of methanol conversion rates on Cu-modified MCM-41. The V-MCM-41 was prepared by direct hydrothermal synthesis method. The adsorption rate of 11 C-methanol and, after the reaction, the desorption rate of the remaining 11 C-derivatives on catalyst were continuously detected by gamma detectors. The derivatives were analyzed by radio-gas chromatography (gas chromatograph with FID coupled on-line with a radioactivity detector). Both dimethyl ether and hydrocarbon formation are also in slight degrees according to weak Lewis and Bronsted acidities. Since the conversion was carried out without added oxygen gas, only the frame oxygen can take part into catalysis. In presence of non-radioactive methyl iodide, the radioactive methanol is converted to radioactive methyl iodide on V-MCM-41. The radio-GC analysis confirmed that the iodide induced change of the reaction performance was reversible i.e. the radioactive methyl iodide was regenerated to non-radioactive methyl

  15. Simultaneous efficient adsorption of Pb2+ and MnO4− ions by MCM-41 functionalized with amine and nitrilotriacetic acid anhydride

    International Nuclear Information System (INIS)

    Chen, Feiyun; Hong, Mingzhu; You, Weijie; Li, Chong; Yu, Yan

    2015-01-01

    Highlights: • MCM-41 was successfully modified with amine and nitrilotriacetic acid anhydride. • The adsorbent can simultaneously remove Pb 2+ and MnO 4 − by adjusting pH of the system. • The maximum adsorption capacities of Pb 2+ and MnO 4 − are 147 mg/g and 156 mg/g. • The absorbent exhibits good regeneration and reusability for 5 cycles use. - Abstract: A novel adsorbent NH 2 /MCM-41/NTAA, capable of simultaneous adsorption of cations and anions from aqueous solution, was prepared by immobilization of amine and nitrilotriacetic acid anhydride (NTAA) onto MCM-41. The structures and properties before and after surface modification were systematically investigated through X-ray diffraction (XRD), transmission electron microscope (TEM) and scanning electron microscope (SEM), nitrogen adsorption–desorption, and infrared spectroscopy (FTIR), thermogravimetry (TGA) and X-ray photoelectron spectroscopy (XPS). They together confirm that the amine and NTAA group were chemically bonded to the internal surface of the mesoporous. The NH 2 /MCM-41/NTAA were used to adsorb Pb 2+ and MnO 4 − in an aqueous solution in a batch system, and the maximum adsorption efficiency was found to occur at pH 5.0 and 3.0, respectively. NH 2 /MCM-41/NTAA exhibit preferable removal of Pb 2+ through electrostatic interactions and chelation, whereas it captures MnO 4 − by means of electrostatic interactions. The experimental data are fitted the Langmuir isotherm model reasonably well, with the maximum adsorption capacity of 147 mg/g for Pb 2+ and of 156 mg/g for MnO 4 − . The adsorption rates of both Pb 2+ and MnO 4 − are found to follow the pseudo-second order kinetics. Furthermore, the NH 2 /MCM-41/NTAA adsorbent performs good recyclability and reusability for 5 cycles use. This study indicates a potential applicability of NH 2 /MCM-41/NTAA as new absorbents for effective simultaneous adsorption of hazardous metal ions and anions from wastewater.

  16. Synthesis of cerium oxide catalysts supported on MCM-41 molecular sieve; Sintese de catalisadores de oxido de cerio suportados na peneira molecular MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Souza, E.L.S.; Barros, T.R.B.; Sousa, B.V. de, E-mail: emylle.souza@gmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia Quimica

    2016-07-01

    Porous materials have been widely studied as catalysts and catalyst support. The MCM-41 structure is the one that has been most studied because of its application possibilities in chemical processes. This work aimed to obtain and characterize cerium oxide catalysts supported on MCM-41 molecular sieve. The molecular sieve was synthesized by the conventional method with the following molar composition: 1 SiO2: 0.30 CTABr: NH3 11: 144 H2O. Then, 25% w/w cerium was incorporated into the MCM-41 using the wet impregnation process and the material obtained was activated by calcination. From the XRD patterns was confirmed the structure of the molecular sieve, and were identified the cerium oxide phases in its structure. The textural catalysts characteristics were investigated by isotherms of N2 adsorption/desorption (BET method). (author)

  17. Preparation and Humidity Sensing Properties of KCl/MCM-41 Composite

    International Nuclear Information System (INIS)

    Li, Liu; Lian-Yuan, Wang; Wei, Li; Li-Ying, Kou; Zhi-Cheng, Zhong; Li-Fang, Liu

    2010-01-01

    KCl/mobil composition of matter-41 (MCM-41) composite has been synthesized via a heat-treating process and characterized by x-ray diffraction, high resolution transmission electron microscopy, and nitrogen adsorption/desorption isotherms. In contrast with pure MCM-41, KCl/MCM-41 composite exhibits improved humidity sensing properties within the relative humidity range of 11–95%. The impedance of KCl/MCM-41 composite changes by about four orders of magnitude over the whole humidity range with the response time and the recovery times are about 30 s and 35 s, respectively. Small humidity hysteresis and good stability are also observed based on our product. These results make our product a good candidate in fabricating humidity sensors with high performances and low synthetic complexity

  18. Synthesis and catalytic performance of ZSM-5/MCM-41 composite molecular sieve from palygorskite

    Science.gov (United States)

    Jiang, Jinlong; Wu, Mei; Yang, Yong; Duanmu, Chuansong; Chen, Jing; Gu, Xu

    2017-10-01

    ZSM-5/MCM-41 composite molecular sieve has been hydrothermally synthesized through a two-step crystallization process using palygorskite (PAL) as silicon and aluminum source. The products were characterized by various means and their catalytic properties for acetalization of cyclohexanone and esterification of acetic acid and n-butanol were also investigated. In the first step ZSM-5 zeolite could be formed from the acid-treated PAL after hydrothermal treatment using tetrapropylammonium bromide as template. XRD patterns, N2 adsorption and desorption data, and TEM images show that the composite obtained in the secondary step had a well-ordered mesoporous MCM-41 phase and a microporous ZSM-5 zeolite phase. Compared with ZSM-5, ZSM-5/MCM-41 composite possessed more total acid amount, weak acid sites and large pore structure due to the formation of MCM-41 and exhibited higher catalytic activity for the acetalization and esterification reaction.

  19. Efeito do cromo nas propriedades catalíticas da MCM-41 The effect of chromium on the catalytic properties of MCM-41

    Directory of Open Access Journals (Sweden)

    Alcineia Conceição Oliveira

    2005-02-01

    Full Text Available The effect of chromium on the catalytic properties of MCM-41 was evaluated in order to develop new catalysts for the trimethylbenzene transalkylation with benzene to produce ethylbenzene, a high-value aromatic in the industry. It was found that chromium decreases the specific surface area but increases the acidity, turning MCM-41 into an active and selective catalyst for ethylbenzene and toluene production. The coke produced on the catalyst is hydrogenated and mainly located outside the pores and thus can be easily removed. The catalyst is more active and selective than mordenite, a commercial catalyst, and thus more promising for commercial applications.

  20. Functionalized bimodal mesoporous silicas as carriers for controlled aspirin delivery

    Science.gov (United States)

    Gao, Lin; Sun, Jihong; Li, Yuzhen

    2011-08-01

    The bimodal mesoporous silica modified with 3-aminopropyltriethoxysilane was performed as the aspirin carrier. The samples' structure, drug loading and release profiles were characterized with X-ray diffraction, scanning electron microscopy, N 2 adsorption and desorption, Fourier transform infrared spectroscopy, TG analysis, elemental analysis and UV-spectrophotometer. For further exploring the effects of the bimodal mesopores on the drug delivery behavior, the unimodal mesoporous material MCM-41 was also modified as the aspirin carrier. Meantime, Korsmeyer-Peppas equation ft= ktn was employed to analyze the dissolution data in details. It is indicated that the bimodal mesopores are beneficial for unrestricted drug molecules diffusing and therefore lead to a higher loading and faster releasing than that of MCM-41. The results show that the aspirin delivery properties are influenced considerably by the mesoporous matrix, whereas the large pore of bimodal mesoporous silica is the key point for the improved controlled-release properties.

  1. Efeito do cromo nas propriedades catalíticas da MCM-41

    OpenAIRE

    Oliveira,Alcineia Conceição; Rangel,Maria do Carmo; Fierro,José Luís Garcia; Reyes,Patrício; Oportus,Marcelo

    2005-01-01

    The effect of chromium on the catalytic properties of MCM-41 was evaluated in order to develop new catalysts for the trimethylbenzene transalkylation with benzene to produce ethylbenzene, a high-value aromatic in the industry. It was found that chromium decreases the specific surface area but increases the acidity, turning MCM-41 into an active and selective catalyst for ethylbenzene and toluene production. The coke produced on the catalyst is hydrogenated and mainly located outside the pores...

  2. Synthesis, Characterization and Application of the novel, regular mesoporous materials MCM-41 and MCM-48

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, R

    1995-07-01

    In the application of zeolites to catalytic cracking of heavy oil fractions the need of regular solids with large pore sizes has become very obvious. The scope of this thesis was to synthesize and characterize the novel mesoporous materials MCM-41 and MCM-48 with the major emphasis laid on MCM-41. MCM-41 materials with bulk Si/Al ratios of 4, 9, 18 and {infinity} were synthesized and characterized by XRD and HREM. The catalytic cracking behaviour of Al-containing MCM-41 materials was investigated by pulse reactor studies using decalin as model feed and by Micro Activity Tests using atmospheric residue or n-hexadecane as feed. Aluminium containing MCM-41 was found to be active for the cracking of heavy oil fractions. Purely siliceous MCM-41 materials with pore sizes ranging from 18 Aa to 40 Aa were synthesized and their properties studied by means of NMR spectroscopy. The MCM-48, which is a cubic member of the M41S family with a three dimensional pore system, was studied by means of a combination of X-ray powder diffraction and HREM technique. 210 refs., 76 figs., 9 tabs.

  3. Synthesis of Co/MCM-41catalysts and characterization by XRD, EDX, DTA/TG, SEM and TEM

    International Nuclear Information System (INIS)

    Sousa, B.V.; Rodrigues, M.G.F.

    2009-01-01

    Full text: In this work, molecular sieve MCM-41 was prepared as well as the Co/MCM-41 catalyst, via humid impregnation with concentration of 5 wt.% and 10 wt.% Co/MCM- 41. The attainment of the mesoporous molecular sieve, Si-MCM-41, was confirmed by the x-ray diffractogram. It was verified that after the calcination all the bromine (Br) was removed indicating that the calcination process removed all surfactant in the mesoporous structure. XRD and EDX analyses indicated that cobalt was found in the form of Co3O2 in the Co/MCM-41 catalysts. The diffraction standards showed that the impregnation and calcination processes caused changes in the structure only for catalyst with 10 wt.% Co/MCM-41. The DTA/TG curves showed that cobalt nitrate was totally decomposed on the MCM-41. From the images of SEM, it was possible to observe that the Co/MCM-41 catalysts were composed by clusters of small crystals. The images obtained from TEM showed clearly the presence of metal cobalt particles in a well dispersed form for catalyst with 5 wt.% Co/MCM41, except for the catalyst with 10 wt.% Co/MCM41. (author)

  4. Novedoso método para preparar materiales nanoporosos compuestos MFI/MCM-41 a partir de caolín venezolano. Efecto de la concentración de NaOH

    Directory of Open Access Journals (Sweden)

    Freddy Imbert

    2012-05-01

    Full Text Available A MFI/MCM-41 composite material, a zeolite type MFI and Al-MCM-41 were synthesized from kaolin, using TPA and CTAB as structure directing agents. The MFI/MCM-41 composite material was synthesized in two steps. In the first, MFI was obtained and then treated with solutions of different NaOH concentrations (1 – 4M, in the second step the reaction mixture was treated under MCM-41 synthesis conditions. The solids obtained were characterized by scanning electron microscopy (SEM, chemical analysis by energy dispersive X-ray spectroscopy (EDX, transmission electron microscopy (TEM, adsorption of N2 at 77K, X-ray diffraction (XRD. In the absence of alkaline treatment two phases were observed – zeolite and mesoporous, whereas the zeolite crystals were larger than mesoporous particles. The alkaline treatment dissolved the zeolite structure creating mesoporosity, modifying the characteristic zeolite morphology and reducing its crystal domains. The treatment with 2 or 3M NaOH eases zeolite dissolution and leads to assemble of the zeolite building units around the surfactant and into the mesoporous walls. The incorporation of the zeolite building units into the mesoporous walls is governed by the relative quantities of crystalline and amorphous materials in the synthesis gel. The treatment with 4M NaOH led exclusively to the formation of Al-MCM-41.

  5. 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.

  6. o-Vanillin functionalized mesoporous silica – coated magnetite nanoparticles for efficient removal of Pb(II) from water

    International Nuclear Information System (INIS)

    Culita, Daniela C.; Simonescu, Claudia Maria; Patescu, Rodica-Elena; Dragne, Mioara; Stanica, Nicolae; Oprea, Ovidiu

    2016-01-01

    o-Vanillin functionalized mesoporous silica – coated magnetite (Fe 3 O 4 @MCM-41-N-oVan) was synthesized and fully characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, N 2 adsorption–desorption technique and magnetic measurements. The capacity of Fe 3 O 4 @MCM-41-N-oVan to adsorb Pb(II) from aqueous solutions was evaluated in comparison with raw mesoporous silica – coated magnetite (Fe 3 O 4 @MCM-41) and amino – modified mesoporous silica coated magnetite (Fe 3 O 4 @MCM-41-NH 2 ). The effect of adsorption process parameters such us pH, contact time, initial Pb(II) concentration was also investigated. The adsorption data were successfully fitted with the Langmuir model, exhibiting a maximum adsorption capacity of 155.71 mg/g at pH=4.4 and T=298 K. The results revealed that the adsorption rate was very high at the beginning of the adsorption process, 80–90% of the total amount of Pb(II) being removed within the first 60 min, depending on the initial concentration. The results of the present work suggest that Fe 3 O 4 @MCM-41-N-oVan is a suitable candidate for the separation of Pb(II) from contaminated water. - Graphical abstract: A novel magnetic adsorbent based on o-vanillin functionalized mesoporous silica – coated magnetite was synthesized and fully characterized and its adsorption capacity for Pb(II) ions in aqueous solutions was evaluated. The maximum adsorption capacity for Pb(II) ions was determined to be 155.71 mg g −1 . The adsorption rate was very high at the beginning of the adsorption process, 90% of the total amount of Pb(II) being removed within the first 60 min. Display Omitted

  7. Selective Catalytic Reduction of NO with NH3 Over V-MCM-41 Catalyst.

    Science.gov (United States)

    Kwon, Woo Hyun; Park, Sung Hoon; Kim, Ji Man; Park, Su Bin; Jung, Sang-Chul; Kim, Sang Chai; Jeon, Jong-Ki; Park, Young-Kwon

    2016-02-01

    V-MCM-41, a mesoporous catalyst doped with V2O5, was applied for the first time to the removal of atmospheric NO. The quantity of V2O5 added was 10 wt% and 30 wt%. The characteristics of the synthesized catalysts were examined using XRD, N2 soprtion, and NH3-TPD. With increasing quantity of V2O5 added, specific surface area decreased and pore size increased. When the quantity of V2O5 was 10 wt%, the MCM-41 structure was retained, whereas considerable collapse of mesoporous structure was observed when 30 wt% V2O5 was added. The examination of acid characteristics using NH3-TPD showed that 30 wt% V-MCM-41 had the higher NH3 adsorption ability, implying that it would exhibit high activity for NH3 SCR reaction. In the NO removal experiments, 30 wt% V-MCM-41 showed much higher NO removal efficiency than 10 wt% V-MCM-41, which was attributed to its high NH3 adsorption ability.

  8. [Degradation of m-Cresol with Fe-MCM-41 in Catalytic Ozonation].

    Science.gov (United States)

    Sun, Wen-jing; Wang, Ya-min; Wei, Huang-zhao; Wang, Sen; Li, Xu-ning; Li, Jing-mei; Sun, Cheng-lin; An, Lu-yang

    2015-04-01

    Fe-MCM-41 was first used for the treatment of m-cresol in catalytic ozonation. The effect of the percentage of Fe dopping mass, catalyst dosage and the natural concentration of substrate on m-cresol conversion and TOC removal were studied. The structural property of Fe-MCM-41 was characterized by X-ray diffraction, temperature-programmed reduction, Mössbauer spectra and BET of catalysts. The results showed that Fe dopping mass had a great effect on the catalytic activity of Fe-MCM-41 in catalytic ozonation and the optimal percentage of dopping mass was 4.4% (wt). The results showed that with Fe dopping mass increase, the degree of crystallinity became weaker, the crystal surface distance reduced, as well as the specific surface area, pore volume and aperture. γ-Fe2O3 was the only form staying on the surface of MCM-41, and the catalyst had good ferromagnetism and stability. Ozonation played a role of both direct oxidation and indirect oxidation in the reaction, approximately the same ratio. Under the experimental condition of the natural pH of model wastewater,using 4.4% (wt) Fe-MCM-41 as catalyst, natural concentration of m-cresol 500 mg x L(-1), catalyst dosage 0.1 g x L(-1) and reaction time 30 min, m-cresol conversion and TOC removal were 100% and 26.8%, respectively.

  9. Characterization of mesoporous VOx/MCM-41 composite materials obtained via post-synthesis impregnation

    International Nuclear Information System (INIS)

    Bukallah, Saeed B.; Bumajdad, Ali; Khalil, Kamal M.S.; Zaki, Mohamed I.

    2010-01-01

    Spherical-particle MCM-41 was synthesized at room temperature, and, then, impregnated with aqueous solutions of NH 4 VO 3 to produce variously loaded VO x /MCM-41 composite materials. Bulk and surface properties of the materials thus produced were characterized by means of X-ray powder diffractometry (XRD), infrared spectroscopy (FTIR), N 2 sorptiometry and X-ray photoelectron spectroscopy (XPS). Results obtained indicated that subsequent calcination at 550 deg. C (for 2 h) of the blank and impregnated MCM-41 particles, results in materials assuming the same bulk structure of MCM-41, and exposing uniformly mesporous, high area surfaces (P w = 2.0-2.3 nm; 974-829 m 2 /g), except for the material obtained at 20 wt%-V 2 O 5 that was shown to suffer a considerable loss on surface area (down to 503 m 2 /g). XPS results implied that the immobilization of the VO x species occurs via interaction with surface OH/H 2 O groups of MCM-41, leading to the formation of vanadate (VO 3 - ) surface species, as well as minor V-O-Si and V 2 O 5 -like species. However, in all cases, the vanadium sites remained pentavalent and exposed on the surface.

  10. Structure, luminescence, and dynamics of Eu2O3 nanoparticles in MCM-41

    International Nuclear Information System (INIS)

    Chen, Wei; Joly, Alan G.; Kowalchuk, George A.; Malm, Jan-Olle; Huang, Yining; Bovin, Jan-Olov

    2001-01-01

    The structure, luminescence spectroscopy, and lifetime decay dynamics of Eu2O3 nanoparticles formed in MCM-41 have been investigated. Both X-ray diffraction and high resolution transmission electron microscope observations indicate that Eu2O3 nanoparticles of monoclinic structure are formed inside channels of MCM-41 by heating at 140 C. However, heat treatment at 600 and 700 C causes migration of Eu2O3 from the MCM-41 channels forming nanoparticles of cubic structure outside of the MCM-41 channels. The feature of the hypersensitive 5D0? 7F2 emission profile of Eu3+ is used to follow the structural changes. Photoluminescence lifetimes show the existence of short (< 1 microsecond) and long (microsecond to millisecond) components for each sample. The fast decay is attributed to quenching by surface states of the nanoparticles or energy transfer to the MCM-41 while the longer time decays show the effects of concentration quenching. The monoclinic sample prepared at 140 C shows a higher luminescence intensity than the cubic samples or the bulk powder

  11. Synthesis of cerium oxide catalysts supported on MCM-41 molecular sieve

    International Nuclear Information System (INIS)

    Souza, E.L.S.; Barros, T.R.B.; Sousa, B.V. de

    2016-01-01

    Porous materials have been widely studied as catalysts and catalyst support. The MCM-41 structure is the one that has been most studied because of its application possibilities in chemical processes. This work aimed to obtain and characterize cerium oxide catalysts supported on MCM-41 molecular sieve. The molecular sieve was synthesized by the conventional method with the following molar composition: 1 SiO2: 0.30 CTABr: NH3 11: 144 H2O. Then, 25% w/w cerium was incorporated into the MCM-41 using the wet impregnation process and the material obtained was activated by calcination. From the XRD patterns was confirmed the structure of the molecular sieve, and were identified the cerium oxide phases in its structure. The textural catalysts characteristics were investigated by isotherms of N2 adsorption/desorption (BET method). (author)

  12. Effect of Co Mo/HSO3-functionalized MCM-41 over heavy oil

    International Nuclear Information System (INIS)

    Schacht, P.; Ramirez G, M.; Ramirez, S.; Aguilar P, J.; Norena F, L.; Abu, I.

    2010-01-01

    The potential of Co-Mo metals supported on functionalized MCM-41 as catalyst to hydrodesulfurization of heavy oil has been explored in this work. The MCM-41 functionalized sample was synthesized according to method previously reported into the support by simultaneous impregnation. The catalyst was characterized by specific surface area and X-ray diffraction. The pore channel of MCM-41 was confirmed by transmission electronic microscopy and infra red spectroscopy. Catalytic activity tests were carried out using heavy oil from Gulf of Mexico. The API gravity was increased from 12.5 to 20.2, the kinematics viscosity was decreased from 18,700 to 110 c St at 298 K, the contents of asphaltene and sulfur were also reduced. (Author)

  13. Effect of Co Mo/HSO{sub 3}-functionalized MCM-41 over heavy oil

    Energy Technology Data Exchange (ETDEWEB)

    Schacht, P.; Ramirez G, M.; Ramirez, S. [Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas No. 152, 07730 Mexico D. F. (Mexico); Aguilar P, J.; Norena F, L. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Av. San Pablo No. 180, 02200 Mexico D. F. (Mexico); Abu, I., E-mail: pschacha@imp.m [University of Calgary, Department of Chemical and Petroleum Engineering, 2500 University Drive NW, Calgary, Alberta T2N 1N4 (Canada)

    2010-07-01

    The potential of Co-Mo metals supported on functionalized MCM-41 as catalyst to hydrodesulfurization of heavy oil has been explored in this work. The MCM-41 functionalized sample was synthesized according to method previously reported into the support by simultaneous impregnation. The catalyst was characterized by specific surface area and X-ray diffraction. The pore channel of MCM-41 was confirmed by transmission electronic microscopy and infra red spectroscopy. Catalytic activity tests were carried out using heavy oil from Gulf of Mexico. The API gravity was increased from 12.5 to 20.2, the kinematics viscosity was decreased from 18,700 to 110 c St at 298 K, the contents of asphaltene and sulfur were also reduced. (Author)

  14. Synthesis, characterization and catalytic activity toward methanol oxidation of electrocatalyst Pt4+-NH2-MCM-41

    International Nuclear Information System (INIS)

    Zheng Huajun; Chen Zuo; Wang Limin; Ma Chun’an

    2012-01-01

    Highlights: ► It was first confirmed that the Pt 4+ exhibited a good electro-catalytic property for methanol oxidation. ► The Pt 4+ perfectly distributed on a mesoporous molecular sieve matrix synthesis by a facile method. ► The good performance of catalyst resistance to poisoning because of a homogeneous distribution of Pt 4+ and large specific surface area. - Abstract: Mesoporous material with functional group (Pt 4+ -NH 2 -MCM-41) was prepared by grafting aminopropyl group and adsorbing platinum ions on the surface of the commercial molecular sieve (MCM-41). The characterization carried out by X-ray photoelectron spectroscopy, X-ray diffraction, and N 2 adsorption–desorption measurement pointed out that Pt was adsorbed on the NH 2 -MCM-41 surface as the oxidation state (Pt 4+ ) and the surface area of Pt 4+ -NH 2 -MCM-41 was up to 564 m 2 /g. Transmission electron microscopy and elemental mapping indicated a homogeneous distribution of Pt 4+ throughout all surface of the mesoporous materials. Electro-catalytic properties of methanol oxidation on the Pt 4+ -NH 2 -MCM-41 electrode were investigated with electrochemical methods. The results showed that the Pt 4+ -NH 2 -MCM-41 electrode exhibited catalytic activity in the methanol electro-oxidation with the apparent activation energy being 49.29 kJ/mol, and the control step of methanol electro-oxidation was the mass transfer process. It is first proved that platinum ions had good electro-catalytic property for methanol oxidation and provided a new idea for developing electrode materials in future.

  15. Preparation and controlled release of mesoporous MCM-41/propranolol hydrochloride composite drug.

    Science.gov (United States)

    Zhai, Qing-Zhou

    2013-01-01

    This article used MCM-41 as a carrier for the assembly of propranolol hydrochloride by the impregnation method. By means of chemical analysis, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy and low-temperature N(2) adsorption-desorption at 77 K, the characterization was made for the prepared materials. The propranolol hydrochloride guest assembly capacity was 316.20 ± 0.31 mg/g (drug/MCM-41). Powder XRD test results indicated that during the process of incorporation, the frameworks of the MCM-41 were not destroyed and the crystalline degrees of the host-guest nanocomposite materials prepared still remained highly ordered. Characterization by SEM and TEM showed that the composite material presented spherical particle and the average particle size of composite material was 186 nm. FT-IR spectra showed that the MCM-41 framework existed well in the (MCM-41)-propranolol hydrochloride composite. Low-temperature nitrogen adsorption-desorption results at 77 K showed that the guest partially occupied the channels of the molecular sieves. Results of the release of the prepared composite drug in simulated body fluid indicated that the drug can release up to 32 h and its maximum released amount was 99.20 ± 0.11%. In the simulated gastric juice release pattern of drug, the maximum time for the drug release was discovered to be 6 h and the maximum cumulative released amount of propranolol hydrochloride was 45.13 ± 0.23%. The drug sustained-release time was 10 h in simulated intestinal fluid and the maximum cumulative released amount was 62.05 ± 0.13%. The prepared MCM-41 is a well-controlled drug delivery carrier.

  16. Synthesis and characterization of Co-Fe Prussian blue nanoparticles within MCM-41

    International Nuclear Information System (INIS)

    Vien Vo; Nguyen Van Minh; Lee, Hyung Ik; Kim, Ji Man; Kim, Youngmee; Kim, Sung Jin

    2009-01-01

    A Prussian blue analogue, K 0.84 Co 1.08 [Fe(CN) 6 ] is prepared by reaction between [Fe(CN) 6 ] 3- in aqueous solution and ion-exchanged Co 2+ in the channels of MCM-41. Powder X-ray diffraction, transmission electron microscopy, thermogravimetric analysis, nitrogen adsorption/desorption isotherms, diffuse reflectance UV-vis absorption spectroscopy and magnetic measurements were employed to characterize the product. The results show that the Prussian blue analogue is in nanoparticles within the channels and the hexagonal phase of MCM-41 remains intact during the reactions. A particle size effect on optical and magnetic properties of the nanoparticles was observed

  17. Preparation and spectroscopic studies of PbS/nanoMCM-41 nanocomposite

    Directory of Open Access Journals (Sweden)

    A. Pourahmad

    2014-11-01

    Full Text Available The present work describes the preparation and characterization of nanosized PbS particles inside the mesopore channels of nanoMCM-41 silicate molecular sieves. The encapsulation of the lead sulfide was carried out at room temperature by ion-exchange method. Diffuse reflectance ultraviolet–visible spectroscopic studies showed a significant shift in the absorption band for the entrapped metal sulfide as compared to corresponding bulk sulfide. Thus, confirming the quantum confinement of the incorporated nanoparticles in nanoMCM-41.

  18. Influence of incorporation method of sulfated zirconia in MCM-41 molecular sieve; Influencia do metodo de incorporacao da zirconia sulfatada na peneira molecular MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, C.E.; Santos, J.S.B.; Cavalcante, J.N.A.; Andrade, M.R.A.; Sousa, B.V., E-mail: eduardopereira.eq@gmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Centro de Ciencia e Tecnologia

    2016-07-01

    Sulfated metal oxides and sulfated zirconia have attracted great attention in recent years due to its high catalytic activity. The sulfated zirconia has the function of assigning the acidic material, through the formation of Bronsted acids and Lewis sites. The incorporation of sulfated zirconia in MCM-41 molecular sieve was carried out through the techniques: dry and wet. The wet process involves the use of an excess of solution on the volume of the support pores. Therefore, the concentration of the metal precursor on the support depends on the solution concentration and the pore volume of the support. In the process of incorporating by dry, the volume of the solution containing the precursor does not exceed the pore volume of the support. After either procedure, the impregnated support must be dried in order to allow the precursor compound can be converted into a catalytically active phase. This study aims to evaluate two methods of incorporation of sulfated zirconia in the mesoporous molecular sieve MCM-41. The process of merger took for wet and dry impregnation. Through the XRD patterns it was possible to identify the presence of the hexagonal structure of the molecular sieve, as well as the tetragonal and monoclinic phases of zirconia. From the spectroscopic analysis in the infrared region to the method the wet, it was possible to identify the vibrational frequencies related to the merger of sulfated zirconia in the MCM-41 structure of the molecular sieve. (author)

  19. MCM-41介孔碳材料的合成及其电化学性能%Synthesis of MCM-41 Mesoporous Carbon Materials and Their Electrochemical Performance

    Institute of Scientific and Technical Information of China (English)

    宋伟明; 徐立洋; 孙立; 邓启刚; 冯建; 程晓宇

    2017-01-01

    以十六烷基三甲基溴化铵(CTAB)为模板剂,可溶性淀粉(Starch)为碳源,通过软模板法一步合成了高度有序的介孔碳材料.通过热重分析(TG)、X射线衍射(XRD)、N2吸附-脱附和透射电子显微镜(TEM)对材料的结构进行了表征.结果表明:当m(模板剂CTAB)∶m(可溶性淀粉)=1.0∶1.5,650℃焙烧碳化3h,并用氢氟酸去除二氧化硅后,所得到的MCM-41有序介孔碳材料(OMC-650)的比表面积为985 m2/g,平均孔径为2.5nm,且孔径分布均匀.XRD和FEM分析结果表明,OMC-650具有典型的MCM-41结构特征,有序性良好.以OMC-650作为工作电极,氧化汞为参比电极,铂为辅助电极,用6 mol/L KOH做电解液,测其比电容为150 F/g,且经过1 000次充放电循环后,其比电容仍为138 F/g,为原电容的92%,说明所合成的材料具有良好的电容稳定性.%A highly ordered mesoporous carbon material was synthesized by a soft template method with hexadecyltrimethylammonium bromide (CTAB) as a template and soluble starch (Starch) as a carbon source.The structures of the resultant materials were characterized by thermal gravimetric analysis (TG),X-ray diffraction (XRD),N2 adsorption-desorption isotherms and transmission electron microscopy (TEM).The results showed that MCM-41 ordered mesoporous carbon material (OMC-650) was obtained when the mass ratio of CTAB to Starch was 1.0∶1.5,carbonized for 3 h at 650 ℃,and then removing the silica with hydrofluoric acid.OMC-650 possessed specific surface area of 985 m2/g and average pore diameter of 2.5 nm and exhibited a uniform distribution.XRD and TEM analysis showed that OMC-650 possesses a typical MCM-41 structural feature with high ordered structure.The electrochemical tests were conducted in a three-electrode system in 6 mol/L KOH solution.When OMC-650 was used as a working electrode,mercury oxide electrode was used as a reference electrode,and Pt wire electrode served as an auxiliary electrode.The specific capacitance of

  20. Selective catalytic reduction of NOx in lean-burn engine exhaust over a Pt/V/MCM-41 catalyst

    International Nuclear Information System (INIS)

    Jeon, Jong Yeol; Kim, Hee Young; Woo, Seong Ihl

    2003-01-01

    The activities of Pt supported on various metal-substituted MCM-41 (V-, Ti-, Fe-, Al-, Ga-, La-, Co-, Mo-, Ce-, and Zr-MCM-41) and V-impregnated MCM-41 were investigated for the reduction of NO by C 3 H 6 . Among these catalysts, Pt supported on V-impregnated MCM-41 showed the best activity. The maximum conversion of NO into N 2 +N 2 O over this Pt/V/MCM-41 catalyst (Pt=1wt.%, V=3.8wt.%) was 73%, and this maximum conversion was sustained over a temperature range of 70C from 270 to 340C. The high activity of Pt/V/MCM-41 over a broad temperature range resulted from two additional reactions besides the reaction occurring on usual supported Pt, the reaction of NO with surface carbonaceous materials, and the reaction of NO occurring on support V-impregnated MCM-41. The former additional reaction showed an oscillation characteristic, a phenomenon in which the concentrations of parts of reactant and product gases oscillate continuously. At low temperature, some water vapor injected into the reactant gas mixture promoted the reaction occurring on usual supported Pt, whereas at high temperature, it suppressed the additional reaction related to carbonaceous materials. Five-hundred parts per million of SO 2 added to the reactant gas mixture only slightly decreased the NO conversion of Pt/V/MCM-41

  1. Enhancement in visible light photocatalytic activity by embedding Cu nanoparticles over CuS/MCM-41 nanocomposite

    Science.gov (United States)

    Sohrabnezhad, Sh.; Karamzadeh, M.

    2017-07-01

    This article indicate the biogenic synthesis of copper nanoparticles (Cu NPs) using the borage flowers extract of Borago officinalis over CuS/MCM-41 nanocomposite (NC). No external reducing was utilized in the developed method. The CuS-MCM-41 NC was used as stabilizing agent. The synthesis of CuS nanostructure in MCM-41 material has been realized by hydrothermal method. Their physiochemical properties have been characterized by X-ray diffraction, transmission electron microscopy (TEM), UV-Visible diffuse reflectance spectroscopy, and Fourier transform infrared spectroscopy. On the basis of TEM images, a layer of Cu NPs has been located over CuS/MCM-41 NC with average diameter of 60-80 nm. The results revealed the spherical nature of the prepared Cu NPs with diameter less than 10 nm. The DR spectra of Cu NPs in MCM-41 and CuS-MCM-41 NCs showed surface plasmon resonance bands at 570 and 500-600 nm, respectively. The photocatalytic activity was evaluated under visible light irradiation using the photocatalytic degradation of methylene blue (MB) as a model reaction. The prepared Cu/CuS/MCM-41 nanocomposite microspheres showed higher photodegradation ability for MB than CuS/MCM-41. The degradation of MB achieved up to 80% after 60 min and the nanocomposite could be recycled and reused.

  2. Efficient Hydrogenolysis of Guaiacol over Highly Dispersed Ni/MCM-41 Catalyst Combined with HZSM-5

    Directory of Open Access Journals (Sweden)

    Songbai Qiu

    2016-09-01

    Full Text Available A series of MCM-41 supported Ni catalysts with high metal dispersion was successfully synthesized by simple co-impregnation using proper ethylene glycol (EG. The acquired Ni-based catalysts performed the outstanding hydrogenolysis activity of guaiacol. The effects of the synthesis parameters including drying temperature, calcination temperature, and metal loading on the physical properties of NiO nanoparticles were investigated through the use of X-ray diffraction (XRD. The drying temperature was found to significantly influence the particle sizes of NiO supported on MCM-41, but the calcination temperature and metal loading had less influence. Interestingly, the small particle size (≤3.3 nm and the high dispersion of NiO particles were also obtained for co-impregnation on the mixed support (MCM-41:HZSM-5 = 1:1, similar to that on the single MCM-41 support, leading to excellent hydrogenation activity at low temperature. The guaiacol conversion could reach 97.9% at 150 °C, and the catalytic activity was comparative with that of noble metal catalysts. The hydrodeoxygenation (HDO performance was also promoted by the introduction of acidic HZSM-5 zeolite and an 84.1% yield of cyclohexane at 240 °C was achieved. These findings demonstrate potential applications for the future in promoting and improving industrial catalyst performance.

  3. On the hydrothermal stability of MCM-41. Evidence of capillary tension-induced effects

    NARCIS (Netherlands)

    Perez, Lidia Lopez; van Eck, Ernst R. H.; Melian-Cabrera, Ignacio

    2016-01-01

    MCM-41's limited hydrothermal stability has been often related to the hydrolysis of Si-O-Si bonds due to the low degree of condensation, its thin walls or a combination of them. In this work, evidence for an additional factor is provided; a physical effect that occurs during the drying of the

  4. FACTORES QUE AFECTAN LA TEXTURA Y ESTRUCTURA DE Ti(R-MCM-41 FACTORES QUE AFECTAN LA TEXTURA Y ESTRUCTURA DE Ti(R-MCM-41

    Directory of Open Access Journals (Sweden)

    J. Ramírez Solís

    2012-02-01

    Full Text Available Se ha estudiado el efecto que tienen el método de remoción del surfactante y el contenido de titanio sobre la estructura y propiedades texturales de los materiales mesoporosos Ti-MCM-41. Los sólidos sintetizados fueron caracterizados por fisisorción de N2, fluorescencia de rayos X (FRX, difracción de rayos X (DRX, microscopía electrónica de alta resolución (HREM, espectroscopía FT-Raman y de reflectancia difusa UV-vis. (DRS. Entre los dos métodos de remoción del surfactante estudiados, la aplicación de un disolvente polar (solución de H2SO4 0.05 M en etanol resultó ser más efectivo para remover el surfactante y disminuir la destrucción del material mesoporoso durante la calcinación. Las muestras tratadas con este método presentaron un mayor orden en el arreglo hexagonal de los poros (HREM, DRX y áreas superficiales más grandes. El efecto del aumento del contenido de TiO2 en los sólidos sintetizados se traduce en una disminución significativa de la intensidad del pico característico de MCM-41 (2Q = 2.2-2.5o y de las características texturales (SBET, volumen de poros, lo que indica que durante la síntesis no es posible incorporar más de 10 mol. % de TiO2 al MCM-41.Studied was the effect surfactant removal and titanium content have on the structure and textural properties of Ti-MCM-41 mesoporous materials. The synthesized solids were characterized by N2 adsorption, X-ray fluorescence (FRX, X-ray diffraction (DRX, electronic microscopy of high resolution(HREM, and FT-Raman and UV-vis diffuse reflectance spectroscopy (DRS. Between the two methods of surfactant removal studied, the application of a polar solvent (solution of 0.05 M H2SO4 in ethanol was to be more effective in removing the surfactant and diminishing the destruction of mesoporous material during calcination. The samples treated by this method showed a more ordered hexagonal pore arrangement (HREM, XRD and larger surface area. The effect of an increase in TiO2

  5. Catalytic steam reforming of tar derived from steam gasification of sunflower stalk over ethylene glycol assisting prepared Ni/MCM-41

    International Nuclear Information System (INIS)

    Karnjanakom, Surachai; Guan, Guoqing; Asep, Bayu; Du, Xiao; Hao, Xiaogang; Samart, Chanatip; Abudula, Abuliti

    2015-01-01

    Highlights: • Ni/MCM-41 was prepared by EG-assisted co-impregnation method. • EG-assisted co-impregnation method resulted in Ni particles well dispersed on MCM-41. • Ni/MCM-41-EG catalyst had high catalytic activity for tar reforming. • The highest H 2 gas yield was obtained when using 20 wt.% Ni/MCM-41-EG. • The catalysts were reused up to 5 cycles without any serious deactivation. - Abstract: Ethylene glycol (EG) assisted impregnation of nickel catalyst on MCM-41 (Ni/MCM-41-EG) was performed and applied for steam reforming of tar derived from biomass. The catalyst was characterized by SEM–EDX, BET, XRD, and TPR. It is found that smaller nickel particles were well dispersed on MCM-41 and better catalytic activity was shown for the Ni/MCM-41-EG when compared with the catalyst of Ni/MCM-41 prepared by using the conventional impregnation method. H 2 yield increased approximately 8% when using 20 wt.% Ni/MCM-41-EG instead of 20 wt.% Ni/MCM-41 for the steam reforming of tar derived from sunflower stalk. The catalyst reusability was also tested up to five cycles, and no obvious activity reduction was observed. It indicates that EG assisted impregnation method is a good way to prepare metal loaded porous catalyst with high catalytic activity, high loading amount and long-term stability for the tar reforming

  6. Prospects of Fe/MCM-41 as a Catalyst for Hydrocarbon Synthesis

    International Nuclear Information System (INIS)

    Cagnoli, Maria V.; Gallegos, Norma G.; Bengoa, Jose F.; Alvarez, Ana M.; Marchetti, Sergio G.; Moreno, Sergio M. J.; Roig, Anna; Mercader, Roberto C.

    2005-01-01

    We report the synthesis of cylindrical nanoparticles of metallic Fe entirely included in MCM-41 pores. Their dimensions are approx.3 nm diameter and approx. 3.8 nm length. We show that a coherent analysis of the results yielded by the various techniques is essential to obtain a catalyst supported on an MCM-41 matrix of ≅ 3 nm average pore diameter, which is active and selective toward olefins. The solids were characterized by low-angle x-ray diffraction, high-resolution transmission electron microscopy, high-resolution scanning transmission electron microscopy equipped with a high-angle annular dark-field, CO chemisorption, volumetric oxidation, and Moessbauer spectroscopy (in controlled atmosphere for the reduced catalysts). Catalytic results in the Fischer-Tropsch synthesis, as well as some unexpected results --like the inhomogeneous pore filling and discontinuous Fe particles-- are also discussed

  7. Coordination and Oxidation States of Iron Incorporated in Mesoporous MCM41

    International Nuclear Information System (INIS)

    Lazar, K.; Pal-Borbely, G.; Szegedi, A.; Beyer, H. K.

    2002-01-01

    Mesoporous Fe-MCM41 samples (Si/Fe=25) were synthesized and characterized under evacuation and reducing/oxidizing treatments by in situ FTIR and Moessbauer spectroscopies. Both Fe(II) and Fe(III) located in low coordination states in top layers of pore walls exhibit Lewis acidity and may participate in Fe(III) ↔ Fe(II) processes at low temperatures (570 K). Furthermore, Fe(III) ↔ Fe(II) cycles can be achieved and repeated with participation of the full amount of iron at higher temperatures (670 K). The accompanying formation of oxygen vacancies and restoration of the structure in the reverse process does not result in extended damages; the MCM41 structure retains its stability under the conditions applied.

  8. Photocatalytic degradation of tetracycline by Ti-MCM-41 prepared at room temperature and biotoxicity of degradation products

    Science.gov (United States)

    Zhou, Kefu; Xie, Xiao-Dan; Chang, Chang-Tang

    2017-09-01

    Ti-doped MCM-41 with different Si/Ti molar ratios was prepared at room temperature to degrade tetracycline antibiotics in aqueous solution. The Ti was doped into the skeleton structure of MCM-41. The photocatalytic activity of Ti-doped MCM-41 was investigated. The optimal catalyst had Si/Ti molar ratio of 25 and over 99% removal of oxytetracycline in 150 min, and the removal could maintain 98% after 5 reuses. Ions and soluble organic matters in natural water affected the degradation reaction when Ti-doped MCM-41 was used to treat simulated wastewater of chicken farms. The degradation products of oxytetracycline, tetracycline and chlortetracycline were detected by Escherichia coli DH5α and HPLC-MS/MS. No intermediate product with higher toxicity was detected.

  9. Synthesis and characterization of V, Mo and Nb incorporated micro-mesoporous MCM-41 materials

    Energy Technology Data Exchange (ETDEWEB)

    Solmaz, Arzu, E-mail: arzu.solmaz@rshm.gov.tr [Gazi University, Faculty of Engineering, Chemical Engineering Department, 06570 Ankara (Turkey); Balci, Suna, E-mail: sunabalci@gazi.edu.tr [Gazi University, Faculty of Engineering, Chemical Engineering Department, 06570 Ankara (Turkey); Dogu, Timur, E-mail: tdogu@metu.edu.tr [Middle East Technical University, Faculty of Engineering, Chemical Engineering Department, 06531 Ankara (Turkey)

    2011-01-01

    Highly microporous metal-MCM-41 ordered mesoporous structure catalysts having different metal/Si (V, Mo, Nb) atomic ratios and combinations of metal sources were hydrothermally synthesized. The structural properties estimated using different techniques were found to be in agreement with each other. Metals were successfully incorporated into MCM-41 without deteriorating the ordered hexagonal structure. The metal ions in the synthesis solutions probably settled on the hydrophilic end of the template hence the metal incorporation resulted improvements in the micropore structure. Low loading of metals caused an increase in the surface area and pore volume values of the catalysts. The highest total (1310 m{sup 2} g{sup -1}) and micropore surface area values (1083 m{sup 2} g{sup -1}) were obtained by Nb incorporation. The micro- and mesopore dimensions of MCM-41 increased from 0.5 to 1.1 nm and from 2.5 to 2.8 nm, respectively, with metal incorporation. Low V/Si ratios and presence of Nb in the starting solution enhanced narrow mesopore size distribution. The pore dimension and wall thickness values estimated from nitrogen adsorption and X-ray diffraction methods were consistent with the corresponding values obtained using transmission electron microscopy.

  10. Sulphonated cobalt phthalocyanine-MCM-41: An active photocatalyst for degradation of 2,4-dichlorophenol

    Energy Technology Data Exchange (ETDEWEB)

    Zanjanchi, M.A., E-mail: zanjanchi@guilan.ac.ir [Department of Chemistry, Faculty of Science, University of Guilan, P.O. Box 1914, Namjoo St., Rasht 41335 (Iran, Islamic Republic of); Ebrahimian, A.; Arvand, M. [Department of Chemistry, Faculty of Science, University of Guilan, P.O. Box 1914, Namjoo St., Rasht 41335 (Iran, Islamic Republic of)

    2010-03-15

    The photocatalytic activity of sulphonated cobalt phthalocyanine immobilized onto MCM-41 was investigated for decomposition of 2,4-dichlorophenol (2,4-DCP) in aqueous solutions. Immobilization of anion sulpho-cobalt phthalocyanine to the walls of MCM-41 was performed by pre-anchorage of 3-(aminopropyl)-triethoxysilane (APTES) onto MCM-41 via post-synthesis method. X-ray diffraction, nitrogen physisorption, diffuse reflectance spectroscopy, energy-dispersive X-ray and FT-IR methods were used to characterize the product. Photocatalytic efficiency of the prepared catalyst for degradation of 2,4-DCP was tested under illumination of UV-A and visible light. The results obtained reveal that the photocatalyst is very active in degradation of 2,4-DCP. The photodegradation process is completed within 3 h using a dose of 0.6 g/L of the catalyst under UV irradiation. The reactions follow a pseudo-first-order kinetics and the observed rate constant values change with 2,4-DCP concentrations. The reproducibility of the catalyst was tested. The reaction intermediates were identified by gas chromatoghraphy-mass spectrometery (GC-MS) technique.

  11. Influence of incorporation method of sulfated zirconia in MCM-41 molecular sieve

    International Nuclear Information System (INIS)

    Pereira, C.E.; Santos, J.S.B.; Cavalcante, J.N.A.; Andrade, M.R.A.; Sousa, B.V.

    2016-01-01

    Sulfated metal oxides and sulfated zirconia have attracted great attention in recent years due to its high catalytic activity. The sulfated zirconia has the function of assigning the acidic material, through the formation of Bronsted acids and Lewis sites. The incorporation of sulfated zirconia in MCM-41 molecular sieve was carried out through the techniques: dry and wet. The wet process involves the use of an excess of solution on the volume of the support pores. Therefore, the concentration of the metal precursor on the support depends on the solution concentration and the pore volume of the support. In the process of incorporating by dry, the volume of the solution containing the precursor does not exceed the pore volume of the support. After either procedure, the impregnated support must be dried in order to allow the precursor compound can be converted into a catalytically active phase. This study aims to evaluate two methods of incorporation of sulfated zirconia in the mesoporous molecular sieve MCM-41. The process of merger took for wet and dry impregnation. Through the XRD patterns it was possible to identify the presence of the hexagonal structure of the molecular sieve, as well as the tetragonal and monoclinic phases of zirconia. From the spectroscopic analysis in the infrared region to the method the wet, it was possible to identify the vibrational frequencies related to the merger of sulfated zirconia in the MCM-41 structure of the molecular sieve. (author)

  12. Experimental study of polyethylene pyrolysis and combustion over HZSM-5, HUSY, and MCM-41.

    Science.gov (United States)

    Huang, Que; Liu, Changcheng; Wei, Ruichao; Wang, Jian

    2017-07-05

    The effects of temperatures, catalysts, and catalyst contents on polyethylene (PE) pyrolysis were investigated by using single-photon ionization time-of-flight mass spectrometry (SPI-TOFMS). The mass spectra of pyrolyzed PE and PE/catalysts from 300°C to 800°C illustrate that the pyrolysis reactions were apparently promoted and varied by introducing HZSM-5, HUSY, and MCM-41. As microporous catalysts, HZSM-5 and HUSY were found to accelerate the BTX formation at 400°C, which could not be observed for pure PE until 800°C. With the existence of MCM-41, only alkenes were produced below 600°C. The pyrolysis processes could to be accelerated by adding catalysts. Principal components analysis (PCA) was finally employed to identify the main factors with influence on the products distribution. Analytical results showed that the yield of the majority of products could be affected by different experimental conditions, that the type of catalysts makes the most significant influence. The impact of different types of catalysts on fire hazard of PE was studied by using the cone calorimeter. The results indicated that the time to ignition (TTI) and the peak heat release rate (pHRR) were changed remarkably. It is worth noting that with the addition of MCM-41, the pHRR is the minimum. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Enhancement of Glycerol Steam Reforming Activity and Thermal Stability by Incorporating CeO2 and TiO2 in Ni- and Co-MCM-41 Catalysts

    Science.gov (United States)

    Dade, William N.

    Hydrogen (H2) has many applications in industry with current focus shifted to production of hydrocarbon fuels and valuable oxygenates using the Fischer-Tropsch technology and direct use in proton exchange membrane fuel cell (PEMFC). Hydrogen is generally produced via steam reforming of natural gas or alcohols like methanol and ethanol. Glycerol, a by-product of biodiesel production process, is currently considered to be one of the most attractive sources of sustainable H2 due to its high H/C ratio and bio-based origin. Ni and Co based catalysts have been reported to be active in glycerol steam reforming (GSR); however, deactivation of the catalysts by carbon deposition and sintering under GSR operating conditions is a major challenge. In this study, a series of catalysts containing Ni and Co nanoparticles incorporated in CeO2 and TiO2 modified high surface area MCM-41 have been synthesized using one-pot method. The catalysts are tested for GSR (at H2O/Glycerol mole ratio of 12 and GHSV of 2200 h-1) to study the effect of support modification and reaction temperature (450 - 700 °C) on the product selectivity and long term stability. GSR results revealed that all the catalysts performed significantly well exhibiting over 85% glycerol conversion at 650 °C except Ni catalysts that showed better low temperature activities. Deactivation studies of the catalysts conducted at 650 °C indicated that the Ni-TiO2-MCM-41 and Ni-CeO 2-MCM-41 were resistant to deactivation with ˜100% glycerol conversion for 40 h. In contrast, Co-TiO2-MCM-41 perform poorly as the catalyst rapidly deactivated after 12 h to yield ˜20% glycerol conversion after 40 h. The WAXRD and TGA-DSC analyses of spent catalysts showed a significant amount of coke deposition that might explain catalysts deactivation. The flattening shape of the original BET type IV isotherm with drastic reduction of catalyst surface area can also be responsible for observed drop in catalysts activities.

  14. Drug delivery from hydrophobic-modified mesoporous silicas: Control via modification level and site-selective modification

    International Nuclear Information System (INIS)

    Tang Qunli; Chen Yuxi; Chen Jianghua; Li Jin; Xu Yao; Wu Dong; Sun Yuhan

    2010-01-01

    Dimethylsilyl (DMS) modified mesoporous silicas were successfully prepared via co-condensation and post-grafting modification methods. The post-grafting modification was carried out by the reaction of the as-synthesized MCM-41 material (before CTAB removal) with diethoxydimethylsinale (DEDMS). N 2 adsorption-desorption and 29 Si MAS NMR characterization demonstrated that different amount of DMS groups were successfully incorporated into the co-condensation modified samples, and the functional DMS groups were placed selectively on the pore openings and external pore surfaces in the post-grafting modified samples. Subsequently, the controlled drug delivery properties from the resulting DMS-modified mesoporous silicas were investigated in detail. The drug adsorption experiments showed that the adsorption capacities were mainly depended on the content of silanol group (CSG) in the corresponding carriers. The in vitro tests exhibited that the incorporation of DMS groups greatly retarded the ibuprofen release rate. Moreover, the ibuprofen release profiles could be well modulated by varying DMS modification levels and site-selective distribution of functional groups in mesoporous carriers. - The distribution of DMS groups on the pore surfaces of the mesostructures strongly affects the drug release rate. The P-M41-1 and the P-M41-2 possess the close DMS modification levels as the C-M41-10, but the ibuprofen release rates from the P-M41-1 and P-M41-2 are much slower than that from the C-M41-10.

  15. AND logic-like pH- and light-dual controlled drug delivery by surface modified mesoporous silica nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Junwei; He, Zhaoshuai; Li, Biao; Cheng, Tanyu, E-mail: tycheng@shnu.edu.cn; Liu, Guohua

    2017-04-01

    Recently, the controlled drug delivery system has become a potential platform for biomedical application. Herein, we developed a pH and light-dual controlled cargo release system exhibiting AND logic based on MCM-41 mesoporous silica nanoparticles, which was surface modified using β-cyclodextrin (β-CD) with imine bond and azobenzene derivative. The complex of β-CD and azobenzene derivative effectively blocked the cargo delivery in pH = 7.0 phosphate buffered saline (PBS) solution without 365 nm UV light irradiation. The cargo was fully released when both factors of acidic environment (pH = 5.0 PBS) and 365 nm UV light irradiation were satisfied, meanwhile only very little cargo was delivered if one factor was satisfied. The result also demonstrates that the opening/closing of the gate and the release of the cargo in small portions can be controlled. - Highlights: • A pH and light-dual controlled cargo release system exhibiting AND logic is developed. • The delivery system can release the cargo in small potions by controlling the opening/closing of the gate. • The delivery system realizes the controlled release in zebrafish.

  16. Rapid synthesis of Ti-MCM-41 by microwave-assisted hydrothermal method towards photocatalytic degradation of oxytetracycline.

    Science.gov (United States)

    Chen, Hanlin; Peng, Yen-Ping; Chen, Ku-Fan; Lai, Chia-Hsiang; Lin, Yung-Chang

    2016-06-01

    This study employed microwave-assisted hydrothermal method to synthesize Ti-MCM-41, which are mesoporous materials with a high surface area and excellent photocatalytic ability. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet-visible spectroscopy (UV-Vis) were employed. The XRD findings showed that Ti-MCM-41 exhibited a peak at 2θ of 2.2°, which was attributed to the hexagonal MCM-41 structure. The BET (Brunauer-Emmett-Teller) results agreed with the TEM findings that Ti-MCM-41 has a pore size of about 3-5nm and a high surface area of 883m(2)/g. FTIR results illustrated the existence of Si-O-Si and Si-O-Ti bonds in Ti-MCM-41. The appearance of Ti 2p peaks in the XPS results confirmed the FTIR findings that the Ti was successfully doped into the MCM-41 structure. Zeta (ζ)-potential results indicated that the iso-electric point (IEP) of Ti-MCM-41 was at about pH3.02. In this study, the photocatalytic degradation of oxytetracycline (OTC) at different pH was investigated under Hg lamp irradiation (wavelength 365nm). The rate constant (K'obs) for OTC degradation was 0.012min(-1) at pH3. Furthermore, TOC (total organic carbon) and high resolution LC-MS (liquid chromatography-mass spectrometry) analyses were conducted to elucidate the possible intermediate products and degradation pathway for OTC. The TOC removal efficiency of OTC degradation was 87.0%, 74.4% and 50.9% at pH3, 7 and 10, respectively. LC-MS analysis results showed that the degradation products from OTC resulted from the removal of functional groups from the OTC ring. Copyright © 2016. Published by Elsevier B.V.

  17. Preparation of mesoporous Cs-POM@MOF-199@MCM-41 under two different synthetic methods for a highly oxidesulfurization of dibenzothiophene.

    Science.gov (United States)

    Li, Si-Wen; Li, Jia-Rong; Jin, Qi-Ping; Yang, Zhi; Zhang, Rong-Lan; Gao, Rui-Min; Zhao, Jian-She

    2017-09-05

    Two different synthetic methods, the direct method and the substitution method, were used to synthesize the Cs-POM@MOF-199@MCM-41 (Cs-PMM), in which the modified heteropolyacid with cesium salt has been encapsulated into the pores with the mixture of MOF and MCM-41. The structural properties of the as-prepared catalysts were characterized using various analytical techniques: powder X-ray diffraction, FT-IR, SEM, TEM, XPS and BET, confirming that the Cs-POM active species retained its Keggin structure after immobilization. The substitution method of Cs-PMM exhibited more excellent catalytic performance for oxidative desulfurization of dibenzothiophene in the presence of oxygen. Under optimal conditions, the DBT conversion rate reached up to 99.6% and could be recycled 10 times without significant loss of catalytic activity, which is mainly attributed to the slow leaching of the active heteropolyacid species from the strong fixed effect of the mixture porous materials. Copyright © 2017. Published by Elsevier B.V.

  18. Decay dynamics of blue-green luminescence in meso-porous MCM-41 nanotubes

    International Nuclear Information System (INIS)

    Lee, Y.C.; Liu, Y.L.; Wang, C.K.; Shen, J.L.; Cheng, P.W.; Cheng, C.F.; Ko, C.-H.; Lin, T.Y.

    2005-01-01

    Time-resolved photoluminescence (PL) was performed to investigate the decay of blue-green luminescence in MCM-41 nanotubes. The PL decay exhibits a clear nonexponential profile, which can be fitted by a stretched exponential function. In the temperature range from 50 to 300 K the photogenerated carriers become thermally activated with a characteristic energy of 29 meV, which is an indication of the phonon-assisted nonradiative process. The temperature dependence of the lifetime of PL decay has been explained using a model based on the radiative recombination of localized carriers and the phonon-assisted nonradiative recombination

  19. Probing the dynamics of 3He atoms adsorbed on MCM-41 with pulsed NMR

    Science.gov (United States)

    Huan, C.; Masuhara, N.; Adams, J.; Lewkowitz, M.; Sullivan, N. S.

    2018-03-01

    We report measurements of the nuclear spin-spin and spin-lattice relaxation times for 3He adsorbed on MCM-41 for temperatures 0.08 < T < 1.2 K. Deviations from Curie behavior are observed at low temperatures. The relaxation times exhibit a two-component behavior representing the differing dynamics of the mobile quasi-free molecules in the center of the tubes compared to the adsorbed layer on the walls. The amplitudes of the two components provide an accurate measure of the number of fluid-like molecules traveling in the center of the nanotubes.

  20. Synthesis, characterization, and near-infrared luminescent properties of the ternary thulium complex covalently bonded to mesoporous MCM-41

    International Nuclear Information System (INIS)

    Feng Jing; Song Shuyan; Xing Yan; Zhang Hongjie; Li Zhefeng; Sun Lining; Guo Xianmin; Fan Weiqiang

    2009-01-01

    The crystal structure of a ternary Tm(DBM) 3 phen complex (DBM=dibenzoylmethane; phen=1, 10-phenanthroline) and the synthesis of hybrid mesoporous material in which the complex covalently bonded to mesoporous MCM-41 are reported. Crystal data: Tm(DBM) 3 phen C 59 H 47 N 2 O 7 Tm, monoclinic, P21/c, a=19.3216(12) A, b=10.6691(7) A, c=23.0165(15) A, α=90 deg., β=91.6330(10) deg., γ=90 deg., V=4742.8(5) A 3 , Z=4. The properties of the Tm(DBM) 3 phen complex and the corresponding hybrid mesoporous material [Tm(DBM) 3 phen-MCM-41] have been studied. The results reveal that the Tm(DBM) 3 phen complex is successfully covalently bonded to MCM-41. Both Tm(DBM) 3 phen complex and Tm(DBM) 3 phen-MCM-41 display typical near-infrared (NIR) luminescence upon excitation at the maximum absorption of the ligands, which contributes to the efficient energy transfer from the ligands to the Tm 3+ ion, an antenna effect. The full width at half maximum (FWHM) centered at 1474 nm in the emission spectrum of Tm(DBM) 3 phen-MCM-41 is 110 nm, which is the potential candidate of broadening amplification band from C band (1530-1560 nm) to S + band (1450-1480 nm) in optical area. - Graphical abstract: The crystal structure of Tm(DBM) 3 phen complex (DBM=dibenzoylmethane; phen=1, 10-phenanthroline). The complex is successfully covalently bonded to MCM-41 (Tm(DBM) 3 phen-MCM-41). After ligand-mediated excitation, the emission spectrum of Tm(DBM) 3 phen-MCM-41 shows the bands 802 and 1474 nm. The FWHM of the 1474-nm band for Tm(DBM) 3 phen-MCM-41 is 110 nm, such a broad spectrum enables a wide gain bandwidth for optical amplification

  1. Removal of Cr(VI from Aqueous Solutions Using mino-fuctionalized Nanoporous MCM-41

    Directory of Open Access Journals (Sweden)

    Farshid Ghorbani

    2016-09-01

    Full Text Available An amino-functionalized nanoporous material was prepared by grafting 3-aminopropyl trimethoxysilane (APTMS group onto MCM-41. The as-synthesized material was characterized by X-ray diffraction (XRD analysis, nitrogen adsorption-desorption measurements (BET, thermogravimetric analysis (TGA, and Fourier transform infrared spectrometry (FTIR to confirm the ordered mesoporous structure and the functionalization of the amino group. The NH2-MCM-41 thus obtained was employed as the sorbent to remove Cr(VI ions from aqueous solutions. The batch adsorption process was carried out to evaluate the effects of solution pH, adsorbent dosage, metal ion concentration, and temperature. Results revealed that removal efficiency increased to a maximum of 124 mg.g‒1 and metal uptake decreased (0.1 g.l‒1 with increasing sorbent dosage from 0.1 to 3.5 g.l‒1. A reverse trend was, however, observed with increasing Cr(VI concentration. It was also found that a pH equal to 3 was the optimum level for the removal of Cr(VI ions from aqueous solutions. Thermodynamic examinations revealed the strong dependence of the adsorption process on temperature such that adsorption capacity increased with increasing temperature, indicating the endothermic and spontaneous nature of the adsorption process.

  2. Kinetic study of the catalytic pyrolysis of elephant grass using Ti-MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Fontes, Maria do Socorro Braga; Melo, Dulce Maria de Araujo; Rodrigues, Glicelia, E-mail: socorro.fontes@yahoo.com.br [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil); Barros, Joana Maria de Farias [Universidade Federal de Campina Grande (UFCG), Cuite, PB (Brazil). Dept. de Quimica; Braga, Renata Martins [Universidade Federal da Paraiba (UFPB/CEAR/DEER), Joao Pessoa, PB (Brazil). Centro de Energias Alternativas e Renovaveis. Dept. de Engenharia de Energia Renovaveis

    2014-08-15

    This work aimed to study the kinetics of thermal and catalytic pyrolysis using Ti-MCM-41 as catalyst in order to assess the catalytic pyrolysis efficiency compared to thermal pyrolysis of elephant grass. Ti-MCM-41 molecular sieve was synthesized by hydrothermal method from hydrogel with the following molar composition: 1.00 CTMABr: 4.00 SiO{sub 2}:X TiO{sub 2}: 1 + X Na{sub 2}O: 200.00 H{sub 2}O, which structure template used was cetyltrimethylammonium bromide (CTMABr). The materials synthesized were characterized by X-ray diffraction, IR spectroscopy, thermogravimetric analysis and specific area by the BET method, for subsequent application in the biomass pyrolysis process. The kinetic models proposed by Vyazovkin and Flynn-Wall were used to determine the apparent activation energy involved in the thermal and catalytic pyrolysis of elephant grass and the results showed that the catalyst used was effective in reducing the apparent activation energy involved in the thermal decomposition of elephant grass. (author)

  3. Manganese porphyrin immobilized on magnetic MCM-41 nanoparticles as an efficient and reusable catalyst for alkene oxidations with sodium periodate

    Science.gov (United States)

    Hajian, Robabeh; Ehsanikhah, Amin

    2018-01-01

    This study describes the immobilization of tetraphenylporphyrinatomanganese(III) chloride, (MnPor), onto imidazole functionalized MCM-41 with magnetite nanoparticle core (Fe3O4@MCM-41-Im). The resultant material (Fe3O4@MCM-41-Im@MnPor) was characterized by X-ray diffractometry (XRD), Fourier transform infra-red (FT-IR), diffuse reflectance UV-Vis spectrophotometry (DR UV-Vis), field emission scanning electron microscopy (FESEM), Inductively coupled plasma (ICP), analyzer transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. This new heterogenized catalyst was applied as an efficient catalyst for the epoxidation of a variety of cyclic and linear olefins with NaIO4 under mild conditions. The prepared catalyst can be easily recovered through the application of an external magnet, and reused several times without any significant decrease in activity and magnetic properties.

  4. The Correlation of Adsorption Behavior between Ciprofloxacin Hydrochloride and the Active Sites of Fe-doped MCM-41

    Directory of Open Access Journals (Sweden)

    Ying Wu

    2018-02-01

    Full Text Available HIGHLIGHTSFe incorporation significantly accelerated the adsorption of CPX on MCM-41.Fe leaching can be ignored when pH was higher than 4.0.pH played an important role in CPX adsorption on Fe-MCM-41.Co-effect of CPX and metal cations on Fe-MCM-41 was investigated.Fe-MCM-41s with various molar ratios of silicon to iron (20, 40, 80, and 160 were prepared to investigate adsorption properties of ciprofloxacin hydrochloride (CPX in aqueous solutions. Fe-MCM-41s were characterized by transmission electron microscope (TEM, X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS, nitrogen adsorption/desorption isotherms, and infrared spectroscopy (FT-IR. Effects of silicon-iron ratio, adsorbent dosage, pH, and temperature were conducted to explore the adsorption mechanism of CPX on Fe-MCM-41. The results showed that the introduction of iron facilitated the absorption quantity for CPX from 20.04 to 83.33 mg g−1 at 120 min of reaction time, which was mainly attributed to surface complexation. The promotion of hydrophobic effect, electrostatic interactions, and π-π electron donor-acceptor interaction also played coordinate roles in the adsorption process. The experimental kinetic data followed both the pseudo-second-order and intra-particle diffusion models, while the adsorption isotherm data fit well to Freundlich model at high temperature. Thermodynamic study showed that the adsorption was spontaneous. Under the effect of electrostatic interaction, pH of the solution strongly affected CPX adsorption. Five representative metal cations (Ca, Cu, Ni, Pb, and Cd were chosen to study the effects on CPX adsorption and their complexation. The inhibiting effect of metal cations on CPX adsorption was sequenced in the order of Cu > Ni > Pb > Cd > Ca, which followed the same order as the complexation stability constants between CPX and cations. The Fe-MCM-41 adsorbent possessed excellent reusability for 4 cycles use, suggesting a potential applicability of

  5. A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids.

    Science.gov (United States)

    Yahaya, Noorfatimah; Sanagi, Mohd Marsin; Abd Aziz, Noorizan; Wan Ibrahim, Wan Aini; Nur, Hadi; Loh, Saw Hong; Kamaruzaman, Sazlinda

    2017-02-01

    A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C 18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile-0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1-10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3-114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis. Copyright © 2016 John Wiley & Sons, Ltd.

  6. Influence of aluminum addition in the framework of MCM-41 mesoporous molecular sieve synthesized by non-hydrothermal method in an alkali-free system

    Energy Technology Data Exchange (ETDEWEB)

    La-Salvia, Nathália; Lovón-Quintana, Juan José; Lovón, Adriana Siviero Pagani; Valença, Gustavo Paim, E-mail: nathalialasalvia@gmail.com [Laboratório para o Estudo de Processos de Adsorção e Catálise - LEPAC, Faculdade de Engenharia Química, Universidade Estadual de Campinas - UNICAMP, Campinas, SP (Brazil)

    2017-11-15

    Purely siliceous MCM-41 and Al-containing MCM-41 (Al-MCM-41) mesoporous materials were synthesized by non-hydrothermal method in alkali-free ions medium at room temperature and short reaction times. Under these synthesis conditions, it was also investigated the influence of Al incorporation in the crystal structure of MCM-41. The solids were characterized by ICP-OES, AAS, N{sub 2} adsorption at 77 K, XRD, TEM, NH3 -TPD, {sup 27}Al and {sup 29}Si-MAS-NMR, FT-IR and TGA. The resulting mesoporous materials showed a well-defined hexagonally ordered pore geometry maintaining a uniform and unimodal pore size distribution with high specific surface areas (1000-1400 m{sup 2} g{sup -1}). The Al{sup +3} ions were introduced successfully in the structure of the purely siliceous MCM-41 expanding the unit cell parameter and forming four-coordinated Al species, and in a less extent, forming six-coordinated Al species. In addition, the surface acidity of the MCM-41 increased with Al loading. Contrary, the presence of Al in the MCM-41 mesoporous structure resulted in a decrease of the crystallinity and specific surface area possibly due to the presence of Al species in highly distorted tetrahedral structures and Al extra-framework or amorphous alumina occluded in the pores. The MCM-41 type mesoporous materials obtained in this work show similar characteristics of those synthesized by conventional hydrothermal methods. (author)

  7. Influence of aluminum addition in the framework of MCM-41 mesoporous molecular sieve synthesized by non-hydrothermal method in an alkali-free system

    International Nuclear Information System (INIS)

    La-Salvia, Nathália; Lovón-Quintana, Juan José; Lovón, Adriana Siviero Pagani; Valença, Gustavo Paim

    2017-01-01

    Purely siliceous MCM-41 and Al-containing MCM-41 (Al-MCM-41) mesoporous materials were synthesized by non-hydrothermal method in alkali-free ions medium at room temperature and short reaction times. Under these synthesis conditions, it was also investigated the influence of Al incorporation in the crystal structure of MCM-41. The solids were characterized by ICP-OES, AAS, N 2 adsorption at 77 K, XRD, TEM, NH3 -TPD, 27 Al and 29 Si-MAS-NMR, FT-IR and TGA. The resulting mesoporous materials showed a well-defined hexagonally ordered pore geometry maintaining a uniform and unimodal pore size distribution with high specific surface areas (1000-1400 m 2 g -1 ). The Al +3 ions were introduced successfully in the structure of the purely siliceous MCM-41 expanding the unit cell parameter and forming four-coordinated Al species, and in a less extent, forming six-coordinated Al species. In addition, the surface acidity of the MCM-41 increased with Al loading. Contrary, the presence of Al in the MCM-41 mesoporous structure resulted in a decrease of the crystallinity and specific surface area possibly due to the presence of Al species in highly distorted tetrahedral structures and Al extra-framework or amorphous alumina occluded in the pores. The MCM-41 type mesoporous materials obtained in this work show similar characteristics of those synthesized by conventional hydrothermal methods. (author)

  8. Selective catalytic reduction of NO{sub x} in lean-burn engine exhaust over a Pt/V/MCM-41 catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Jeon, Jong Yeol; Kim, Hee Young [Division of Advanced Chemical Technology, Korea Reasearch Institute of Chemical Technology, P.O. Box 107, Yusong, Taejon 305-600 (Korea, Republic of); Woo, Seong Ihl [Department of Chemical and Biomolecular Engineering, Center for Ultramicrochemical Process Systems, Korea Advanced Institute of Science and Technology, 373-1, Kusong-dong, Yusong-gu, Taejon, 305-701 (Korea, Republic of)

    2003-09-08

    The activities of Pt supported on various metal-substituted MCM-41 (V-, Ti-, Fe-, Al-, Ga-, La-, Co-, Mo-, Ce-, and Zr-MCM-41) and V-impregnated MCM-41 were investigated for the reduction of NO by C{sub 3}H{sub 6}. Among these catalysts, Pt supported on V-impregnated MCM-41 showed the best activity. The maximum conversion of NO into N{sub 2}+N{sub 2}O over this Pt/V/MCM-41 catalyst (Pt=1wt.%, V=3.8wt.%) was 73%, and this maximum conversion was sustained over a temperature range of 70C from 270 to 340C. The high activity of Pt/V/MCM-41 over a broad temperature range resulted from two additional reactions besides the reaction occurring on usual supported Pt, the reaction of NO with surface carbonaceous materials, and the reaction of NO occurring on support V-impregnated MCM-41. The former additional reaction showed an oscillation characteristic, a phenomenon in which the concentrations of parts of reactant and product gases oscillate continuously. At low temperature, some water vapor injected into the reactant gas mixture promoted the reaction occurring on usual supported Pt, whereas at high temperature, it suppressed the additional reaction related to carbonaceous materials. Five-hundred parts per million of SO{sub 2} added to the reactant gas mixture only slightly decreased the NO conversion of Pt/V/MCM-41.

  9. Fe/MCM-41 sylilated catalyst: structural changes determination during the Fischer-Tropsch reaction

    International Nuclear Information System (INIS)

    Bengoa, J. F.; Fellenz, N. A.; Cagnoli, M. V.; Cano, L. A.; Gallegos, N. G.; Alvarez, A. M.; Marchetti, S. G.

    2010-01-01

    Two Fe/MCM-41 systems, one of them sylilated, were obtained to be used as catalysts in Fischer-Tropsch reaction. They have more than 90% of the iron species located inside the support channels, leading to a narrow crystal size distribution accessible to reactive gases. The samples were characterized by X-ray diffraction, atomic absorption spectroscopy, N 2 adsorption, Moessbauer spectroscopy and Fourier transformer infrared spectroscopy. Moessbauer spectroscopy allowed us to demonstrate that the catalytic active species were the same in both catalysts. The only difference between them was the surface hydrophobicity, which decreases the 'water gas shift reaction' in the sylilated catalyst. Besides, this solid is more active for hydrocarbon production, with a lower methane yield.

  10. Hydroconversion of methyl laurate on bifunctional Ni2P/AlMCM-41 catalyst prepared via in situ phosphorization using triphenylphosphine

    Science.gov (United States)

    Zhao, Sha; Zhang, Zhena; Zhu, Kongying; Chen, Jixiang

    2017-05-01

    A series of Ni2P/AlMCM-41-x bifunctional catalysts with different Si/Al ratios (x) were synthesized by in situ phosphorization of Ni/AlMCM-41-x with triphenylphosphine (nominal Ni/P ratio of 0.75) at 300 °C on a fixed-bed reactor. For comparison, NiP/AlMCM-41-5-TPR was also prepared by the TPR method from the supported nickel phosphate with the Ni/P ratio of 1.0, during which metallic Ni rather than Ni2P formed. TEM images show that Ni and Ni2P particles uniformly distributed in Ni2P/AlMCM-41-x and NiP/AlMCM-41-5-TPR. The Ni2P/AlMCM-41-x acidity increased with decreasing the Si/Al ratio. In the hydroconversion of methyl laurate, the conversions were close to 100% on all catalysts at 360 °C, 3.0 MPa, methyl laurate WHSV of 2 h-1 and H2/methyl laurate ratio of 25. As to Ni2P/AlMCM-41-x, with decreasing the Si/Al ratio, the total selectivity to C11 and C12 hydrocarbons decreased, while the total selectivity to isoundecane and isododecane (Si-C11+i-C12) firstly increased and then decreased. Ni2P/AlMCM-41-5 gave the largest Si-C11+i-C12 of 43.2%. While NiP/AlMCM-41-5-TPR gave higher Si-C11+i-C12 than Ni2P/AlMCM-41-5, it was more active for the undesired Csbnd C bond cleavage and methanation. We propose that the in-situ phosphorization adopted here is a promising approach to preparing Ni2P-based bifunctional catalysts.

  11. High selectivity and stability of Mg-doped Al-MCM-41 for in-situ catalytic upgrading fast pyrolysis bio-oil

    International Nuclear Information System (INIS)

    Karnjanakom, Surachai; Suriya-umporn, Thanyamai; Bayu, Asep; Kongparakul, Suwadee; Samart, Chanatip; Fushimi, Chihiro; Abudula, Abuliti; Guan, Guoqing

    2017-01-01

    Highlights: • Mg-doped Al-MCM-41 was developed for in-situ catalytic upgrading of bio-oils. • Mg/Al-MCM-41 exhibited high selectivity to aromatic hydrocarbons. • The ratio of produced hydrocarbon reached up to 80% in upgraded bio-oil. • 1 wt.% Mg/Al-MCM-41 showed the highest catalytic activity. • Mg/Al-MCM-41 had stable reusability due to its coking inhabitation ability. - Abstract: In-situ catalytic upgrading of bio-oils derived from the fast pyrolysis of cellulose, lignin or sunflower stalk over Mg-doped Al-MCM-41 was investigated in details. It is found that Mg species with doping amounts ranged between 0.25 and 10 wt.% was well dispersed on Al-MCM-41, and that doping Mg on Al-MCM-41 effectively adjusted the acidity and basicity of the catalysts, resulting in significant improvement of bio-oil quality. Mg/Al-MCM-41 exhibited high selective conversion of bio-oils derived from cellulose, lignin or sunflower stalk to high value-added aromatic hydrocarbons via catalytic cracking, deoxygenation and aromatization. In the upgraded bio-oil, the relative total hydrocarbon amount reached up to approximately ≥80%, which consisted of aromatic hydrocarbon approximately 76% and aliphatic hydrocarbon approximately 4% for all feedstocks. The selectivity to the monocyclic aromatic hydrocarbons (MAHs) such as benzene, toluene and xylenes (BTXs) increased while the coke formed on the catalyst decreased with the increase in Mg doping amount. 1 wt.% Mg/Al-MCM-41 resulted in the highest relative total hydrocarbon amount in the upgraded bio-oil at lower catalytic deoxygenation temperature, and showed stable reusability for at least 5 cycles. It is expected that Mg/Al-MCM-41 can be widely applied for bio-oil upgrading in a practical process.

  12. o-Vanillin functionalized mesoporous silica – coated magnetite nanoparticles for efficient removal of Pb(II) from water

    Energy Technology Data Exchange (ETDEWEB)

    Culita, Daniela C., E-mail: danaculita@yahoo.co.uk [“Ilie Murgulescu” Institute of Physical Chemistry, Splaiul Independentei 202, Bucharest (Romania); Simonescu, Claudia Maria; Patescu, Rodica-Elena [Politehnica University, Faculty of Applied Chemistry and Materials Science, Bucharest (Romania); Dragne, Mioara [S.C. KEMCRISTAL S.R.L., Muncii Str., No. 51, Fundulea, Călăraşi (Romania); Stanica, Nicolae [“Ilie Murgulescu” Institute of Physical Chemistry, Splaiul Independentei 202, Bucharest (Romania); Oprea, Ovidiu [Politehnica University, Faculty of Applied Chemistry and Materials Science, Bucharest (Romania)

    2016-06-15

    o-Vanillin functionalized mesoporous silica – coated magnetite (Fe{sub 3}O{sub 4}@MCM-41-N-oVan) was synthesized and fully characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, N{sub 2} adsorption–desorption technique and magnetic measurements. The capacity of Fe{sub 3}O{sub 4}@MCM-41-N-oVan to adsorb Pb(II) from aqueous solutions was evaluated in comparison with raw mesoporous silica – coated magnetite (Fe{sub 3}O{sub 4}@MCM-41) and amino – modified mesoporous silica coated magnetite (Fe{sub 3}O{sub 4}@MCM-41-NH{sub 2}). The effect of adsorption process parameters such us pH, contact time, initial Pb(II) concentration was also investigated. The adsorption data were successfully fitted with the Langmuir model, exhibiting a maximum adsorption capacity of 155.71 mg/g at pH=4.4 and T=298 K. The results revealed that the adsorption rate was very high at the beginning of the adsorption process, 80–90% of the total amount of Pb(II) being removed within the first 60 min, depending on the initial concentration. The results of the present work suggest that Fe{sub 3}O{sub 4}@MCM-41-N-oVan is a suitable candidate for the separation of Pb(II) from contaminated water. - Graphical abstract: A novel magnetic adsorbent based on o-vanillin functionalized mesoporous silica – coated magnetite was synthesized and fully characterized and its adsorption capacity for Pb(II) ions in aqueous solutions was evaluated. The maximum adsorption capacity for Pb(II) ions was determined to be 155.71 mg g{sup −1}. The adsorption rate was very high at the beginning of the adsorption process, 90% of the total amount of Pb(II) being removed within the first 60 min. Display Omitted.

  13. EFFECT OF AGING TIME TOWARD CRYSTALLINITY OF PRODUCTS IN SYNTHESIS OF MESOPOROUS SILICATES MCM-41

    Directory of Open Access Journals (Sweden)

    Suyanta Suyanta

    2010-12-01

    Full Text Available Researches about the effects of aging time toward crystallinity of products in the synthesis of mesoporous silicates MCM-41 have been done. MCM-41 was synthesized by hydrothermal treatment to the mixture of sodium silicate, sodium hydroxide, cetyltrimetylammoniumbromide (CTMAB and aquadest in the molar ratio of 8Na2SiO3 : CTMAB : NaOH : 400H2O. Hydrothermal treatment was carried out at 110 °C in a teflon-lined stainless steel autoclave heated in the oven, with variation of aging time, i.e.: 4, 8, 12, 16, 24, 36, 48, and 72 h respectively. The solid phase were filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcinations at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined powders were characterized by using FTIR spectroscopy and X-ray diffraction method. The relative crystallinity of products was evaluated based on the intensity of d100 peaks. The best product was characterized by using N2 physisorption method in order to determine the specific surface area, mean pore diameter, lattice parameter, and pore walls thickness. It was concluded that the relative crystallinity of the products was sensitively influenced by the aging time. The highest relative crystallinity was achieved when used 36 h of aging time in hydrothermal treatment. In this optimum condition the product has 946.607 m2g-1 of specific surface area, 3.357 nm of mean pore diameter, 4.533 nm of lattice parameter, and 1.176 nm of pore walls thickness.

  14. Eco-friendly synthesis for MCM-41 nanoporous materials using the non-reacted reagents in mother liquor.

    Science.gov (United States)

    Ng, Eng-Poh; Goh, Jia-Yi; Ling, Tau Chuan; Mukti, Rino R

    2013-03-04

    Nanoporous materials such as Mobil composite material number 41 (MCM-41) are attractive for applications such as catalysis, adsorption, supports, and carriers. Green synthesis of MCM-41 is particularly appealing because the chemical reagents are useful and valuable. We report on the eco-friendly synthesis of MCM-41 nanoporous materials via multi-cycle approach by re-using the non-reacted reagents in supernatant as mother liquor after separating the solid product. This approach was achieved via minimal requirement of chemical compensation where additional fresh reactants were added into the mother liquor followed by pH adjustment after each cycle of synthesis. The solid product of each successive batch was collected and characterized while the non-reacted reagents in supernatant can be recovered and re-used to produce subsequent cycle of MCM-41. The multi-cycle synthesis is demonstrated up to three times in this research. This approach suggests a low cost and eco-friendly synthesis of nanoporous material since less waste is discarded after the product has been collected, and in addition, product yield can be maintained at the high level.

  15. Experimental Study of the Effect of Si/Al Composition on the Aluminum Distribution in (Al)MCM-41

    Czech Academy of Sciences Publication Activity Database

    Dědeček, Jiří; Žilková, Naděžda; Čejka, Jiří

    44-45, 1/3 (2001), s. 259-266 ISSN 1387-1811 R&D Projects: GA AV ČR IAA4040001; GA AV ČR IBS4040017 Institutional research plan: CEZ:AV0Z4040901 Keywords : (Al)MCM-41 * Al distribution * VIS spectroscopy Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.497, year: 2001

  16. 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

  17. Gel-like properties of MCM-41 material and its transformation to MCM-50 in a caustic alkaline surround

    International Nuclear Information System (INIS)

    Saputra, Hens; Othman, Raihan; Sutjipto, A.G.E.; Muhida, R.; Ani, M.H.

    2012-01-01

    Highlights: ► MCM-41 material transforms gradually into MCM-50 lamellar gel upon controlled exposure to 6 M KOH. ► The formation of MCM-50 ordered gel structure occurs at KOH weight content of 40–70 wt. %. ► MCM gel phase shows pseudoplastic behavior and possesses homogeneous matrix texture. -- Abstract: MCM-41 material, prepared by sol–gel method, reveals gel-like properties in a caustic alkaline environment, i.e., 6 M potassium hydroxide (KOH) electrolyte. The gellation of MCM-41 starts at a KOH weight ratio of 40 wt.%. The structural change of the material is verified with X-Ray diffractograms and supported by observation using Scanning Electron Microscope (SEM). As the KOH weight ratio increases, the MCM-41 hexagonal arrays structure gradually transforms into MCM-50 lamellar structure before disappearing completely at 80 wt.% KOH. The MCM gel phase is further characterized by rotational viscometry and texture analysis. The gel phase shows shear thinning or pseudoplastic behavior and possesses homogeneous matrix structure.

  18. Cross flow ultrafiltration of Cr (VI) using MCM-41, MCM-48 and Faujasite (FAU) zeolite-ceramic composite membranes.

    Science.gov (United States)

    Basumatary, Ashim Kumar; Kumar, R Vinoth; Ghoshal, Aloke Kumar; Pugazhenthi, G

    2016-06-01

    This work describes the removal of Cr (VI) from aqueous solution in cross flow mode using MCM-41, MCM-48 and FAU zeolite membranes prepared on circular shaped porous ceramic support. Ceramic support was manufactured using locally available clay materials via a facile uni-axial compaction method followed by sintering process. A hydrothermal technique was employed for the deposition of zeolites on the ceramic support. The porosity of ceramic support (47%) is reduced by the formation of MCM-41 (23%), MCM-48 (22%) and FAU (33%) zeolite layers. The pore size of the MCM-41, MCM-48 and FAU membrane is found to be 0.173, 0.142, and 0.153 μm, respectively, which is lower than that of the support (1.0 μm). Cross flow ultrafiltration experiments of Cr (VI) were conducted at five different applied pressures (69-345 kPa) and three cross flow rates (1.11 × 10(-7) - 2.22 × 10(-7) m(3)/s). The filtration studies inferred that the performance of the fabricated zeolite composite membranes is optimum at the maximum applied pressure (345 kPa) and the highest rejection is obtained with the lowest cross flow rate (1.11 × 10(-7) m(3)/s) for all three zeolite membrane. The permeate flux of MCM-41, MCM-48 and FAU zeolite composite membranes are almost remained constant in the entire duration of the separation process. The highest removal of 82% is shown by FAU membrane, while MCM-41 and MCM-48 display 75% and 77% of Cr (VI) removal, respectively for the initial feed concentration of 1000 ppm with natural pH of the solution at an applied pressure of 345 kPa. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. The correlation of adsorption behavior between ciprofloxacin hydrochloride and the active sites of Fe-doped MCM-41

    Science.gov (United States)

    Wu, Ying; Tang, Yiming; Li, Laisheng; Liu, Peihong; Li, Xukai; Chen, Weirui; Xue, Ying

    2018-02-01

    Fe-MCM-41s with various molar ratios of silicon to iron (20, 40, 80 and 160) were prepared to investigate adsorption properties of ciprofloxacin hydrochloride (CPX) in aqueous solutions. Fe-MCM-41s were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and infrared spectroscopy (FT-IR). Effects of silicon–iron ratio, adsorbent dosage, pH and temperature were conducted to explore the adsorption mechanism of CPX on Fe-MCM-41. The results showed that the introduction of iron facilitated the absorption quantity for CPX from 20.04 to 83.33 mg g-1 at 120 min of reaction time, which was mainly attributed to surface complexation. The promotion of hydrophobic effect, electrostatic interactions and π-π electron donor–acceptor interaction also played coordinate roles in the adsorption process. The experimental kinetic data followed both the pseudo-second-order and intra-particle diffusion models, while the adsorption isotherm data fit well to Freundlich model at high temperature. Thermodynamic study showed that the adsorption was spontaneous. Under the effect of electrostatic interaction, pH of the solution strongly affected CPX adsorption. Five representative metal cations (Ca, Cu, Ni, Pb and Cd) were chosen to study the effects on CPX adsorption and their complexation. The inhibiting effect of metal cations on CPX adsorption was sequenced in the order of Cu > Ni > Pb > Cd > Ca, which followed the same order as the complexation stability constants between CPX and cations. The Fe-MCM-41 adsorbent possessed excellent reusability for 4 cycles use, suggesting a potential applicability of Fe-MCM-41 to remove CPX in water.

  20. Synthesis and characterization of Co (Ni or Cu)-MCM-41 mesoporous molecular sieves with different amount of metal obtained by using microwave irradiation method

    International Nuclear Information System (INIS)

    Jiang Tingshun; Zhao Qian; Chen Kangmin; Tang Yajing; Yu Longbao; Yin Hengbo

    2008-01-01

    Co (Ni or Cu)-MCM-41 mesoporous molecular sieves with different amount of metal were synthesized by using cetyltrimethyl ammonium bromide as a template and by a novel microwave irradiation method. These samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N 2 physical adsorption. The experimental results show that Co (Ni or Cu)-MCM-41 mesoporous molecular sieves were successfully synthesized. When the as-synthesized samples were calcined at 550 deg. C for 10 h, the template was effectively removed. Under microwave irradiation condition, Co-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 745.7-1188.8 m 2 /g and average pore sizes in a range of 2.46-2.75 nm; Ni-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 625.8-1161.3 m 2 /g and average pore sizes of ca. 2.7 nm; Cu-MCM-41 mesoporous molecular sieves have specific surface areas in a range of 601.6-1142.9 m 2 /g and average pore sizes in a range of 2.46-2.76 nm. On the other hand, with increasing the introduced metal amount, the specific surface area and pore volume of the synthesized Co (Ni or Cu)-MCM-41 mesoporous molecular sieves became small, and the mesoporous ordering of the samples became poor. Under the comparable synthesis conditions, the synthesized Co-MCM-41 mesoporous molecular sieve has a bigger specific surface area and a more uniform pore distribution as compared with the synthesized Ni-MCM-41and Cu-MCM-41 mesoporous molecular sieves

  1. Synthesis of PdO/MCM-41 nanocomposites using trans-[PdCl2(PEt3)2] as the source of metal

    International Nuclear Information System (INIS)

    Hernandez-Pineda, Jessica; Rio, Jose Manuel del; Carreto, Enrique; Terres, Eduardo; Montoya, J. Asencion; Zuniga-Gonzalez, Maria de Jesus; Morgado, Jorge

    2009-01-01

    Three PdO/MCM-41 nanocomposites containing PdO species that are dispersed on an MCM-41 support have been prepared using trans-[PdCl 2 (PEt 3 ) 2 ] as the source of metal. Thermal gravimetric analysis of the decomposition of this complex in air reveals a remarkable mass loss of all nonmetallic elements centered at 300 deg. C. The materials were characterized with X-ray powder diffraction (XRPD), nitrogen sorption and TEM, which showed that the PdO nanoparticles were present inside the pores of MCM-41. XRPD analysis confirms formation of PdO (palladinite) nanocrystals, as the sole crystalline phase present in the nanocomposites.

  2. Cascade synthesis of dihydrobenzofuran via Claisen rearrangement of allyl aryl ethers using FeCl3/MCM-41 catalyst

    Directory of Open Access Journals (Sweden)

    Sachin S. Sakate

    2018-05-01

    Full Text Available Dihydrobenzofuran as one of the active ingredients of the naturally occurring motif is synthesized by using in situ generation of ortho allyl phenols. Aryl allyl ethers on reacting with catalytic amounts of non noble metal iron (III chloride supported on MCM-41 under moderate reaction conditions yield dihydrobenzofuran. First step via Claisen rearrangement gives ortho allyl phenol followed by its in situ cyclization to yield dihydrobenzofuran in very good yields. Both Lewis as well as Brønsted acidity of the catalyst as evidenced by Py-FTIR studies was found to catalyze the cascade synthesis of dihydrobenzofuran. The scope of the present strategy was successfully demonstrated for several substrates with varying electronic effects for the synthesis of corresponding dihydrobenzofuran with high yields in a range of 71–86%. Keywords: Claisen rearrangement, Dihydrobenzofuran, Aryl allyl ether, MCM-41, Ferric chloride

  3. Epoxidation of natural limonene extracted from orange peels with hydrogen peroxide over Ti-MCM-41 catalyst

    Directory of Open Access Journals (Sweden)

    Wróblewska Agnieszka

    2018-03-01

    Full Text Available The paper presents the oxidation of natural limonene (extracted from waste orange peels by 60 wt% hydrogen peroxide, in the presence of Ti-MCM-41 catalyst and in methanol as the solvent. The aim of the research was to develop the most favorable technological parameters for the process of limonene oxidation (temperature, molar ratio of limonene to hydrogen peroxide, methanol concentration, Ti-MCM-41 catalyst content and reaction time by analyzing changes in the main functions describing this process: the conversion of limonene, selectivities of appropriate products, the conversion of hydrogen peroxide and the effective conversion of hydrogen peroxide. The process is environmentally friendly process and it uses renewable raw material - limonene and a safe oxidant -hydrogen peroxide. During the study, very valuable oxygenated derivatives of limonene were obtained: 1,2-epoxylimonene, its diol, carvone, carveol, and perillyl alcohol. These compounds are used in medicine, cosmetics, perfumery, food and polymers industries.

  4. Neutron spin echo measurements of monolayer and capillary condensed water in MCM-41 at low temperatures

    International Nuclear Information System (INIS)

    Yoshida, K; Yamaguchi, T; Kittaka, S; Bellissent-Funel, M-C; Fouquet, P

    2012-01-01

    Neutron spin echo measurements of monolayer and capillary condensed heavy water (D 2 O) confined in MCM-41 C10 (pore diameter 2.10 nm) were performed in a temperature range of 190-298 K. The intermediate scattering functions were analyzed by the Kohlrausch-Williams-Watts stretched exponential function. The relaxation times of confined D 2 O in the capillary condensed state follow remarkably well the Vogel-Fulcher-Tammann equation between 298 and 220 K, whereas below 220 K they show an Arrhenius type behavior. That is, the fragile-to-strong (FTS) dynamic crossover occurs, which has never been seen in experiments on bulk water. On the other hand, for monolayer D 2 O, the FTS dynamic crossover was not observed in the temperature range measured. The FTS dynamic crossover observed in capillary condensed water would take place in the central region of the pore, not near the pore surface. Because the tetrahedral-like water structure in the central region of the pore is more preserved than that near the pore surface, the FTS dynamic crossover would be concerned with the tetrahedral-like water structure. (paper)

  5. A Cu/Al-MCM-41 mesoporous molecular sieve: application in the abatement of no in exhaust gases

    Directory of Open Access Journals (Sweden)

    M. S. Batista

    2005-09-01

    Full Text Available Propane oxidation and reduction of NO to N2 with propane under oxidative conditions on a Cu-Al-MCM-41 mesoporous molecular sieve and Cu-ZSM-5 zeolites were studied. Both types of catalysts were prepared by ion exchange in aqueous solutions of copper acetate and characterised by X-ray diffraction (XRD, nitrogen sorption measurement, diffuse reflectance ultra-violet spectroscopy (DRS-UV, diffuse reflectance infra-red Fourier transform spectroscopy (DRIFTS of the adsorption of CO on Cu+ and temperature-programmed reduction with hydrogen (H2-TPR. The NO reduction was performed between 200 and 500 ºC using a GHSV = 42,000 h-1. H2-TPR data showed that in the prepared Cu-Al-MCM-41 all the Cu atoms are on the surface of the mesopores as highly dispersed CuO, which results in a decrease in specific surface area and in mesopore volume. H2-TPR together with DRIFTS data provided evidence that in Cu/ZSM-5 catalysts, Cu atoms are found as two different Cu2+ cations: Cualpha2+ and Cubeta2+, which are located on charge compensation sites, and their thermo-redox properties were different from those of Cu atoms in Cu-Al-MCM-41. The specific activity of the Cu2+ exchangeable cations in Cu-ZSM-5, irrespective of their nature, was much greater than that of the Cu2+ in Cu-Al-MCM-41, where they are found as CuO.

  6. Efeito de diferentes fontes de sílica nos parâmetros texturais da peneira molecular MCM-41

    Directory of Open Access Journals (Sweden)

    M. S. B. Fontes

    2016-03-01

    Full Text Available Resumo Nas últimas décadas, pesquisas estão sendo desenvolvidas para obtenção de materiais eficientes e economicamente viáveis para aplicação em diversos setores da indústria. Os materiais mesoporosos da família MCM-41 estão entre os candidatos eficazes pela facilidade de síntese e estrutura que favorece uma gama de aplicações. O objetivo desse trabalho foi apresentar uma abordagem rítica das características e propriedades dos materiais mesoporosos do tipo MCM-41, enfocando nos aspectos estruturais. Além isso, foram discutidas as vantagens e desvantagens do uso de sílica comerciais e alternativas. As fontes de sílica comerciais analisadas foram sílica gel e TEOS; já as fontes de sílica alternativas foram cinza da casca de arroz, quartzo e pó de vidro. Os materiais analisados foram sintetizados pelo método hidrotérmico e caracterizados por DRX, FTIR, BET e TG. Os resultados apresentados comprovam a eficiência das fontes de sílica alternativas na síntese do MCM-41, pois os materiais apresentaram propriedades texturais dentro dos padrões exigidos. Dessa forma, eles estão aptos a serem testados na indústria em substituição aos MCM-41 sintetizados com fonte de sílica comercial.

  7. Mesoporous MCM-41 embeded with Ru(II)-based chemosensor: Preparation, characterization, and emission variation towards pH

    International Nuclear Information System (INIS)

    Jingxia, Wang

    2014-01-01

    In this article, a pH sensing mesoporous MCM-41 material containing covalently bonded Ru(II) complex in the silicate network was prepared and named as Ru–MCM-41. The emission signal shows a tendency to decrease upon increasing pH values. The luminescent pH sensor can be explained by the protonation and deprotonation of the PIP ligand (PIP=2-phenyl-1H-imidazo[4,5-f][1,10]phenanthroline) and the fact that the mesoporousity of the MCM-41 matrix favors the –OH that diffused to the complex, resulting in quick emission quenching. It also shows a slight sensitivity towards dissolved molecular oxygen and varying temperatures, which, however, may not be too troublesome for actual applications. The sensing mechanism is also investigated. - Highlights: • An Ru complex was covalently grafted in mesoporous silicate network. • The emission signal decreased with increasing pH values. • The protonation and deprotonation of the ligand caused emission variation. • The emission was insensitive towards oxygen and temperature

  8. Synthesis of magnetic core-shell structure Fe3O4@MCM-41 nanoparticle by vesicles in aqueous solutions☆

    Institute of Scientific and Technical Information of China (English)

    Weiming Song; Xuesong Liu; Ying Yang; Xuejia Han; Qigang Deng

    2015-01-01

    In this study, magnetic core–shel structure Fe3O4@MCM-41 nanoparticles were synthesized with vesicles as soft templates. In the preparation, FeCl2 and tetraethy orthosilicate (TEOS) were selected as Fe processor and Si pre-cursor, respectively. Stable vesicles first formed in 0.03 mol·L−1 1:2 mixture of anionic surfactant sodium dode-cyl sulfate and cationic surfactant cetyltrimethyl ammonium bromide. Then, TEOS was added in the vesicle aqueous solution, leading to a highly dispersed solution. After high-temperature calcination, Fe3O4@MCM-41 nanoparticles were obtained. Their structure and morphology were characterized by Saturn Digisizer, transmis-sion electron microscope and vibrating sample magneto-meter. The results indicate that the vesicles are spherical and their size could be tuned between 20 and 50 nm. The average grain diameter of synthesize magnetic core–shel Fe3O4@MCM-41 particles is 100–150 nm and most of them are in el iptical shape. The dispersion of magnet-ic particles is very good and magnetization values are up to 33.44 emu·g−1, which are superior to that of other Fe3O4 materials reported.

  9. Synthesis of sulfated titania supported on mesoporous silica using direct impregnation and its application in esterification of acetic acid and n-butanol

    International Nuclear Information System (INIS)

    Wang Yuhong; Gan Yunting; Whiting, Roger; Lu Guanzhong

    2009-01-01

    A new method has been developed for the preparation of sulfated titania (S-TiO 2 ) supported on mesoporous silica. The use of direct exchange of metal containing precursors for the surfactants in the as-synthesized MCM-41 substrate produced a product with high sulfur content without serious blockage of the pore structure of MCM-41. The pore sizes and volumes of the resultant S-TiO 2 /MCM-41 composites were found to vary markedly with the loading of TiO 2 . The strong acidic character of the composites obtained was examined by using them as catalysts for the esterification of acetic acid and n-butanol. - Abstract: XRD profiles of the composites of S-TiO 2 /MCM-41 with different TiO 2 contents. The low angle peaks indicate the MCM-41-like structure retained and a TiO 2 phase appeared at high angle region. Display Omitted

  10. Study on performance of composite polymer films doped with modified molecular sieve for lithium-ion batteries

    International Nuclear Information System (INIS)

    Zhang Yuqing; Zhang Guodong; Du Tingdong; Zhang Lizao

    2010-01-01

    To improve the tensile strength and ionic conductivity of composite polymer films for lithium-ion batteries, molecular sieves of MCM-41 modified with sulfated zirconia (SO 4 2- /ZrO 2 , SZ), denoted as MCM-41/SZ, were doped into a poly(vinylidene fluoride) (PVdF) matrix to fabricate MCM-41/SZ composite polymer films, denoted as MCM-41/SZ films. Examination by transmission electron microscope (TEM) shows that modified molecular sieves have lower aggregation and a more porous structure. Tensile strength tests were carried out to investigate the mechanical performance of MCM-41/SZ films, and then the electrochemical performance of batteries with MCM-41/SZ films as separators was tested. The results show that the tensile strength (σ t ) of MCM-41/SZ film was up to 7.8 MPa; the ionic conductivity of MCM-41/SZ film was close to 10 -3 S cm -1 at room temperature; and the coulombic efficiency of the assembled lithium-ion battery was 92% at the first cycle and reached as high as 99.99% after the 20th cycle. Meanwhile, the charge-discharge voltage plateau of the lithium-ion battery presented a stable state. Therefore, MCM-41/SZ films are a good choice as separators for lithium-ion batteries due to their high tensile strength and ionic conductivity.

  11. Sonogashira Reaction of Aryl and Heteroaryl Halides with Terminal Alkynes Catalyzed by a Highly Efficient and Recyclable Nanosized MCM-41 Anchored Palladium Bipyridyl Complex

    Directory of Open Access Journals (Sweden)

    Chung-Yuan Mou

    2010-12-01

    Full Text Available A heterogeneous catalyst, nanosized MCM-41-Pd, was used to catalyze the Sonogashira coupling of aryl and heteroaryl halides with terminal alkynes in the presence of CuI and triphenylphosphine. The coupling products were obtained in high yields using low Pd loadings to 0.01 mol%, and the nanosized MCM-41-Pd catalyst was recovered by centrifugation of the reaction solution and re-used in further runs without significant loss of reactivity.

  12. Adsorption of toxic metal ion Cr(VI) from aqueous state by TiO2-MCM-41: equilibrium and kinetic studies.

    Science.gov (United States)

    Parida, Kulamani; Mishra, Krushna Gopal; Dash, Suresh Kumar

    2012-11-30

    This paper deals with the immobilization of various weight percentage of TiO(2) on mesoporous MCM-41, characterization of the materials by X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier Transform Infrared (FTIR) analysis, UV-vis diffuse reflectance spectroscopy (DRS) and evaluation of the adsorption capacity toward Cr(VI) removal. It is found that the MCM-41 structure retained after loading of TiO(2) but the surface area and pore diameter decreased due to pore blockage. Adsorption of Cr(VI) from aqueous state was investigated on TiO(2)-MCM-41 by changing various parameters such as pH, metal ion concentration, and the temperature. When TiO(2) loading was more than 20 wt.%, the adsorption activity (25)TiO(2)-MCM-41 reduced significantly due to considerable decrease in the surface area. It is also observed that TiO(2) and neat MCM-41 exhibits very less Cr(VI) adsorption compared to TiO(2)-MCM-41. The adsorption of Cr(VI) onto (20)TiO(2)-MCM-41 at pH~5.5 and temperature 323 K was 91% at 100mg/L Cr(VI) metal ion concentration in 80 min. The experimental data fitted well to Langmuir and Freundlich isotherms. The adsorption of Cr(VI) on TiO(2)-MCM-41 followed a second order kinetics with higher values of intra-particle diffusion rate. Thermodynamic parameters suggested that the adsorption process is endothermic in nature and desorption studies indicated a chemisorption mode. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Functionalized silica materials for electrocatalysis

    Indian Academy of Sciences (India)

    To increase the efficiency of the electrocatalytic process and to increase the electrochemical accessibility of the immobilized electrocatalysts, functionalized and non-functionalized mesoporous organo-silica (MCM41-type-materials) are used in this study. These materials possess several suitable properties to be durable ...

  14. Development of an Amperometric Glucose Biosensor Based on the Immobilization of Glucose Oxidase on the Se-MCM-41 Mesoporous Composite

    Directory of Open Access Journals (Sweden)

    Sabriye Yusan

    2018-01-01

    Full Text Available A new bioenzymatic glucose biosensor for selective and sensitive detection of glucose was developed by the immobilization of glucose oxidase (GOD onto selenium nanoparticle-mesoporous silica composite (MCM-41 matrix and then prepared as a carbon paste electrode (CPE. Cyclic voltammetry was employed to probe the catalytic behavior of the biosensor. A linear calibration plot is obtained over a wide concentration range of glucose from 1 × 10−5 to 2 × 10−3 M. Under optimal conditions, the biosensor exhibits high sensitivity (0.34 µA·mM−1, low detection limit (1 × 10−4 M, high affinity to glucose (Km = 0.02 mM, and also good reproducibility (R.S.D. 2.8%, n=10 and a stability of about ten days when stored dry at +4°C. Besides, the effects of pH value, scan rate, mediator effects on the glucose current, and electroactive interference of the biosensor were also discussed. As a result, the biosensor exhibited an excellent electrocatalytic response to glucose as well as unique stability and reproducibility.

  15. Structural analysis and characterization of synthesized ordered mesoporous silicate (MCM-41) using small angle X-rays scattering and complementary techniques

    Science.gov (United States)

    Akinlalu, Ademola V.

    were generated with a proprietary software called edens. In this dissertation, the following observations have been revealed resulting from SAXS measurement. 1. As one increases the hydrolysis duration of ethyl acetate, a gradual collapse of the lattice spacing of the mesoporous silcate MCM-41 is observed. We found from SAXS that there is a slight right shift of the spectra toward the higher q-values indicating that we are gradually losing orderliness in the lattice spacing and hexagonal structure of the mesoporous silica. Also, the intensity of the peak of second and third peaks are diminutive when compared to sample with shorter hydrolysis time. 2. A comparison of the SAXS spectra for the different molar concentration sample reveals that the 0:5M samples shows a deteriorating structural characteristics as compared to the 0:25 and 0:75M samples respectively and a clear decrease in the (100) reflection planes. Also noticed is the slight rightward shift in the overall spectrum prole. This observation suggest that further analysis is needed so as to better understand the result. 3. We establish that during MCM-41 synthesis, longer reaction time is needed to produce quality sample with well defined structurally characteristic for its intended application because according to spectrum for the sample with a longer reaction time (aging), a shift towards the lower q-values indicates that a sample with a larger lattice parameter and wall thickness but the intensities of its peak are diminishing when compared to the other of relatively shorter reaction time. Other complementary techniques were used to corroborated the result obtained from SAXS. Nitrogen adsorption-desorption analysis at 77K was used to generate the isotherms while B.E.T method was used in conjunction with the isotherms to obtained the very important surface area information. SEM provide a visual structural morphology of the samples and FTIR gave the fingerprint detail of the bonds and vibration types between

  16. Efficient adsorption concentration and photolysis of acetaldehyde on titania-mesoporous silica composite

    Science.gov (United States)

    Yamaguchi, Satoshi; Matsumoto, Akihiko

    2017-07-01

    Titania-mesoporous silica composite (TiO2/MCM) was prepared by hydrolysis of titaniumtetraisopropoxide (TTIP) with the presence of mesoporous silica MCM-41. The TiO2/MCM samples consisted of highly dispersed TiO2 on the surface of MCM-41. Dynamic adsorption and photocatalytic decomposition features for acetaldehyde (CH3CHO) were measured by flow method. The amount of CH3CHO decomposition on TiO2/MCM-41 increased with the TiO2 amount, suggesting that a large amount of CH3CHO was adsorbed on mesopores of MCM-41 of the TiO2/MCM and was efficiently decomposed on finely dispersed TiO2 surface by ultraviolet irradiation.

  17. Hydroconversion of methyl laurate on bifunctional Ni{sub 2}P/AlMCM-41 catalyst prepared via in situ phosphorization using triphenylphosphine

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Sha; Zhang, Zhena [Tianjin Key Laboratory of Applied Catalysis Science and Technology, Department of Catalysis Science and Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Zhu, Kongying, E-mail: ausky@tju.edu.cn [Analysis and Measurement Center, Tianjin University, Tianjin 300072 (China); Chen, Jixiang, E-mail: jxchen@tju.edu.cn [Tianjin Key Laboratory of Applied Catalysis Science and Technology, Department of Catalysis Science and Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China)

    2017-05-15

    Highlights: • Bifunctional Ni{sub 2}P/AlMCM-41 was prepared by in situ phosphorization at 300 °C. • There were similar Ni{sub 2}P particle sizes in Ni{sub 2}P/AlMCM-41 with different Si/Al ratios. • The acid amount of Ni{sub 2}P/AlMCM-41 increased with decreasing the Si/Al ratio. • Ni{sub 2}P/AlMCM-41 with the Si/Al ratio of 5 had the highest activity for isomerization. • Ni{sub 2}P/AlMCM-41 had very low activity for methanation and C−C bond hydrogenolysis. - Abstract: A series of Ni{sub 2}P/AlMCM-41-x bifunctional catalysts with different Si/Al ratios (x) were synthesized by in situ phosphorization of Ni/AlMCM-41-x with triphenylphosphine (nominal Ni/P ratio of 0.75) at 300 °C on a fixed-bed reactor. For comparison, NiP/AlMCM-41-5-TPR was also prepared by the TPR method from the supported nickel phosphate with the Ni/P ratio of 1.0, during which metallic Ni rather than Ni{sub 2}P formed. TEM images show that Ni and Ni{sub 2}P particles uniformly distributed in Ni{sub 2}P/AlMCM-41-x and NiP/AlMCM-41-5-TPR. The Ni{sub 2}P/AlMCM-41-x acidity increased with decreasing the Si/Al ratio. In the hydroconversion of methyl laurate, the conversions were close to 100% on all catalysts at 360 °C, 3.0 MPa, methyl laurate WHSV of 2 h{sup −1} and H{sub 2}/methyl laurate ratio of 25. As to Ni{sub 2}P/AlMCM-41-x, with decreasing the Si/Al ratio, the total selectivity to C11 and C12 hydrocarbons decreased, while the total selectivity to isoundecane and isododecane (S{sub i-C11+i-C12}) firstly increased and then decreased. Ni{sub 2}P/AlMCM-41-5 gave the largest S{sub i-C11+i-C12} of 43.2%. While NiP/AlMCM-41-5-TPR gave higher S{sub i-C11+i-C12} than Ni{sub 2}P/AlMCM-41-5, it was more active for the undesired C−C bond cleavage and methanation. We propose that the in-situ phosphorization adopted here is a promising approach to preparing Ni{sub 2}P-based bifunctional catalysts.

  18. Nature of active vanadium nanospecies in MCM-41 type catalysts for olefins oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Chanquía, Corina M., E-mail: cchanquia@cab.cnea.gov.ar [Centro Atómico Bariloche, Comisión Nacional de Energía Atómica (CAB-CNEA). Av. Bustillo 9500, R8402AGP, San Carlos de Bariloche, Río Negro (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET). Avenida Rivadavia 1917, C1033AAJ, Ciudad Autónoma de Buenos Aires (Argentina); Cánepa, Analía L. [Centro de Investigación y Tecnología Química (CITeQ), Universidad Tecnológica Nacional, Facultad Regional Córdoba (UTN-FRC), Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016, Córdoba Capital (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET). Avenida Rivadavia 1917, C1033AAJ, Ciudad Autónoma de Buenos Aires (Argentina); Winkler, Elin L. [Centro Atómico Bariloche, Comisión Nacional de Energía Atómica (CAB-CNEA). Av. Bustillo 9500, R8402AGP, San Carlos de Bariloche, Río Negro (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET). Avenida Rivadavia 1917, C1033AAJ, Ciudad Autónoma de Buenos Aires (Argentina); and others

    2016-06-01

    A multi-technique physicochemical investigation including UV–Vis-DRS, Raman spectroscopy, XPS, ESR and FTIRS with pyridine adsorption was performed to analyze the nature of different vanadium nanospecies present on MCM-41 type catalysts. By employing a direct hydrothermal synthesis, vanadium species were incorporated into siliceous structure mainly as tetrahedrally coordinated isolated V{sup δ+} ions, which would be located inside the wall and on the wall surface of the mesoporous channels. The coexistence of both vanadium oxidation states V{sup 4+} and V{sup 5+} was also revealed. Acidity measurements permitted to infer about the majority presence of Lewis acid sites, which increase with vanadium content. The catalytic performance of these materials was evaluated in the reaction of α-pinene oxidation with H{sub 2}O{sub 2}. The highest intrinsic activity of the sample with lower V loading was attributed to the high dispersion and efficiency of the isolated V{sup δ+} species that actuate as active sites. A mixture of reaction products arising from competitive processes of epoxidation and allylic oxidation was found. - Highlights: • Nature of vanadium nanospecies in mesoporous silicates was investigated. • From hydrothermal sol–gel synthesis, isolated V{sup δ+} sites were mainly generated. • The coexistence of both vanadium oxidation states V{sup 4+} and V{sup 5+} was revealed. • The catalytic performance was evaluated in α-pinene oxidation with H{sub 2}O{sub 2}. • The high catalytic activity is attributed to high dispersion of isolated V{sup δ+} ions.

  19. Modified silica sol coatings for surface enhancement of leather.

    Science.gov (United States)

    Mahltig, Boris; Vossebein, Lutz; Ehrmann, Andrea; Cheval, Nicolas; Fahmi, Amir

    2012-06-01

    The presented study reports on differently modified silica sols for coating applications on leather. Silica sols are prepared by acidic hydrolysis of tetraethoxysilane and modified by silane compounds with fluorinated and non-fluorinated alkylgroups. In contrast to many earlier investigations regarding sol-gel applications on leather, no acrylic resin is used together with the silica sols when applying on leather. The modified silica particles are supposed to aggregate after application, forming thus a modified silica coating on the leather substrate. Scanning electron microscopy investigation shows that the applied silica coatings do not fill up or close the pores of the leather substrate. However, even if the pores of the leather are not sealed by this sol-gel coating, an improvement of the water repellent and oil repellent properties of the leather substrates are observed. These improved properties of leather by application of modified silica sols can provide the opportunity to develop sol-gel products for leather materials present in daily life.

  20. Photooxidation of ethylene over Cu-modified and unmodified silica

    OpenAIRE

    Ichihashi, Yuichi; Matsumura, Yasuyuki

    2003-01-01

    Silica catalyzes photooxidation of ethylene to carbon dioxide and modification of copper on silica results in the lower reaction rate and partial production of ethylene oxide. The reaction does not proceed by the light irradiation through a color filter (λ>280 nm). ESR measurement indicates that radical oxygen species assignable T-shape Si − O3− can be produced on silica by UV irradiation at 77 K. The same species are also found on silica modified with copper by UV irradiation whi...

  1. CO2 capture on micro/meso-porous composites of (zeolite A)/(MCM-41) with Ca2+ located: Computer simulation and experimental studies

    International Nuclear Information System (INIS)

    Jianhai Zhou; Huiling Zhao; Jinxia Li; Yujun Zhu; Jun Hu; Honglai Liu; Ying Hu

    2013-01-01

    Composing of both zeolite and meso-porous structures, micro/meso-porous composites exhibit promising CO 2 capture capabilities. In this work, a full-atomic mimetic 5A-MCM-41 structure with bimodal pores has been constructed, in which the microporous structure of 5A zeolite is constructed and optimized based on zeolite A with Ca and Na cations introduced; whereas the meso-porous MCM-41 structure is produced by caving the cylindrical pores in the obtained 5A zeolite matrix. CO 2 adsorption on 5A-MCM- 41 has been simulated by the grand canonical Monte Carlo (GCMC). The simulation results demonstrated that CO 2 is preferentially adsorbed in micropores, and the CO 2 adsorption capacity and its isosteric heat on 5A-MCM-41 are much larger than those of N 2 . The CO 2 selectivity of 5A-MCM-41 results from the electrostatic interaction of the quadrupole CO 2 molecule with Ca 2+ cations of the zeolite. Furthermore, the hierarchical micro/meso-porous composites are synthesized to verify the simulated predictions. By the hydrothermal reaction using 5A zeolite 'seeds' as the silicon source and hexadecyl trimethylammonium bromide (CTAB) as the meso-porous template, 5A-MCM-41 composites are obtained, the characteristic results show that typical 5A microporous structure is remained and disordered meso-porous networks are produced in the composites.Moreover, the CO 2 adsorption capacity of the 5A-MCM- 41 composites can reach as high as 4.08 mmol/g at 100 kPa and 298 K. These observations have been strongly supported that micro/meso-porous composites with metal ions located would be promising adsorbents for CO 2 separation. (authors)

  2. Kinetics of propane dehydrogenation in CO{sub 2} presence over chromium and gallium oxide catalysts based on MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Lapidus, A.L.; Gaidai, N.A.; Nekrasov, N.V.; Agafonov, A.Yu.; Botavina, M.A. [Russian Academy of Sciences, Moscow (Russian Federation). N.D. Zelinsky Institute of Organic Chemistry

    2012-07-01

    Chromium and gallium catalysts based on MCM-41 with different contents of active metals were prepared and tested for propane dehydrogenation in the presence and absence of CO{sub 2}. It was shown that CO{sub 2} increased the yield of propene and decreased considerably the rate of deactivation of Cr/MCM-41 and decreased propene yield and slightly improved the stability of Ga/MCM-41. The study of kinetics in unstationary and stationary fields showed that the decrease of propene yield was connected with strong competitive adsorption of CO{sub 2} over Ga-catalysts what presented difficulties for propane adsorption. The formation of cracking products was decreased in CO{sub 2} presence over both catalysts. The catalysts were differed by the adsorption capacity of the reaction components: C{sub 3}H{sub 6} was tied more strongly than CO{sub 2} over Cr-catalysts, CO{sub 2} was tied more firmly than C{sub 3}H{sub 6} over Ga-catalysts. Kinetic data showed that of H{sub 2} was bounded with the surface of Ga-catalysts very firmly, reverse watergas shift reaction proceeded in considerably more extent over Cr-catalysts than over Gaones. CO{sub 2} took active participation in oxidation of coke and surface of Cr-catalysts. The positive role of CO{sub 2} in propane dehydrogenation over Ga-catalysts consisted in a decrease of coke and cracking products. Kinetic equations and step-schemes for propene and cracking products formation were proposed. (orig.)

  3. Transformation of levoglucosan over H-MCM-22 zeolite and H-MCM-41 mesoporous molecular sieve catalysts

    International Nuclear Information System (INIS)

    Kaeldstroem, M.; Kumar, N.; Heikkilae, T.; Tiitta, M.; Salmi, T.; Murzin, D. Yu.

    2011-01-01

    Catalytic transformation of levoglucosan (1-6-anhdyro-β-D-glucopyranose) was carried out in a fixed bed reactor at 573 K over zeolite and mesoporous material catalysts. Proton forms of MCM-22-30 and MCM-41-20 catalysts were tested in the conversion, changing also the residence time. The yield of the transformation product phases was substantially influenced by the structures, at the same time the formation of the different compounds were dependent on the structures of the acidic zeolite catalysts. Oxygenated species were the main liquid product, consisting mainly of aldehydes and furfurals (glycolaldehyde, formaldehyde, acetaldehyde, furfural, 5-methylfurfural, acetic acid). The formation of the liquid products was higher over MCM-41-20 than over MCM-22-30 for all the oxygenated species except acetic acid, indicating larger formation of non-condensable products over the microporous material. By increasing the residence time the formation of acetic acid increased in transformations over MCM-22, however, such increase also led to generation of more gases with both catalysts. The deactivation due to coking was more severe over the zeolite compared to the mesoporous material. It was, however, possible to successfully regenerate the spent zeolites without changing the structure. -- Highlights: → Transformation of levoglucosan (1-6-anhdyro-β-D-glucopyranose) was done at 573 K. → MCM-22-30 and MCM-41-20 catalysts were tested. → Oxygenated species (glycolaldehyde, formaldehyde, acetaldehyde, furfural, 5-methylfurfural, acetic acid) were the main liquid products. → Acidity had an influence on product distribution and deactivation.

  4. 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)

  5. Phase separation of acetonitrile-water mixtures and minimizing of ice crystallites from there in confinement of MCM-41.

    Science.gov (United States)

    Kittaka, Shigeharu; Kuranishi, Miki; Ishimaru, Shinji; Umahara, Osamu

    2007-03-07

    The effect of confinement of an acetonitrile-water mixture, whose correlation length was comparable to the pore size of the mesopores of MCM-41 (d=2.4-3.6 nm), on the phase changes was studied. Used techniques were low temperature differential scanning calorimetry and Fourier transform infrared spectroscopy, where the phase separation, lowering of the freezing and melting temperatures, and phase transitions of the acetonitrile were detected. The latter occurred in the mesopores at temperatures similar to that of the pure liquid, while the melting temperature of the water in the mesopores<3.1 nm decreased markedly at higher acetonitrile contents, suggesting a marked lowering of ice crystallite size.

  6. Ni/Ce-MCM-41 mesostructured catalysts for simultaneous production of hydrogen and nanocarbon via methane decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Guevara, J.C.; Wang, J.A.; Chen, L.F.; Valenzuela, M.A. [ESIQIE, Instituto Politecnico Nacional, Col. Zacatenco, Av. Politecnico s/n, 07738 Mexico D. F. (Mexico); Salas, P. [Centro de Fisica Aplicada y Tecnologia Avanzada, Universidad Nacional Autonoma de Mexico, Apartado Postal 1-1010, Queretaro 76000 (Mexico); Garcia-Ruiz, A. [UPIICSA, Instituto Politecnico Nacional, Te 950 Col. Granjas-Mexico, 08400 Mexico D.F. (Mexico); Toledo, J.A.; Cortes-Jacome, M.A.; Angeles-Chavez, C. [Programa de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D. F. (Mexico); Novaro, O. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, A. P. 20-364, 01000 Mexico D.F. (Mexico)

    2010-04-15

    For the first time, simultaneous production of hydrogen and nanocarbon via catalytic decomposition of methane over Ni-loaded mesoporous Ce-MCM-41 catalysts was investigated. The catalytic performance of the Ni/Ce-MCM-41 catalysts is very stable and the reaction activity remained almost unchanged during 1400 min steam on time at temperatures 540, 560 and 580 C, respectively. The methane conversion level over these catalysts reached 60-75% with a 100% selectivity towards hydrogen. TEM observations revealed that most of the Ni particles located on the tip of the carbon nanofibers/nanotubes in the used catalysts, keeping their exposed surface clean during the test and thus remaining active for continuous reaction without obvious deactivation. Two kinds of carbon materials, graphitic carbon (C{sub g}) as major and amorphous carbon (C{sub A}) as minor were produced in the reaction, as confirmed by XRD analysis and TEM observations. Carbon nanofibers/nanotubes had an average diameter of approximately 30-50 nm and tens micrometers in length, depending on the reaction temperature, reaction time and Ni particle diameter. Four types of carbon nanofibers/nanotubes were detected and their formations greatly depend on the reaction temperature, time on steam and degree of the interaction between the metallic Ni and support. The respective mechanisms of the formation of nanocarbons were postulated and discussed. (author)

  7. Application of AlMCM-41 for competitive adsorption of methylene blue and rhodamine B: Thermodynamic and kinetic studies

    International Nuclear Information System (INIS)

    Eftekhari, S.; Habibi-Yangjeh, A.; Sohrabnezhad, Sh.

    2010-01-01

    AlMCM-41 was applied for adsorption of methylene blue (MB) and rhodamine B (RB) in single and binary component systems. In the single component systems, AlMCM-41 represents higher adsorption capacity for MB than RB with the maximal adsorption capacity of 2.08 x 10 -4 and 8.74 x 10 -5 mol/g at 25 deg. C for MB and RB, respectively. In the binary component system, MB and RB exhibit competitive adsorption onto the adsorbent. The adsorption is approximately reduced to 94 and 79% of single component adsorption systems for MB and RB (initial concentration of 8 x 10 -6 M) at 25 deg. C. In single and binary component systems, kinetic and adsorption isotherm studies demonstrate that the data are following pseudo-second-order kinetic model and Langmuir isotherm. Effect of solution pH on the adsorption in single and binary component systems was studied and the results were described by electrostatic interactions.

  8. Ordered mesoporous silica-based inorganic nanocomposites

    International Nuclear Information System (INIS)

    Wang Qingqing; Shantz, Daniel F.

    2008-01-01

    This article reviews the synthesis and characterization of nanoparticles and nanowires grown in ordered mesoporous silicas (OMS). Summarizing work performed over the last 4 years, this article highlights the material properties of the final nanocomposite in the context of the synthesis methodology employed. While certain metal-OMS systems (e.g. gold in MCM-41) have been extensively studied this article highlights that there is a rich set of chemistries that have yet to be explored. The article concludes with some thoughts on future developments and challenges in this area. - Graphical abstract: HAADF TEM image of gold nanoparticles in amine-functionalized MCM-41 (from Ref. [22])

  9. Vanadium-substituted heteropolyacids immobilized on amine- functionalized mesoporous MCM-41: A recyclable catalyst for selective oxidation of alcohols with H2O2

    International Nuclear Information System (INIS)

    Dong, Xinbo; Wang, Danjun; Li, Kebin; Zhen, Yanzhong; Hu, Huaiming; Xue, Ganglin

    2014-01-01

    Graphical abstract: Vanadium-substituted phosphotungstic acids are immobilized on amine- functionalized mesoporous MCM-41 and the hybrid catalyst is proved to be a highly efficient solid catalyst for the oxidation of aromatic alcohols to the corresponding carbonyl compounds with H 2 O 2 , featured by the high conversion and selectivity, easy recovery, and quite steady reuse. - Highlights: • Vanadium-substituted phosphotungstic acid immobilized on amine-functionalized mesoporous MCM-41 are prepared. • HPAs were fixed on the inner surface of mesoporous MCM-41 by chemical bonding to aminosilane groups. • The hybrid catalyst showed much higher catalytic activity than the pure HPAs. • The hybrid catalyst is a highly efficient recyclable solid catalyst for the selective oxidation of aromatic alcohols. - Abstract: New hybrid materials of vanadium-substituted phosphotungstic acids (VHPW) immobilized on amine-functionalized mesoporous MCM-41 (VHPW/MCM-41/NH 2 ) are prepared and characterized by FT-IR, XRD, N 2 adsorption, elemental analysis, SEM and TEM for their structural integrity and physicochemical properties. It is found that the structure of the heteropolyacids is retained upon immobilization over mesoporous materials. The catalytic activities of these hybrid materials are tested in the selective oxidation of alcohols to the carbonyl products with 30% aqueous H 2 O 2 as oxidant in toluene. The catalytic activities of different number of vanadium-substituted phosphotungstic acid are investigated, and among the catalysts, H 5 [PV 2 W 10 O 40 ] immobilized on amine-functionalized MCM-41 exhibits the highest activity with 97% conversion and 99% selectivity in the oxidation of benzyl alcohol to benzaldehyde. The hybrid catalyst is proved to be a highly efficient recyclable solid catalyst for the selective oxidation of aromatic alcohols to the corresponding aldehydes with H 2 O 2

  10. Vanadium-substituted heteropolyacids immobilized on amine- functionalized mesoporous MCM-41: A recyclable catalyst for selective oxidation of alcohols with H{sub 2}O{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Xinbo [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China); Wang, Danjun [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China); College of Chemistry Chemical Engineering, Yanan University, Shaanxi Key Laboratory of Chemical Reaction Engineering, Yan' an 716000 (China); Li, Kebin [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China); Zhen, Yanzhong [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China); College of Chemistry Chemical Engineering, Yanan University, Shaanxi Key Laboratory of Chemical Reaction Engineering, Yan' an 716000 (China); Hu, Huaiming [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China); Xue, Ganglin, E-mail: xglin707@163.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Department of Chemistry (Ministry of Education), Northwest University, Xi' an 710069 (China)

    2014-09-15

    Graphical abstract: Vanadium-substituted phosphotungstic acids are immobilized on amine- functionalized mesoporous MCM-41 and the hybrid catalyst is proved to be a highly efficient solid catalyst for the oxidation of aromatic alcohols to the corresponding carbonyl compounds with H{sub 2}O{sub 2}, featured by the high conversion and selectivity, easy recovery, and quite steady reuse. - Highlights: • Vanadium-substituted phosphotungstic acid immobilized on amine-functionalized mesoporous MCM-41 are prepared. • HPAs were fixed on the inner surface of mesoporous MCM-41 by chemical bonding to aminosilane groups. • The hybrid catalyst showed much higher catalytic activity than the pure HPAs. • The hybrid catalyst is a highly efficient recyclable solid catalyst for the selective oxidation of aromatic alcohols. - Abstract: New hybrid materials of vanadium-substituted phosphotungstic acids (VHPW) immobilized on amine-functionalized mesoporous MCM-41 (VHPW/MCM-41/NH{sub 2}) are prepared and characterized by FT-IR, XRD, N{sub 2} adsorption, elemental analysis, SEM and TEM for their structural integrity and physicochemical properties. It is found that the structure of the heteropolyacids is retained upon immobilization over mesoporous materials. The catalytic activities of these hybrid materials are tested in the selective oxidation of alcohols to the carbonyl products with 30% aqueous H{sub 2}O{sub 2} as oxidant in toluene. The catalytic activities of different number of vanadium-substituted phosphotungstic acid are investigated, and among the catalysts, H{sub 5}[PV{sub 2}W{sub 10}O{sub 40}] immobilized on amine-functionalized MCM-41 exhibits the highest activity with 97% conversion and 99% selectivity in the oxidation of benzyl alcohol to benzaldehyde. The hybrid catalyst is proved to be a highly efficient recyclable solid catalyst for the selective oxidation of aromatic alcohols to the corresponding aldehydes with H{sub 2}O{sub 2}.

  11. Study of radon transport through concrete modified with silica fume

    International Nuclear Information System (INIS)

    Chauhan, R.P.; Kumar, Amit

    2013-01-01

    The concentration of radon in soil usually varies between a few kBq/m 3 and tens or hundreds of kBq/m 3 depending upon the geographical region. This causes the transport of radon from the soil to indoor environments by diffusion and advection through the pore space of concrete. To reduce indoor radon levels, the use of concrete with low porosity and a low radon diffusion coefficient is recommended. A method of reducing the radon diffusion coefficient through concrete and hence the indoor radon concentration by using silica fume to replace an optimum level of cement was studied. The diffusion coefficient of the concrete was reduced from (1.63 ± 0.3) × 10 −7 to (0.65 ± 0.01) × 10 −8 m 2 /s using 30% substitution of cement with silica fume. The compressive strength of the concrete increased as the silica-fume content increased, while radon exhalation rate and porosity of the concrete decreased. This study suggests a cost-effective method of reducing indoor radon levels. -- Highlights: • Radon diffusion study through silica fume modified concrete was carried out. • Radon diffusion coefficient of concrete decreased with increase of silica fume contents. • Compressive strength increased with increase of silica fume. • Radon exhalation rates and porosity of samples decreased with addition of silica fume. • Radon diffusion coefficient decreased to 2.6% by 30% silica fume substitution

  12. Quick photo-Fenton degradation of phenolic compounds by Cu/Al2O3-MCM-41 under visible light irradiation: small particle size, stabilization of copper, easy reducibility of Cu and visible light active material.

    Science.gov (United States)

    Pradhan, Amaresh C; Nanda, Binita; Parida, K M; Das, Mira

    2013-01-14

    The present study reports the photo-Fenton degradation of phenolic compounds (phenol, 2-chloro-4-nitrophenol and 4-chloro-2-nitrophenol) in aqueous solution using mesoporous Cu/Al(2)O(3)-MCM-41 nanocomposite as a heterogeneous photo-Fenton-like catalyst. The in situ incorporation of mesoporous Al(2)O(3) (MA) into the framework of MCM-41 (sol-gel method) forms Al(2)O(3)-MCM-41 and wetness impregnation of Cu(II) on Al(2)O(3)-MCM-41 generates mesoporous Cu/Al(2)O(3)-MCM-41 composite. The effects of pH and H(2)O(2) concentration on degradation of phenol, 2-chloro-4-nitrophenol and 4-chloro-2-nitrophenol are studied. Kinetics analysis shows that the photocatalytic degradation reaction follows a first-order rate equation. Mesoporous 5 Cu/Al(2)O(3)-MCM-41 is found to be an efficient photo-Fenton-like catalyst for the degradation of phenolic compounds. It shows nearly 100% degradation in 45 min at pH 4. The combined effect of small particle size, stabilization of Cu(2+) on the support Al(2)O(3)-MCM-41, ease reducibility of Cu(2+) and visible light activeness are the key factors for quick degradation of phenolic compounds by Cu/Al(2)O(3)-MCM-41.

  13. Surface chemistry and catalytic properties of VOX/Ti-MCM-41 catalysts for dibenzothiophene oxidation in a biphasic system

    International Nuclear Information System (INIS)

    González, J.; Chen, L.F.; Wang, J.A.; Manríquez, Ma.; Limas, R.; Schachat, P.; Navarrete, J.; Contreras, J.L.

    2016-01-01

    Highlights: • Oxidative desulfurization of model diesel was tested in a biphasic system. • ODS activity was proportional to the V 5+ /(V 4+ + V 5+ ) values of the catalysts. • Lewis acidity was related to vanadium content and catalytic activity. • 99.9% DBT was oxidized using 25%V 2 O 5 /Ti-MCM-41 at 60 °C within 60 min. - Abstract: A series of vanadium oxide supported on Ti-MCM-41 catalysts was synthesized via the incipient impregnation method by varying the vanadia loading from 5 wt% to 10, 15, 20 and 25 wt%. These catalysts were characterized by a variety of advanced techniques for investigating their crystalline structure, textural properties, and surface chemistry information including surface acidity, reducibility, vanadium oxidation states, and morphological features. The catalytic activities of the catalysts were evaluated in a biphasic reaction system for oxidative desulfurization (ODS) of a model diesel containing 300 ppm of dibenzothiophene (DBT) where acetonitrile was used as extraction solvent and H 2 O 2 as oxidant. ODS activity was found to be proportional to the V 5+ /(V 4+ + V 5+ ) values of the catalysts, indicating that the surface vanadium pentoxide (V 2 O 5 ) was the active phase. Reaction temperature would influence significantly the ODS efficiency; high temperature, i.e., 80 °C, would lead to low ODS reaction due to the partial decomposition of oxidant. All the catalysts contained both Lewis and Brønsted acid sites but the former was predominant. The catalysts with low vanadia loading (5 or 10 wt%V 2 O 5 ) had many Lewis acid sites and could strongly adsorb DBT molecule via the electron donation/acceptance action which resulted in an inhibition for the reaction of DBT with the surface peroxometallic species. The catalyst with high vanadia loading (25wt%V 2 O 5 /Ti-MCM-41) showed the highest catalytic activity and could remove 99.9% of DBT at 60 °C within 60 min.

  14. Efficient Hydrogenolysis of Alkanes at Low Temperature and Pressure Using Tantalum Hydride on MCM-41, and a Quantum Chemical Study

    KAUST Repository

    Polshettiwar, Vivek

    2012-02-10

    Hydrogenolysis of hydrocarbons is of considerable technological importance for applications such as the hydroprocessing of petrochemical feedstocks to generate high-value and useful chemicals and fuels. We studied the catalytic activity of tantalum hydride supported on MCM-41 for the hydrogenolysis of alkanes at low temperature and low atmospheric pressure in a dynamic reactor. The reactions proceed with good turnover numbers, and the catalyst could be reused for several times, which makes the overall catalytic process sustainable. We derived the plausible mechanism by using DFT calculations and identified the preferred pathways by the analysis of potential energy surface. Our results and the proposed reaction mechanism demonstrate the viability of the "catalyst-by-design" approach. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Efficient Hydrogenolysis of Alkanes at Low Temperature and Pressure Using Tantalum Hydride on MCM-41, and a Quantum Chemical Study

    KAUST Repository

    Polshettiwar, Vivek; Pasha, Farhan Ahmad; De Mallmann, Aimery; Norsic, Sé bastien; Thivolle-Cazat, Jean; Basset, Jean-Marie

    2012-01-01

    Hydrogenolysis of hydrocarbons is of considerable technological importance for applications such as the hydroprocessing of petrochemical feedstocks to generate high-value and useful chemicals and fuels. We studied the catalytic activity of tantalum hydride supported on MCM-41 for the hydrogenolysis of alkanes at low temperature and low atmospheric pressure in a dynamic reactor. The reactions proceed with good turnover numbers, and the catalyst could be reused for several times, which makes the overall catalytic process sustainable. We derived the plausible mechanism by using DFT calculations and identified the preferred pathways by the analysis of potential energy surface. Our results and the proposed reaction mechanism demonstrate the viability of the "catalyst-by-design" approach. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Surface chemistry and catalytic properties of VOX/Ti-MCM-41 catalysts for dibenzothiophene oxidation in a biphasic system

    Science.gov (United States)

    González, J.; Chen, L. F.; Wang, J. A.; Manríquez, Ma.; Limas, R.; Schachat, P.; Navarrete, J.; Contreras, J. L.

    2016-08-01

    A series of vanadium oxide supported on Ti-MCM-41 catalysts was synthesized via the incipient impregnation method by varying the vanadia loading from 5 wt% to 10, 15, 20 and 25 wt%. These catalysts were characterized by a variety of advanced techniques for investigating their crystalline structure, textural properties, and surface chemistry information including surface acidity, reducibility, vanadium oxidation states, and morphological features. The catalytic activities of the catalysts were evaluated in a biphasic reaction system for oxidative desulfurization (ODS) of a model diesel containing 300 ppm of dibenzothiophene (DBT) where acetonitrile was used as extraction solvent and H2O2 as oxidant. ODS activity was found to be proportional to the V5+/(V4+ + V5+) values of the catalysts, indicating that the surface vanadium pentoxide (V2O5) was the active phase. Reaction temperature would influence significantly the ODS efficiency; high temperature, i.e., 80 °C, would lead to low ODS reaction due to the partial decomposition of oxidant. All the catalysts contained both Lewis and Brønsted acid sites but the former was predominant. The catalysts with low vanadia loading (5 or 10 wt%V2O5) had many Lewis acid sites and could strongly adsorb DBT molecule via the electron donation/acceptance action which resulted in an inhibition for the reaction of DBT with the surface peroxometallic species. The catalyst with high vanadia loading (25wt%V2O5/Ti-MCM-41) showed the highest catalytic activity and could remove 99.9% of DBT at 60 °C within 60 min.

  17. The performance of Ti-MCM-41 in aqueous media and after mechanical treatment studied by in situ XANES, UV/Vis and test reactions

    DEFF Research Database (Denmark)

    Hagen, Anke; Schueler, K.; Roessner, F.

    2002-01-01

    The influence of water on the epoxidation of cyclohexene with H2O2 and tert-butyl hydroperoxide (tbhp) on Ti-MCM-41 molecular sieves prepared by post-synthetic modification of the support with titanium alkoxides was investigated. The catalytic performance depends on the hydrophilicity/hydrophobic...

  18. Synthesis of an Ionic Liquid and Its Application as Template for the Preparation of Mesoporous Material MCM-41: A Comprehensive Experiment for Undergraduate Students

    Science.gov (United States)

    Hu, Jun; Yin, Jinxiang; Lin, Tianshu; Li, Guangtao

    2012-01-01

    A new solvent-free microwave experiment to synthesize the ionic liquid 1-hexadecyl-3-methylimidazolium bromide (HDMIm-Br) in high yield is presented. The structure is confirmed by IR and [superscript 1]H NMR spectra. HDMIm-Br is then used to prepare an organic-inorganic mesoporous material MCM-41. The microscopic arrangements of mesoporous…

  19. Microwave-Enhanced Sulphated Zirconia and SZ/MCM-41 Catalyzed Regioselective Synthesis of β-Amino Alcohols Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Eduardo González-Zamora

    2008-04-01

    Full Text Available A solvent-free approach for the regioselective synthesis of β-amino alcohols inshorter reaction times and higher yields, compared to conventional heating is described. Itinvolves microwave (MW exposure of undiluted reactants in the presence of sulphatedzirconia (SZ or sulphated zirconia over MCM-41 (SZM as catalyst. Both acid materialscan be easily recovered and reused.

  20. Reduction of tobacco smoke components yield in commercial cigarette brands by addition of HUSY, NaY and Al-MCM-41 to the cigarette rod.

    Science.gov (United States)

    Marcilla, A; Gómez-Siurana, A; Berenguer, D; Martínez-Castellanos, I; Beltrán, M I

    2015-01-01

    The effect of two zeolites, HUSY, NaY and a mesoporous synthesized Al-MCM-41 material on the smoke composition of ten commercial cigarettes brands has been studied. Cigarettes were prepared by mixing the tobacco with the three powdered materials, and the smoke obtained under the ISO conditions was analyzed. Up to 32 compounds were identified and quantified in the gas fraction and 80 in the total particulate matter (TPM) condensed in the cigarettes filters and in the traps located after the mouth end of the cigarettes. Al-MCM-41 is by far the best additive, providing the highest reductions of the yield for most compounds and brands analyzed. A positive correlation was observed among the TPM and nicotine yields with the reduction obtained in nicotine, CO, and most compounds with the three additives. The amount of ashes in additive free basis increases due to the coke deposited on the solids, especially with Al-MCM-41. Nicotine is reduced with Al-MCM-41 by an average of 34.4% for the brands studied (49.5% for the brand where the major reduction was obtained and 18.5 for the brand behaving the worst). CO is reduced by an average of 18.6% (ranging from 10.3 to 35.2% in the different brands).

  1. Reduction of tobacco smoke components yield in commercial cigarette brands by addition of HUSY, NaY and Al-MCM-41 to the cigarette rod

    Directory of Open Access Journals (Sweden)

    A. Marcilla

    2015-01-01

    Full Text Available The effect of two zeolites, HUSY, NaY and a mesoporous synthesized Al-MCM-41 material on the smoke composition of ten commercial cigarettes brands has been studied. Cigarettes were prepared by mixing the tobacco with the three powdered materials, and the smoke obtained under the ISO conditions was analyzed. Up to 32 compounds were identified and quantified in the gas fraction and 80 in the total particulate matter (TPM condensed in the cigarettes filters and in the traps located after the mouth end of the cigarettes. Al-MCM-41 is by far the best additive, providing the highest reductions of the yield for most compounds and brands analyzed. A positive correlation was observed among the TPM and nicotine yields with the reduction obtained in nicotine, CO, and most compounds with the three additives. The amount of ashes in additive free basis increases due to the coke deposited on the solids, especially with Al-MCM-41. Nicotine is reduced with Al-MCM-41 by an average of 34.4% for the brands studied (49.5% for the brand where the major reduction was obtained and 18.5 for the brand behaving the worst. CO is reduced by an average of 18.6% (ranging from 10.3 to 35.2% in the different brands.

  2. Activators generated by electron transfer for atom transfer radical polymerization of styrene in the presence of mesoporous silica nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Khezri, Khezrollah, E-mail: kh.khezri@ut.ac.ir [School of Chemistry, University College of Science, University of Tehran, PO Box 14155-6455, Tehran (Iran, Islamic Republic of); Roghani-Mamaqani, Hossein [Department of Polymer Engineering, Sahand University of Technology, PO Box 51335-1996, Tabriz (Iran, Islamic Republic of)

    2014-11-15

    Graphical abstract: Effect of mesoporous silica nanoparticles (MCM-41) on the activator generated by electron transfer for atom transfer radical polymerization (AGET ATRP) is investigated. Decrement of conversion and number average molecular weight and also increment of polydispersity index (PDI) values are three main results of addition of MCM-41 nanoparticles. Incorporation of MCM-41 nanoparticles in the polystyrene matrix can clearly increase thermal stability and decrease glass transition temperature of the nanocomposites. - Highlights: • Spherical morphology, hexagonal structure, and high surface area with regular pore diameters of the synthesized MCM-41 nanoparticles are examined. • AGET ATRP of styrene in the presence of MCM-41 nanoparticles is performed. • Effect of MCM-41 nanoparticles addition on the polymerization rate, conversion and molecular weights of the products are discussed. • Improvement in thermal stability of the nanocomposites and decreasing T{sub g} values was also observed by incorporation of MCM-41 nanoparticles. - Abstract: Activator generated by electron transfer for atom transfer radical polymerization was employed to synthesize well-defined mesoporous silica nanoparticles/polystyrene composites. Inherent features of spherical mesoporous silica nanoparticles were evaluated by nitrogen adsorption/desorption isotherm, X-ray diffraction and scanning electron microscopy analysis techniques. Conversion and molecular weight evaluations were carried out using gas and size exclusion chromatography respectively. By the addition of only 3 wt% mesoporous silica nanoparticles, conversion decreases from 81 to 58%. Similarly, number average molecular weight decreases from 17,116 to 12,798 g mol{sup −1}. However, polydispersity index (PDI) values increases from 1.24 to 1.58. A peak around 4.1–4.2 ppm at proton nuclear magnetic resonance spectroscopy results clearly confirms the living nature of the polymerization. Thermogravimetric

  3. Desorption Kinetics and Mechanisms of CO2 on Amine-Based Mesoporous Silica Materials

    Directory of Open Access Journals (Sweden)

    Yang Teng

    2017-01-01

    Full Text Available Tetraethylenepentamine (TEPA-based mesoporous MCM-41 is used as the adsorbent to determine the CO2 desorption kinetics of amine-modified materials after adsorption. The experimental data of CO2 desorption as a function of time are derived by zero-length column at different temperatures (35, 50, and 70 °C and analyzed by Avrami’s fractional-order kinetic model. A new method is used to distinguish the physical desorption and chemical desorption performance of surface-modified mesoporous MCM-41. The activation energy Ea of CO2 physical desorption and chemical desorption calculated from Arrhenius equation are 15.86 kJ/mol and 57.15 kJ/mol, respectively. Furthermore, intraparticle diffusion and Boyd’s film models are selected to investigate the mechanism of CO2 desorption from MCM-41 and surface-modified MCM-41. For MCM-41, there are three rate-limiting steps during the desorption process. Film diffusion is more prominent for the CO2 desorption rates at low temperatures, and pore diffusion mainly governs the rate-limiting process under higher temperatures. Besides the surface reaction, the desorption process contains four rate-limiting steps on surface-modified MCM-41.

  4. Magnetic Fe3O4@MCM-41 core-shell nanoparticles functionalized with thiol silane for efficient l-asparaginase immobilization.

    Science.gov (United States)

    Ulu, Ahmet; Noma, Samir Abbas Ali; Koytepe, Suleyman; Ates, Burhan

    2018-06-06

    l-Asparaginase (l-ASNase) is a vital enzyme for medical treatment and food industry. Here, we assessed the use of Fe 3 O 4 @Mobil Composition of Matter No. 41 (MCM-41) magnetic nanoparticles as carrier matrix for l-ASNase immobilization. In addition, surface of Fe 3 O 4 @MCM-41 magnetic nanoparticles was functionalized with 3-mercaptopropyltrimethoxysilane (MPTMS) to enhance stability of l-ASNase. The chemical structure, thermal properties, magnetic profile and morphology of the thiol-functionalized Fe 3 O 4 @MCM-41 magnetic nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), differential thermal analysis (DTA), differential scanning calorimetry (DSC), vibrating sample magnetometer (VSM), scanning electron microscope (SEM), energy dispersive X-ray (EDX) spectroscopy and zeta-potential measurement. l-ASNase was covalently immobilized onto the thiol-functionalized Fe 3 O 4 @MCM-41 magnetic nanoparticles. The properties of the immobilized enzyme, including optimum pH, temperature, kinetic parameters, thermal stability, reusability and storage stability were investigated and compared to free one. Immobilized enzyme was found to be stable over a wide range of pH and temperature range than free enzyme. The immobilized l-ASNase also showed higher thermal stability after 180 min incubation at 50 °C. The immobilized enzyme still retained 63% of its original activity after 16 times of reuse. The Km value for the immobilized enzyme was 1.15-fold lower than the free enzyme, which indicates increased affinity for the substrate. Additionally, the immobilized enzyme was active over 65% and 53% after 30 days of storage at 4 °C and room temperature (∼25 °C), respectively. Thereby, the results confirmed that thiol-functionalized Fe 3 O 4 @MCM-41 magnetic nanoparticles had high efficiency for l-ASNase immobilization and improved stability of L-ASNase.

  5. Use of TiO{sub 2}/Cr-MCM-41 molecular sieve irradiated with visible light for the degradation of thiophene in the gas phase

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Fabielle C.; Canela, Maria Cristina; Stumbo, Alexandre M. [Laboratorio de Ciencias Quimicas (LCQUI), Universidade Estadual do Norte Fluminense Darcy Ribeiro, Av. Alberto Lamego, 2000 Campos dos Goytacazes-RJ, CEP 28013-602 (Brazil)

    2008-04-15

    Photocatalytic processes using TiO{sub 2} and UV radiation to eliminate pollutants are not yet suitable for industrial facilities due to their high consumption of energy. Transition metals incorporated onto mesoporous MCM-41 molecular sieves impregnated with TiO{sub 2} constitute an alternative that allows the use of solar light. In this study, Cr-substituted MCM-41 were synthesized (Si/Cr = 100, 50 and {infinity}) and impregnated with TiO{sub 2} (10 and 20 wt.%). Raman results showed the formation of anatase. Electronic spectroscopy and EPR exposed the formation of trivalent chromium after impregnation with TiO{sub 2}, which is related to a Cr-TiO{sub 2} interaction. The synthesized photocatalysts, as well as TiO{sub 2} P25, were tested in the degradation of thiophene in gaseous phase. A test with UV lamp showed 100% of conversion for 20%TiO{sub 2}/Cr-MCM-41(100) and exceeded the activity of TiO{sub 2} P25, probably due to the higher dispersion of TiO{sub 2} on the surface of the molecular sieve. During tests using visible light and 20%TiO{sub 2}/Cr-MCM-41(50) higher conversions than those of 20%TiO{sub 2}/Cr-MCM-41(100) and TiO{sub 2} P25 were observed. These results indicate that chromium concentration is a key factor influencing the photocatalytic activity under visible light. (author)

  6. Synthesis of Nano-Zinc Oxide Loaded on Mesoporous Silica by Coordination Effect and Its Photocatalytic Degradation Property of Methyl Orange.

    Science.gov (United States)

    Shen, Zhichuan; Zhou, Hongjun; Chen, Huayao; Xu, Hua; Feng, Chunhua; Zhou, Xinhua

    2018-05-09

    Salicylaldimine-modified mesoporous silica (Sal-MCM-3 and Sal-MCM-9) was prepared through a co-condensation method with different amounts of added salicylaldimine. With the coordination from the salicylaldimine, zinc ions were impregnated on Sal-MCM-3 and Sal-MCM-9. Then, Zn-Sal-MCM-3 and Zn-Sal-MCM-9 were calcined to obtain nano-zinc oxide loaded on mesoporous silica (ZnO-MCM-3 and ZnO-MCM-9). The material structures were systematically studied by Fourier transform infrared spectroscopy (FTIR), N₂ adsorption/desorption measurements, X-ray powder diffraction (XRD), zeta potential, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet diffused reflectance spectrum (UV-vis DRS), and thermogravimetry (TGA). Methyl orange (MO) was used to investigate the photocatalysis behavior of ZnO-MCM-3 and ZnO-MCM-9. The results confirmed that nano ZnO was loaded in the channels as well as the outside surface of mesoporous silica (MCM-41). The modification of salicylaldimine helped MCM-41 to load more nano ZnO on MCM-41. When the modification amount of salicylaldimine was one-ninth and one-third of the mass of the silicon source, respectively, the load of nano ZnO on ZnO-MCM-9 and ZnO-MCM-3 had atomic concentrations of 1.27 and 2.03, respectively. ZnO loaded on ZnO-MCM-9 had a wurtzite structure, while ZnO loaded on ZnO-MCM-3 was not in the same crystalline group. The blocking effect caused by nano ZnO in the channels reduced the orderliness of MCM-41. The photodegradation of MO can be divided in two processes, which are mainly controlled by the surface areas of ZnO-MCM and the loading amount of nano ZnO, respectively. The pseudo-first-order model was more suitable for the photodegradation process.

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

    Directory of Open Access Journals (Sweden)

    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.

  8. 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

  9. A Smart pH-responsive Nano-Carrier as a Drug Delivery System: A hybrid system comprised of mesoporous nanosilica MCM-41 (as a nano-container) & a pH-sensitive polymer (as smart reversible gatekeepers): Preparation, characterization and in vitro release studies of an anti-cancer drug.

    Science.gov (United States)

    Abbaszad Rafi, Abdolrahim; Mahkam, Mehrdad; Davaran, Soodabeh; Hamishehkar, Hamed

    2016-10-10

    A smart pH-responsive drug nano-carrier for controlled release of anti-cancer therapeutics was developed through a facile route. The nano-carrier consisted of two main parts: first, the nano-container part (that mesoporous silica nanoparticles (MCM-41) were selected for this aim); and second, pH-sensitive gatekeepers (that a pH-sensitive polymer, Poly4-vinylpyridine, played this role). In the first step, MCM-41 was synthesized via template assisted sol-gel process. In the second step, polymerizable functional groups were attached onto pore entrances rather than inside walls. In the third step, polymeric gatekeepers were introduced onto pore entrances via precipitation polymerization of functionalized MCM-41 with monomers. Different methods and analysis, such as Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Powder Diffraction (XRD), Thermo-Gravimetric Analysis (TGA), Energy-Dispersive X-ray Spectroscopy (EDX), Zeta Potentials, Dynamic Light Scattering (DLS), Field Emission Scanning Electron Microscope (FE-SEM) and Transmission Electron Microscopy (TEM) were employed to approve the successful attachment of gatekeepers. Furthermore, the release studies of methotroxate (MTX), an anti-cancer drug, were performed in different media (pH4, 5.8 and 7.4) at 37±1°C. The release profiles and curves show that the release rates are completely pH-dependent and it proceeds with a decrease in pH. It is concluded that in the higher pH the gatekeepers are in their close state, but they switch to the open state as a consequence of repulsive forces between positively charged polymer chains appear in acidic media. The results suggest that this smart nano-carrier can be considered as an appropriate candidate to deliver therapeutics to cancerous tissues. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Manganese–Schiff base complex immobilized silica materials

    Indian Academy of Sciences (India)

    III)]+ and [Mn(salophen)]+: [N,N′-bis(salicylaldehyde)-1,2-phenylenediimino manganese(III)]+ were introduced into/onto the MCM-41 type silica spheres and used for the electrocatalytic reduction of oxygen. Synthesized materials were ...

  11. Dynamic filtration and static adsorption of lead ions in aqueous solution by use of blended polysulfone membranes with nano size MCM-41 particles coated by polyaniline.

    Science.gov (United States)

    Toosi, Mohammad Reza; Emami, Mohammad Reza Sarmasti; Hajian, Sudeh

    2018-05-11

    MCM-41 mesopore was prepared by hydrothermal method and used for synthesis of polyaniline/MCM-41 nanocomposite via in situ polymerization. The nanocomposite was blended with polysulfone to prepare mixed matrix membrane in different content of nanocomposite by phase inversion method. Structural and surface properties of the samples were characterized by SEM, XRD, FTIR, AFM, TGA, BET, and zeta potential measurements. Effect of the nanocomposite content on the hydrophilicity, porosity, and permeability of the membrane was determined. Membrane performance was evaluated for removal of lead ions in dynamic filtration and static adsorption. The membranes were found as effective adsorptive filters for removal of lead ions via interactions between active sites of nanocomposite in membrane structure and lead ions during filtration. Results of batch experiments proved adsorptive mechanism of membranes for removal of lead ions with the maximum adsorption capacity of 19.6 mg/g.

  12. Grafting of palladium nanoparticles onto mesoporous molecular sieve MCM-41: Heterogeneous catalysts for the formation of an N-substituted pyrrol

    Czech Academy of Sciences Publication Activity Database

    Demel, Jan; Čejka, Jiří; Bakardjieva, Snejana; Štěpnička, P.

    2007-01-01

    Roč. 263, 1-2 (2007), s. 259-265 ISSN 1381-1169 R&D Projects: GA ČR GA104/05/0192; GA MŠk(CZ) LC06070 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z40320502 Keywords : palladium * nanoparticles * MCM-41 * pyrrol * catalysis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.707, year: 2007

  13. The used of palladium nanoparticles supported on MCM-41 mesoporous molecular sieves in Heck reaction: A comparison of basic and neutral supports

    Czech Academy of Sciences Publication Activity Database

    Demel, Jan; Čejka, Jiří; Štěpnička, P.

    2007-01-01

    Roč. 274, 1-2 (2007), s. 127-132 ISSN 1381-1169 R&D Projects: GA ČR GA104/05/0192; GA MŠk(CZ) LC06070 Institutional research plan: CEZ:AV0Z40400503 Keywords : bifunctional catalysts * supported catalysts * palladium * nanoparticles * MCM-41 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.707, year: 2007

  14. Síntesis de nopol a partir de β-pineno y aceite de trementina con el catalizador Sn-MCM-41

    Directory of Open Access Journals (Sweden)

    Edwin Alarcón Durango

    2006-01-01

    Full Text Available Se obtuvo nopol mediante la reacción de Prins por condensación de β-pineno y paraformaldehído usando el catalizador Sn-MCM-41. El catalizador se sintetizó por deposición química al vapor de una sal precursora de Sn sobre MCM-41. Las reacciones se realizaron partiendo de β-pineno de alta pureza o aceite comercial de trementina. Se evaluó el efecto de varios parámetros en la selectividad a nopol, tales como: la carga de Sn en el catalizador, la cantidad de solvente y catalizador, la temperatura y el tiempo de reacción. Los catalizadores se caracterizaron por DRX, IR, UV-VIS, absorción atómica y área superficial BET. Usando Sn-MCM-41 con bajas cargas de Sn se alcanzaron rendimientos a nopol cercanos a 100% con β-pineno de alta pureza. Partiendo de trementina como fuente de β-pineno y relaciones equimolares de reactivos, se alcanzaron selectividades a nopol hasta del 93%.

  15. Copper hexacyanoferrate formation on the modified silica surface with DAB-Am-16 dendrimer

    International Nuclear Information System (INIS)

    Carmo, Devaney R. do; Gabriel Junior, Suelino; Bicalho, Urquisa O.; Paim, Leonardo L.

    2009-01-01

    The dendrimer hexadecamine poly(propylene)imine (DAB-Am-16) of third generation (G-3) was anchored on the silica gel surface. The modified silica interact easily with Cu 2+ and then with hexacyanoferrate to form copper hexacyanoferrate. The modified silica was characterized by following techniques: nuclear magnetic resonance (NMR), infrared (FTIR), energy dispersive X-ray (EDX) and cyclic voltammetry. As application of the composite obtained, the modified silica containing copper hexacyanoferrate (CuHCFSD) was tested for a voltammetric determination of nitrite using a graphite paste modified electrode. The modified graphite paste electrode can be applied also to the determination of others biological substances with success. (author)

  16. Polyacrolein/mesoporous silica nanocomposite: Synthesis, thermal stability and covalent lipase immobilization

    Energy Technology Data Exchange (ETDEWEB)

    Motevalizadeh, Seyed Farshad; Khoobi, Mehdi; Shabanian, Meisam [Department of Medicinal Chemistry, Faculty of Pharmacy and Pharmaceutical Sciences Research Center, Tehran University of Medical Sciences, Tehran 14176 (Iran, Islamic Republic of); Asadgol, Zahra; Faramarzi, Mohammad Ali [Department of Pharmaceutical Biotechnology, Faculty of Pharmacy and Biotechnology Research Center, Tehran University of Medical Sciences, P.O. Box 14155-6451, Tehran 14176 (Iran, Islamic Republic of); Shafiee, Abbas, E-mail: ashafiee@ams.ac.ir [Department of Medicinal Chemistry, Faculty of Pharmacy and Pharmaceutical Sciences Research Center, Tehran University of Medical Sciences, Tehran 14176 (Iran, Islamic Republic of); Center of Excellence in Biothermodynamics, University of Tehran, Tehran (Iran, Islamic Republic of)

    2013-12-16

    In this work, new polyacrolein/MCM-41 nanocomposites with good phase mixing behavior were prepared through an emulsion polymerization technique. Mesoporous silica was synthesized by in situ assembly of tetraethyl orthosilicate (TEOS) and cetyl trimethyl ammonium bromide (CTAB). The structure and properties of polyacrolein containing nanosized MCM-41 particle (5 and 10 wt%), were investigated by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, Dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N{sub 2} adsorption techniques, and thermogravimetric (TGA) analyses. The SEM images from the final powder have revealed good dispersion of the MCM-41 nanoparticles throughout polymeric matrix with no distinct voids between two phases. The results indicated that the thermal properties of the nanocomposite were enhanced by addition of MCM-41. Thermomyces lanuginosa lipase (TLL) was used as a model biocatalyst and successfully immobilized with polyacrolein and the nanocomposite via covalent bonds with the aldehyde groups. The activity between free enzyme, polyacrolein, and MCM-41 nanocomposite (10 wt%)-immobilized TLL was compared. The immobilized lipase with the nanocomposite shows better operational stability such as pH tolerance, thermal and storage stability. In addition, the immobilized lipase with the nanocomposite can be easily recovered and retained at 74% of its initial activity after 15 time reuses. - Graphical abstract: The influence of incorporation of mesoporous MCM-41 nanoparticle with polyacrolein on the thermal properties and enzyme immobilization was investigated. - Highlights: • Polyacrolein/MCM-41 nanocomposites were prepared by emulsion polymerization method. • Thermal stability and char residues in nanocomposites were improved. • Nanocomposites significant effects on immobilization of lipase.

  17. Preparation of Silica Modified with 2-Mercaptoimidazole and its SorptionProperties of Chromium(III

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2009-01-01

    Full Text Available Modified silica gel was prepared to remove the heavy metal of chromium(III from water sample. Silica gel was used as supporting material and the 2-mercaptoimidazole was immobilized onto surface silica so that the silica would have selective properties to adsorb the heavy metal chromium(III through the formation of coordination compound between the 2-mercaptoimidazole and chromium(III. The characterization of modified silica gel was carried out by analyzing the Fourier Transform Infrared Spectrum of this material in order to ensure the immobilization of 2-mercaptoimidazole onto the surface. The effect of pH solution, initial concentration of chromium(III, and interaction time were investigated in batch mode to find the adsorption properties of chromium(III onto modified silica. The condition optimum of these parameters was applied to determine the removal percentage of chromium(III in water sample using the modified silica gel

  18. Synthesis and application of silica gel modified with alkoxyalcohols. Alkoxyalcohol shushoku silica gel no gosei to riyo

    Energy Technology Data Exchange (ETDEWEB)

    Moriguchi, T.; Ishiguro, H.; Matsubara, Y.; Yoshihara, M.; Maeshima, T.; Ito, S. (Kinki University, Osaka (Japan). Faculty of Science and Engineering)

    1991-08-20

    Several kinds of silica gel modified by alkoxyalcohols were synthesized by refluxing and dehyration and the organic reactions were studied when these silica gels were used as the catalyst. It could be confirmed by FT-IR spectra, DTA and elementary analysis that alkoxylalcohols adhere to the surface of silica gels without any decomposition. The acetate was produced by using alkyl halides. It was found that the modified silica gels had clearly the catalytic action for the reaction with n-hexyl bromide and dibromoethane although unmodified silica gels did not show the catalytic action. The reducing reaction of carbonyl compounds was carried out. The reaction proceeded at 25 centigrade for acetophenone, cyclohexanone, 1-indanone and 2-octanone to produce the corresponding reduction products. 11 refs., 5 figs., 4 tabs.

  19. Properties of nano-silica modified pervious concrete

    Directory of Open Access Journals (Sweden)

    Bashar S. Mohammed

    2018-06-01

    Full Text Available The aim of this study is to evaluate the effects of inclusion nano-silica (also known as nano-SiO2 on the properties of pervious concrete containing fly ash (FA as a partial replacement to cement. It has been found, for cementitious paste, that incorporating NS leads to reduce the cumulative pore volume by 13.4%. While the compressive strength of NS modified pervious concrete has been improved without adversely affecting its void ratio and permeability. The workability has been adversely affected by the inclusion of NS, which can be enhanced by incorporating the fly ash and superplasticizer. The porosity of cementitious paste has increased as the FA content is increased. These results are in good agreement with SEM results. For the pervious concrete voids ratio, permeability and infiltration rate were decreased against the increase of paste to the aggregate ratio Response surface methodology (RSM has also been used to develop a model for navigating the design space of NS modified pervious concrete. Models revealed 95% significance of confidence level with difference less than 0.2 between Pred R-Squared value of 0.9515 and Adj R-Squared. The general expression has been developed for all the responses with the different coefficients using the RSM. Keywords: Fly ash, Final setting time, Infiltration rate, Pervious concrete, Nano-silica

  20. THE INFLUENCE OF Pd IMPREGNATION INTO Al-MCM-41 ON THE CHARACTERS AND ACTIVITY FOR BIOGASOLINE PRODUCTION BY CATALYTIC HYDROCRACKING OF FAMEs FROM NYAMPLUNG SEED OIL (Calophyllum Inophyllum

    Directory of Open Access Journals (Sweden)

    Hendro Juwono

    2013-08-01

    Full Text Available Biogasoline have been synthesized through catalytic hydrocracking reaction against FAMEs compounds (fatty acid methyl esters obtained from the transesterification of Nyamplung seed oil. The performance of Al-MCM-41 and Pd/Al-MCM-41 as the catalytic hydrocracking was compared. In this research, the influence of Pd impregnation into Al-MCM-41 catalyst on the characters and catalytic activity has been evaluated. The characters determined were crystallinity by using X-Ray Diffractometer (XRD, Si/Al ratio by Inductively Coupled Plasma (ICP, the acidity by pyridine adsorption, the surface area and pore volume by surface area analyzer and the morphology by Scanning Electron Microscopy (SEM. Catalytic activity was examined for hydrocracking of free fatty acid methyl esters (FAMEs produced from the transesterification of Nyamplung seed oil, by Hydrogen flowing. The research result showed that impregnation of Pd into Al-MCM-41 has been successfully carried out, which did not destroy the structural morphology of the catalyst. It was also discovered that the Pd impregnation could increase Si/Al ratio and the acidity but it leads to decrease in the catalyst surface area and the volume. Furthermore, Pd impregnated Al-MCM-41 showed superior activity compared to Al-MCM-41 for FAMEs hydrocracking. The superiority was indicated by higher effectiveness and yields selectiveness, that were 100% hydrocarbon composed of C9-C18 that was dominated by C12 emerging the gasoline fraction, compared of that by the results used Al-MCM-41 catalyst that were 97% hydrocarbon consisted of C8-C20 with equal abundance.

  1. Ruthenium-modified MCM-41 mesoporous molecular sieve and Y zeolite catalysts for selective hydrogenation of cinnamaldehyde

    Czech Academy of Sciences Publication Activity Database

    Hájek, J.; Kumar, N.; Mäki-Arvela, P.; Salmi, T.; Murzin, D. Z.; Paseka, Ivo; Heikkilä, T.; Laine, E.; Laukkanen, P.; Väyrynen, J.

    2003-01-01

    Roč. 251, č. 2 (2003), s. 385-396 ISSN 0926-860X R&D Projects: GA ČR GA104/03/0409 Institutional research plan: CEZ:AV0Z4032918 Keywords : mesoporous molecular sieve * zeolites * ruthenium Subject RIV: CA - Inorganic Chemistry Impact factor: 2.825, year: 2003

  2. Sonochemical synthesis of (3-aminopropyl)triethoxysilane-modified monodispersed silica nanoparticles for protein immobilization

    International Nuclear Information System (INIS)

    Shen, Shou-Cang; Ng, Wai Kiong; Chia, Leonard; Dong, Yuan-Cai; Tan, Reginald B.H.

    2011-01-01

    Graphical abstract: 3-Aminopropyltriethoxysilane modified monodispersed silica nanoparticles were synthesized by rapid sonochemical co-condensation to achieve high capability for protein immobilization. Highlights: → Amino-modified monodispersed silica nanoparticles were synthesized by rapid co-condensation. → Strong positive charge was created by aminopropyl-modification. → Capability for immobilization of negatively charged protein was enhanced. → Electrostatic interaction between proteins and surface contributed to the enhanced adsorption. -- Abstract: 3-Aminopropyltriethoxysilane modified monodispersed silica nanoparticles were synthesized by a rapid sonochemical co-condensation synthesis procedure. The chemical nature of surface organic modifier on the obtained modified silica nanoparticle was characterized by 13 C and 29 Si MAS Nuclear Magnetic Resonance (NMR) spectroscopies, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA)- differential scanning calorimetry (DSC). Due to the strengthened positive surface charge of the silica nanoparticles by the modification with aminopropyl groups, the capability for bovine serum albumin (BSA) adsorption was significantly increased as compared with bare silica nanoparticles. 80 mg/g BSA was adsorbed on modified silica nanoparticles, whereas only 20 mg/g BSA could be loaded on pure silica nanoparticles. The enhanced positive surface charge repelled proteins with net positive charge and the modified silica nanoparticles exhibited negligible adsorption of lysozyme, thus a selective adsorption of proteins could be achieved.

  3. Sonochemical synthesis of (3-aminopropyl)triethoxysilane-modified monodispersed silica nanoparticles for protein immobilization

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Shou-Cang, E-mail: shen_shoucang@ices.a-star.edu.sg [Institute of Chemical and Engineering Sciences, A-STAR (Agency for Science, Technology and Research), 1 Pesek Road, Jurong Island, Singapore 627833 (Singapore); Ng, Wai Kiong; Chia, Leonard; Dong, Yuan-Cai [Institute of Chemical and Engineering Sciences, A-STAR (Agency for Science, Technology and Research), 1 Pesek Road, Jurong Island, Singapore 627833 (Singapore); Tan, Reginald B.H., E-mail: reginald_tan@ices.a-star.edu.sg [Institute of Chemical and Engineering Sciences, A-STAR (Agency for Science, Technology and Research), 1 Pesek Road, Jurong Island, Singapore 627833 (Singapore); Department of Chemical and Biomolecular Engineering, The National University of Singapore, 4 Engineering Drive 4, Singapore 117576 (Singapore)

    2011-10-15

    Graphical abstract: 3-Aminopropyltriethoxysilane modified monodispersed silica nanoparticles were synthesized by rapid sonochemical co-condensation to achieve high capability for protein immobilization. Highlights: {yields} Amino-modified monodispersed silica nanoparticles were synthesized by rapid co-condensation. {yields} Strong positive charge was created by aminopropyl-modification. {yields} Capability for immobilization of negatively charged protein was enhanced. {yields} Electrostatic interaction between proteins and surface contributed to the enhanced adsorption. -- Abstract: 3-Aminopropyltriethoxysilane modified monodispersed silica nanoparticles were synthesized by a rapid sonochemical co-condensation synthesis procedure. The chemical nature of surface organic modifier on the obtained modified silica nanoparticle was characterized by {sup 13}C and {sup 29}Si MAS Nuclear Magnetic Resonance (NMR) spectroscopies, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA)- differential scanning calorimetry (DSC). Due to the strengthened positive surface charge of the silica nanoparticles by the modification with aminopropyl groups, the capability for bovine serum albumin (BSA) adsorption was significantly increased as compared with bare silica nanoparticles. 80 mg/g BSA was adsorbed on modified silica nanoparticles, whereas only 20 mg/g BSA could be loaded on pure silica nanoparticles. The enhanced positive surface charge repelled proteins with net positive charge and the modified silica nanoparticles exhibited negligible adsorption of lysozyme, thus a selective adsorption of proteins could be achieved.

  4. Electronic properties of an organic molecule within MCM-41 host: a spectroscopic and theoretical study toward elucidating the variation in band gaps of the guest species

    CERN Document Server

    Zhang, L Z; Tang Guo Qing; Liao Dai Zhen

    2003-01-01

    An organic molecule salicylidene-1,2-ethanediamine 1, has been encapsulated in the nanocavities of MCM-41 and this nanocomposite material has been investigated by X-ray diffraction, absorption and emission spectroscopy. Results from the spectroscopic measurements show that the bathochromic shift of the 0-0 transitions is correlated with the reduction of the HOMO-LUMO band gap accompanying by the energy changes of the frontier orbitals. Theoretical studies indicate that the energy levels of HOMO and LUMO increase when 1 is confined, and the HOMO is more sensitive than the LUMO.

  5. Sedimentation behaviour and colloidal properties of porous, chemically modified silicas in non-aqueous solvents

    NARCIS (Netherlands)

    Vissers, J.P.C.; Laven, J.; Claessens, H.A.; Cramers, C.A.M.G.; Agterof, W.G.M.

    1997-01-01

    The sedimentation behaviour and colloidal properties of porous, chemically modified silicas dispersed in non-aqueous solvents have been studied. The free settling behaviour of non-aggregated silica suspensions could effectively be described with a modified Stokes equation that takes into account the

  6. Extraction of metal ions using chemically modified silica gel: a PIXE analysis.

    Science.gov (United States)

    Jal, P K; Dutta, R K; Sudarshan, M; Saha, A; Bhattacharyya, S N; Chintalapudi, S N; K Mishra, B

    2001-08-30

    Organic ligand with carboxyhydrazide functional group was immobilised on the surface of silica gel and the metal binding capacity of the ligand-embedded silica was investigated. The functional group was covalently bonded to the silica matrix through a spacer of methylene groups by sequential reactions of silica gel with dibromobutane, malonic ester and hydrazine in different media. Surface area value of the modified silica was determined. The changes in surface area were correlated with the structural change of the silica surface due to chemical modifications. A mixture solution of metal ions [K(I),Cr(III),Co(II),Ni(II),Cu(II),Zn(II),Hg(II) and U(VI)] was treated with the ligand-embedded silica in 10(-3) M aqueous solution. The measurement of metal extraction capacity of the silica based ligand was done by multielemental analysis of the metal complexes thus formed by using Proton Induced X-ray Emission (PIXE) technique.

  7. Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography-mass spectrometry for the determination of antidepressant drugs in biological fluids.

    Science.gov (United States)

    Kamaruzaman, Sazlinda; Sanagi, Mohd Marsin; Yahaya, Noorfatimah; Wan Ibrahim, Wan Aini; Endud, Salasiah; Wan Ibrahim, Wan Nazihah

    2017-11-01

    A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r 2  = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. SAPO-34/AlMCM-41, as a novel hierarchical nanocomposite: preparation, characterization and investigation of synthesis factors using response surface methodology

    Science.gov (United States)

    Roohollahi, Hossein; Halladj, Rouein; Askari, Sima; Yaripour, Fereydoon

    2018-06-01

    SAPO-34/AlMCM-41, as a new hierarchical nanocomposite was successfully synthesized via hydrothermal and dry-gel conversion. In an experimental and statistical study, effect of five input parameters including synthesis period, drying temperature, NaOH/Si, water/dried-gel and SAPO% were investigated on range-order degree of mesochannels and the relative crystallinity. X-ray diffraction (XRD) patterns were recorded to characterize the ordered AlMCM-41 and crystalline SAPO-34 structures. Nitrogen adsorption-desorption technique, scanning electron microscopy (SEM), field-emission SEM (FESEM) equipped with an energy-dispersive X-ray spectroscopy (EDS-Map) and transmission electron microscopy (TEM) were used to study the textural properties, morphology and surface elemental composition. Two reduced polynomials were fitted to the responses with good precision. Further, based on analysis of variances, SAPO% and time duration of dry-gel conversion were observed as the most effective parameters on the composite structure. The hierarchical porosity, narrow pore size distribution, high external surface area and large specific pore volume were of interesting characteristics for this novel nanocomposite.

  9. Effect of SiO2/Al2O3 Ratio on Micro-Mesopore Formation for Pt/Beta-MCM-41 via NaOH Treatment and the Catalytic Performance in N-heptane Hydro isomerization

    Science.gov (United States)

    Gao, Li; Shi, Zhiyuan; Liu, Yingming; Zhao, Yuanshou; Liu, Qinghua; Xu, Chengguo; Bai, Peng; Yan, Zifeng

    2018-01-01

    Micro-mesoporous composite material Beta-MCM-41(BM) were hydrothermally synthesized by treating parent beta with molar SiO2/Al2O3 ratios of 12.5, 20 and 30 as precursors. The influence of SiO2/Al2O3 ratio of zeolite beta on effective micro-mesoporous composite formation was studied by investigating the crystallinity, morphology, chemical composition, acidity and textural property of Beta-MCM-41 through XRD, nitrogen adsorption, SEM, TEM, NH3-TPD, FTIR and Pyridine-FTIR. The catalytic performance was evaluated in terms of n-heptane hydro isomerization. The results demonstrated that Beta-MCM-41 supported Pt catalysts showed higher selectivity to isoheptanes than Pt/Beta. It was attributed to the superiorities of the pore structure and mesoporous accelerated the diffusion of larger molecules of isoheptanes.

  10. Pyrolysis of soybean oil with H-ZSM5 (Proton-exchange of Zeolite Socony Mobil 5) and MCM41 (Mobil Composition of Matter No. 41) catalysts in a fixed-bed reactor

    International Nuclear Information System (INIS)

    Ngo, Thanh-An; Kim, Jinsoo; Kim, Sun Kuk; Kim, Seung-Soo

    2010-01-01

    Soybean oil was pyrolyzed with various catalysts in a fixed-bed reactor under nitrogen flow at 420 and 450 o C. The H-ZSM5 catalysts (molar ratio SiO 2 /Al 2 O 3 = 28, 40, and 180) and 2 wt% (Ga, Al or Cu) impregnated MCM41 catalysts were used in order to investigate the effect of catalysts during the pyrolysis process. The gas products in all experiments were mainly methane, ethane and propylene. The liquid products in the presence of H-ZSM5 catalysts were mainly aromatic components while those with metal/MCM41 catalysts were a mixture of alkanes, alkenes, alkadienes, aromatic and carboxylic acids. The highest coke yield of 4.4 wt% was obtained with Ga/MCM41 catalyst at the pyrolysis temperature of 420 o C. The effect of catalysts on product yield and composition was systematically investigated.

  11. Utilization of a by-product produced from oxidative desulfurization process over Cs-mesoporous silica catalysts.

    Science.gov (United States)

    Kim, Hyeonjoo; Jeong, Kwang-Eun; Jeong, Soon-Yong; Park, Young-Kwon; Kim, Do Heui; Jeon, Jong-Ki

    2011-02-01

    We investigated the use of Cs-mesoporous silica catalysts to upgrade a by-product of oxidative desulfurization (ODS). Cs-mesoporous silica catalysts were characterized through N2 adsorption, XRD, CO2-temperature-programmed desorption, and XRF. Cs-mesoporous silica prepared by the direct incorporation method showed higher catalytic performance than a Cs/MCM-41 catalyst by impregnation method for the catalytic decomposition of sulfone compounds produced from ODS process.

  12. Structural evolution of silica sols modified with formamide

    Directory of Open Access Journals (Sweden)

    Lenza R.F.S.

    2001-01-01

    Full Text Available In this work we investigated the influence of formamide on the acid-catalyzed sol-gel process by Fourier transform infrared spectroscopy (FTIR. Three silica sols were studied: Sol catalyzed with nitric acid without formamide, sol catalyzed with nitric acid containing formamide and sol catalyzed with a mixture of nitric acid and hydrofluoric acid and modified with formamide. Following the time evolution of both the Si-(OH stretching vibration at around 950 cm-1 and the Si-O-(Si vibration between 1040 cm-1 and 1200 cm-1 we were able to describe the structural evolution of each sol. The curve of evolution of Si-(OH stretching vibration corresponding to sol A has a simple asymptotic evolution. In the case of formamide containing sol, we observed a two-step structural evolution indicating that for the system containing formamide the polymerization goes through a temporary stabilization of oligomers, which can explain the non-variation of the Si-O(H bond wavenumber for a certain time. Gelation times were of several days for gels without formamide and few hours for gels containing additive. The presence of additive resulted in a highly interconnected gel.

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

    KAUST Repository

    Patil, Umesh; Fihri, Aziz; Emwas, Abdul-Hamid M.; Polshettiwar, Vivek

    2012-01-01

    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

  14. Surface chemistry and catalytic properties of VO{sub X}/Ti-MCM-41 catalysts for dibenzothiophene oxidation in a biphasic system

    Energy Technology Data Exchange (ETDEWEB)

    González, J. [ESIQIE, Instituto Politécnico Nacional, Av. Instituto Politécnico Nacional s/n, 07738 Col. Zacatenco, Mexico City (Mexico); Chen, L.F., E-mail: lchen@ipn.mx [ESIQIE, Instituto Politécnico Nacional, Av. Instituto Politécnico Nacional s/n, 07738 Col. Zacatenco, Mexico City (Mexico); Wang, J.A.; Manríquez, Ma.; Limas, R. [ESIQIE, Instituto Politécnico Nacional, Av. Instituto Politécnico Nacional s/n, 07738 Col. Zacatenco, Mexico City (Mexico); Schachat, P.; Navarrete, J. [Dirección de Investigación, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F. (Mexico); Contreras, J.L. [Laboratorio de Catálisis y Polímeros, División de Ciencias Básicas e Ingeniería, Universidad Autónoma Metropolitana-A, Av. San Pablo No. 180, 02200 México D.F. (Mexico)

    2016-08-30

    Highlights: • Oxidative desulfurization of model diesel was tested in a biphasic system. • ODS activity was proportional to the V{sup 5+}/(V{sup 4+} + V{sup 5+}) values of the catalysts. • Lewis acidity was related to vanadium content and catalytic activity. • 99.9% DBT was oxidized using 25%V{sub 2}O{sub 5}/Ti-MCM-41 at 60 °C within 60 min. - Abstract: A series of vanadium oxide supported on Ti-MCM-41 catalysts was synthesized via the incipient impregnation method by varying the vanadia loading from 5 wt% to 10, 15, 20 and 25 wt%. These catalysts were characterized by a variety of advanced techniques for investigating their crystalline structure, textural properties, and surface chemistry information including surface acidity, reducibility, vanadium oxidation states, and morphological features. The catalytic activities of the catalysts were evaluated in a biphasic reaction system for oxidative desulfurization (ODS) of a model diesel containing 300 ppm of dibenzothiophene (DBT) where acetonitrile was used as extraction solvent and H{sub 2}O{sub 2} as oxidant. ODS activity was found to be proportional to the V{sup 5+}/(V{sup 4+} + V{sup 5+}) values of the catalysts, indicating that the surface vanadium pentoxide (V{sub 2}O{sub 5}) was the active phase. Reaction temperature would influence significantly the ODS efficiency; high temperature, i.e., 80 °C, would lead to low ODS reaction due to the partial decomposition of oxidant. All the catalysts contained both Lewis and Brønsted acid sites but the former was predominant. The catalysts with low vanadia loading (5 or 10 wt%V{sub 2}O{sub 5}) had many Lewis acid sites and could strongly adsorb DBT molecule via the electron donation/acceptance action which resulted in an inhibition for the reaction of DBT with the surface peroxometallic species. The catalyst with high vanadia loading (25wt%V{sub 2}O{sub 5}/Ti-MCM-41) showed the highest catalytic activity and could remove 99.9% of DBT at 60 °C within 60 min.

  15. Improvement of thermal stability of UV curable pressure sensitive adhesive by surface modified silica nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pang, Beili; Ryu, Chong-Min; Kim, Hyung-Il, E-mail: hikim@cnu.ac.kr

    2013-11-01

    Highlights: • Silica nanoparticles were modified to carry the vinyl groups for photo-crosslinking. • Acrylic copolymer was modified to have the vinyl groups for photo-crosslinking. • Strong and extensive interfacial bondings were formed between polymer and silica. • Thermal stability of PSA was improved by forming nanocomposite with modified silica. -- Abstract: Pressure sensitive adhesives (PSAs) with higher thermal stability were successfully prepared by forming composite with the silica nanoparticles modified via reaction with 3-methacryloxypropyltrimethoxysilane. The acrylic copolymer was synthesized as a base resin for PSAs by solution polymerization of 2-EHA, EA, and AA with AIBN as an initiator. The acrylic copolymer was further modified with GMA to have the vinyl groups available for UV curing. The peel strength decreased with the increase of gel content which was dependent on both silica content and UV dose. Thermal stability of the composite PSAs was improved noticeably with increasing silica content and UV dose mainly due to the strong and extensive interfacial bonding between the organic polymer matrix and silica.

  16. Multifunctional Silica Nanoparticles Modified via Silylated-Decaborate Precursors

    Directory of Open Access Journals (Sweden)

    Fatima Abi-Ghaida

    2015-01-01

    Full Text Available A new class of multifunctional silica nanoparticles carrying boron clusters (10-vertex closo-decaborate and incorporating luminescent centers (fluorescein has been developed as potential probes/carriers for potential application in boron neutron capture therapy (BNCT. These silica nanoparticles were charged in situ with silylated-fluorescein fluorophores via the Stöber method and their surface was further functionalized with decaborate-triethoxysilane precursors. The resulting decaborate dye-doped silica nanoparticles were characterized by TEM, solid state NMR, DLS, nitrogen sorption, elemental analysis, and fluorescence spectroscopy.

  17. Efficacy of Nanoencapsulated Thymus eriocalyx and Thymus kotschyanus Essential Oils by a Mesoporous Material MCM-41 Against Tetranychus urticae (Acari: Tetranychidae).

    Science.gov (United States)

    Ebadollahi, Asgar; Sendi, Jalal Jalali; Aliakbar, Alireza

    2017-12-05

    Inspite of well-established potentiality of plant essential oils as biopesticides, their environmentally low persistence is considered as a hindering obstacle for its commercialization. In the present study, chemical composition and toxicity of essential oils isolated from leaves of Thymus eriocalyx and Thymus kotschyanus were evaluated against two-spotted spider mite, Tetranychus urticae. The chemicals present in the crude oil were found to be thymol (28.83%), oleic acid (11.51%), palmitic acid (8.60%), borneol (5.72%), ρ-cymene (3.60%), and 1,8-cineole (3.57%) in the essential oil of T. eriocalyx, and camphene (35.59%), linalyl acetate (20.47%), linalool (14.75%), α-terpineol (13.87%), and geranyl acetate (3.07%) in the essential oil of T. kotschyanus. The essential oils had strong fumigant toxicity on the adult females of Te. urticae and their fumigation persistence was prolonged until 6 and 5 d, respectively, for T. eriocalyx and T. kotschyanus. Loading of essential oils in MCM-41 increased their stability and persistence was extended up to 20 and 18 d for T. eriocalyx and T. kotschyanus. Further, mite mortality increased from 80 to 203 mites by T. eriocalyx and from 58 to 186 mites by T. kotschyanus nanoencapsulated essential oils. Based on these results, nanoencapsulation of T. eriocalyx and T. kotschyanus essential oils in MCM-41 may be a useful method for their application in the management of Te. urticae. © The Author(s) 2017. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  18. A Clean, Mild, and Efficient Preparation of Aryl 14H-benzo[a,j]xanthene leuco-dye Derivatives Via Nanocatalytic MCM-41-SO3H Under Ultrasonic Irradiation in Aqueous Media.

    Science.gov (United States)

    Fathollahi, Mostafa; Rostamizadeh, Shahnaz; Amani, Ali M

    2018-01-01

    The present study has developed an efficient and eco-friendly protocol for the synthesis of aryl-14-H-dibenzo[a,j] xanthenes through a one-pot condensation reaction of 2-naphthol and arylaldehydes in aqueous media using the nanocatalytic MCM-41-SO3H under ultrasonic illumination. Using SEM and XRD analyses, MCM-41-SO3H nanoparticles were characterized. Therefore, for high magnification, taking the SEM image, the mesoporous surface of MCM-41-SO3H nanoparticles coated with gold for 2 minutes was characterized. Moreover, at a scan rate of 0.02° (2θ)/sec, XRD analysis from 1.5° (2θ) to 10.0° (2θ) was performed. For our considered sample, some well-ordered XRD patterns with one main peak as well as three minor peaks equal to those of MCM-41 materials were observed. The suggested route demonstrates very promising properties like higher yields, decrease in the time of reaction (5-10 min), mild and straightforward conditions, low level of toxicity, and inclusion of a cost-efficient and ecofriendly catalyst having considerable reusability. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  19. Ordered Functionalized Silica Materials with High Proton Conductivity

    Czech Academy of Sciences Publication Activity Database

    Marschall, R.; Rathouský, Jiří; Wark, M.

    2007-01-01

    Roč. 19, č. 26 (2007), s. 6401-6407 ISSN 0897-4756 R&D Projects: GA MŠk 1M0577 Grant - others:Deutsche Forschungsgemeinschaft(DE) CA 147/13-1, SPP1181 Institutional research plan: CEZ:AV0Z40400503 Source of funding: R - rámcový projekt EK Keywords : silica * high proton conductivity * Si-MCM-41 Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.883, year: 2007

  20. MCM-41 support for ultrasmall gamma-Fe2O3 nanoparticles for H2S removal

    Czech Academy of Sciences Publication Activity Database

    Cara, C.; Rombi, E.; Musinu, A.; Mameli, V.; Ardu, A.; Angotzi, M. S.; Atzori, L.; Nižňanský, Daniel; Xin, H. L.; Cannas, C.

    2017-01-01

    Roč. 5, č. 41 (2017), s. 21688-21698 ISSN 2050-7488 Institutional support: RVO:61388980 Keywords : Nano-sized particles * mesoporous silica nanoparticles * oxide sorbents Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 8.867, year: 2016

  1. Antidegradation and reinforcement effects of phenyltrimethoxysilane- or N-[3-(trimethoxysilyl)propyl]aniline-modified silica particles in natural rubber composites

    Energy Technology Data Exchange (ETDEWEB)

    Tunlert, Apinya [Program in Petrochemistry and Polymer Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Center for Petroleum, Petrochemical and Advanced Material, Chulalongkorn University Bangkok 10330 (Thailand)

    2016-04-15

    The modification of silica particles with phenyltrimethoxysilane or N-[3-(trimethoxysilyl)propyl]aniline via a sol–gel reaction was performed in order to improve the dispersion of silica and antidegradation in natural rubber (NR). The functional groups on the modified silica surface were characterized by Fourier transform infrared spectroscopy, while the morphology was evaluated by scanning and transmission electron microscopy. The surface properties and antioxidant activity of the modified silica particles were determined by the water contact angle and 2, 2-diphenyl-1-picrylhydrazyl assay, respectively. The modified silica particles exhibited a higher hydrophobicity and a decreased interfacial adhesion energy compared with the unmodified silica particles. The modified silica particles were then incorporated into NR. The better dispersion of the modified silica particles than the unmodified ones in the NR matrix resulted in improved mechanical properties in terms of the modulus at 300% elongation (2.9 ± 0.02 MPa), hardness (52.5 ± 0.2 Shore A), abrasion resistance (241 ± 8 mm{sup 3}) and compression set (20.2 ± 0.6%). In addition, the inclusion of the modified silica particles in the NR matrix gave a high initial temperature of decomposition and retarded the ozone-induced degradation compared with the NR filled with unmodified silica particles. - Highlights: • Silica was surface modified with PhTMS or ATMS via a sol–gel reaction. • Modified silica showed a decreased interfacial adhesion energy. • Modified silica showed an enhanced free radical scavenging activity. • Modified silica improved the mechanical properties, thermal stability and ozone resistance in NR vulcanizates.

  2. On the PEEK composites reinforced by surface-modified nano-silica

    International Nuclear Information System (INIS)

    Lai, Y.H.; Kuo, M.C.; Huang, J.C.; Chen, M.

    2007-01-01

    The nano-sized silica fillers reinforced poly(ether ether ketone) (PEEK) composites were fabricated by means of compression molding technique. The nano-sized silica, measuring 30 nm in size, was firstly modified by surface pretreatment with stearic acid. The performances and properties of the resulting PEEK/SiO 2 nanocomposites were examined in terms of tensile loading, hardness, dynamic mechanical analysis (DMA), thermomechanical analysis (TMA), thermogravimetry analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The modified nano-silica was seen to disperse more uniformly than the unmodified counterpart. The XRD patterns of the modified silica reinforced PEEK composites reveal a systematic shift toward higher angles, suggesting the smaller d-spacing of the PEEK crystallites. The coefficient of thermal expansion (CTE) becomes lowered when the content of the nano-silica increases. Furthermore, the CTE of the modified silica filled PEEK nanocomposites shows the higher CTE values. A logic model is proposed. The increment of the dynamic modulus for the PEEK nanocomposites is up to 40% at elevated temperatures from 100 to 250 deg. C, indicating the apparent improvement of elevated temperature mechanical properties

  3. Effect of nano silica based modifying agent for hydrophobic coating application

    International Nuclear Information System (INIS)

    Nurul Huda Mudri; Nik Ghazali Nik Salleh; Mek Zah Salleh

    2016-01-01

    Hydrophobic coatings find wide application in industry due to their unique features such as water repellent and self-cleaning properties. In this study, modifying agent was synthesized by way of nano silica particles dispersion in polydimethyl siloxane with addition of surfactant, catalyst and stabilizer using high speed distemper. The modifying agent was added into coating formulation and cured under UV exposure. Scanning Electron Microscopy image of the film found that the nano silica particles were distributed well on substrate. Contact angle measurement gave the highest reading of 116 degree for 20 % wt of the modifying agent. The optical properties of the film were evaluated via transmission and haze test. (author)

  4. Surface modification to produce hydrophobic nano-silica particles using sodium dodecyl sulfate as a modifier

    Energy Technology Data Exchange (ETDEWEB)

    Qiao, Bing; Liang, Yong; Wang, Ting-Jie, E-mail: wangtj@tsinghua.edu.cn; Jiang, Yanping

    2016-02-28

    Graphical abstract: Nano silica particle was modified to produce hydrophobic surface with contact angle of 107° using the water soluble SDS as a modifier through a new route. The grafted density reached 1.82–2 nm. Brønsted acid sites supply proton to react with SDS via generating carbocation, forming a Si–O–C structure. - Highlights: • Silica was modified to produce hydrophobic surface using SDS as modifier. • The route is free of organic solvent and gets perfect contact of SDS and silica. • Contact angle of modified silica particles reached 107°. • Grafted density on the silica surface reached 1.82 SDS nm{sup −2}. • Brønsted acid sites supply proton to react with SDS via generating carbocation. - Abstract: Hydrophobic silica particles were prepared using the surfactant sodium dodecyl sulfate (SDS) as a modifier by a new route comprising three processes, namely, aqueous mixing, spray drying and thermal treatment. Since SDS dissolves in water, this route is free of an organic solvent and gave a perfect dispersion of SDS, that is, there was excellent contact between SDS and silica particles in the modification reaction. The hydrophobicity of the modified surface was verified by the contact angle of the nano-sized silica particles, which was 107°. The SDS grafting density reached 1.82 nm{sup −2}, which is near the highest value in the literature. The optimal parameters of the SDS/SiO{sub 2} ratio in the aqueous phase, process temperature and time of thermal treatment were determined to be 20%, 200 °C and 30 min, respectively. The grafting mechanism was studied by comparing the modification with that on same sized TiO{sub 2} particles, which indicated that the protons of the Brønsted acid sites on the surface of SiO{sub 2} reacted with SDS to give a carbocation which then formed a Si–O–C structure. This work showed that the hydrophilic surface of silica can be modified to be a hydrophobic surface by using a water soluble modifier SDS in a

  5. Environmentally responsive surface-modified silica nanoparticles for enhanced oil recovery

    International Nuclear Information System (INIS)

    Behzadi, Abed; Mohammadi, Aliasghar

    2016-01-01

    Environmentally responsive surface-modified nanoparticles are colloidal nanoparticles coated with, at least, two physicochemically distinct surface groups. Recent advances in the synthesis and production of nanoparticles have enabled the production of environmentally responsive surface-modified nanoparticles with both hydrophilic and hydrophobic surface groups. These nanoparticles act like colloidal surfactants. In this paper, environmentally responsive surface-modified silica nanoparticles are synthesized and used for enhancement of oil recovery. For this purpose, silica nanoparticles are coated with polyethylene glycol chains as hydrophilic agent and propyl chains as hydrophobic agent at various quantities, and their ability to modulate oil–water interface properties and oil recovery is examined. Oil–water interfacial tension and water surface tension are decreased by 50 % in the presence of silica nanoparticles coated with both agents. Measuring oil-drop contact angle on oil-wetted glass slides and carbonate rock sections, after aging in various surface-modified silica nanofluids, indicates that the wettability of various oil-wetted surfaces is modified from strongly oil-wet to water-wet. Flooding nanofluids to glass micro-models and pore-level investigations demonstrate that surface modification of silica nanoparticles, specially, with both hydrophilic and hydrophobic agents improves considerably their performance in increasing oil recovery and wettability alteration.

  6. Environmentally responsive surface-modified silica nanoparticles for enhanced oil recovery

    Energy Technology Data Exchange (ETDEWEB)

    Behzadi, Abed; Mohammadi, Aliasghar, E-mail: amohammadi@sharif.edu [Sharif University of Technology, Department of Chemical and Petroleum Engineering (Iran, Islamic Republic of)

    2016-09-15

    Environmentally responsive surface-modified nanoparticles are colloidal nanoparticles coated with, at least, two physicochemically distinct surface groups. Recent advances in the synthesis and production of nanoparticles have enabled the production of environmentally responsive surface-modified nanoparticles with both hydrophilic and hydrophobic surface groups. These nanoparticles act like colloidal surfactants. In this paper, environmentally responsive surface-modified silica nanoparticles are synthesized and used for enhancement of oil recovery. For this purpose, silica nanoparticles are coated with polyethylene glycol chains as hydrophilic agent and propyl chains as hydrophobic agent at various quantities, and their ability to modulate oil–water interface properties and oil recovery is examined. Oil–water interfacial tension and water surface tension are decreased by 50 % in the presence of silica nanoparticles coated with both agents. Measuring oil-drop contact angle on oil-wetted glass slides and carbonate rock sections, after aging in various surface-modified silica nanofluids, indicates that the wettability of various oil-wetted surfaces is modified from strongly oil-wet to water-wet. Flooding nanofluids to glass micro-models and pore-level investigations demonstrate that surface modification of silica nanoparticles, specially, with both hydrophilic and hydrophobic agents improves considerably their performance in increasing oil recovery and wettability alteration.

  7. 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.

  8. Tetragonal zirconia quantum dots in silica matrix prepared by a modified sol-gel protocol

    Science.gov (United States)

    Verma, Surbhi; Rani, Saruchi; Kumar, Sushil

    2018-05-01

    Tetragonal zirconia quantum dots (t-ZrO2 QDs) in silica matrix with different compositions ( x)ZrO2-(100 - x)SiO2 were fabricated by a modified sol-gel protocol. Acetylacetone was added as a chelating agent to zirconium propoxide to avoid precipitation. The powders as well as thin films were given thermal treatment at 650, 875 and 1100 °C for 4 h. The silica matrix remained amorphous after thermal treatment and acted as an inert support for zirconia quantum dots. The tetragonal zirconia embedded in silica matrix transformed into monoclinic form due to thermal treatment ≥ 1100 °C. The stability of tetragonal phase of zirconia is found to enhance with increase in silica content. A homogenous dispersion of t-ZrO2 QDs in silica matrix was indicated by the mapping of Zr, Si and O elements obtained from scanning electron microscope with energy dispersive X-ray analyser. The transmission electron images confirmed the formation of tetragonal zirconia quantum dots embedded in silica. The optical band gap of zirconia QDs (3.65-5.58 eV) was found to increase with increase in zirconia content in silica. The red shift of PL emission has been exhibited with increase in zirconia content in silica.

  9. Structural changes in femtosecond laser modified regions inside fused silica

    International Nuclear Information System (INIS)

    Juodkazis, Saulius; Kohara, Shinji; Ohishi, Yasuo; Hirao, Norihisa; Vailionis, Arturas; Mizeikis, Vygantas; Saito, Akira; Rode, Andrei

    2010-01-01

    Structural characterization of photomodified microvolumes formed by tightly focused femtosecond laser pulses inside silica glass was carried out using synchrotron x-ray diffraction. The observed distinct separation between the O–O and Si–Si pair correlation peaks can be interpreted as a phase separation induced by microexplosions at the focal volume. The mechanisms of structural transitions induced by femtosecond laser pulses inside dielectrics are discussed

  10. Influence of surface modified nano silica on alkyd binder before and after accelerated weathering

    DEFF Research Database (Denmark)

    Nikolic, Miroslav; Nguyen, Hiep Dinh; Daugaard, Anders Egede

    2016-01-01

    Introduction of nano fillers in exterior wood coatings is not straight forward. Influence on aging of polymer binder needs to be taken into account along with possible benefits that nano fillers can provide immediately after application. This study shows the influence of two differently modified...... hydrophobic nano silica on an alkyd binder for exterior wood coatings. One month after application, the highest strength and energy required to break the films was obtained with addition of 3% disilazane modified silica. Changes in tensile properties were accompanied with a small increase in glass transition...

  11. Solid State NMR Characterization of Ibuprofen:Nicotinamide Cocrystals and New Idea for Controlling Release of Drugs Embedded into Mesoporous Silica Particles.

    Science.gov (United States)

    Skorupska, Ewa; Kaźmierski, Sławomir; Potrzebowski, Marek J

    2017-05-01

    Grinding and melting methods were employed for synthesis of pharmaceutical cocrystals formed by racemic (R/S) and entiomeric (S) ibuprofen (IBU) and nicotinamide (NA) as coformer. Obtained (R/S)-IBU:NA and (S)-IBU:NA cocrystals were fully characterized by means of advanced one- and two-dimensional solid state nuclear magnetic resonance (SS NMR) techniques with very fast magic angle spinning (MAS) at 60 kHz. The distinction in molecular packing and specific hydrogen bonding pattern was clearly recognized by analysis of 1 H, 13 C, and 15 N spectra. It is concluded from these studies that both methods (grinding and melting) provide exactly the same, specific forms of cocrystals. Thermal solvent-free (TSF) approach was used for loading of (R/S)-IBU:NA and (S)-IBU:NA into the pores of MCM-41 mesoporous silica particle (MSP). The progress and efficiency of this process was analyzed by NMR spectroscopy. It has been confirmed that TSF method is an effective and safe technique of filling the MSP pores with active pharmaceutical ingredients (APIs). By analyzing the NMR results, it has been further proved that excess of IBU and NA components, which are not embedded into the pores during melting and cooling, crystallize on the MCM-41 walls preserving very specific arrangement, characteristic for crystalline samples. By investigating kinetic of release for (R/S)-IBU/MCM-41, (S)-IBU:NA/MCM-41, and (R/S)-IBU:NA/MCM-41 samples containing active components exclusively inside of the pores, it was revealed that release of IBU is much faster for the first of the samples compared to those containing IBU and NA inside the pores. The hypothesis that the rate of release of API can be controlled by specific composition of cocrystal embedded into the MSP pore was further supported by study of (R/S)-IBU:BA/MCM-41 sample with benzoic acid (BA) as coformer.

  12. Effect of Mesoporous Silica and Hydroxyapatite Nanoparticles on the Tensile and Dynamic Mechanical Thermal Properties of Polypropylene and Polypropylene Foam

    Directory of Open Access Journals (Sweden)

    Alireza Albooyeh

    2014-12-01

    Full Text Available The main purpose of this paper is the experimental study on the tensile and dynamic - mechanical thermal properties of polypropylene (PP and polypropylene foam reinforced with mesoporous silica (MCM-41, hydroxyapatite (HA and the composite of mesoporous silica and hydroxyapatite (MCM41-HA nanoparticles. Nanocomposites and nanocomposite foams containing PP, maleic anhydride grafted polypropylene, different nanoparticles and chemical blowing agent (for foam samples are mixed using the melt-compounding technique in a twin-screw extruder. The results of the tests show that at the same nanoparticles content, all the nanofillers cause better mechanical properties than neat PP and PP foam. Also, due to the porous structure of the foam samples, these samples have the higher damping characteristics and lower tensile properties than the solid samples. Because of higher rigidity and higher strength of HA nanoparticles, the greatest increase in modulus and tensile strength occurs by adding these nanoparticles to neat PP and PP foam. The highest damping factor is obtained by adding MCM-41-HA nanoparticles to PP and PP foam, because of the porous nature of the MCM-41 particles which were reinforced by HA particles. The results of differential scanning calorimetry show that the addition of different nanoparticles does not have any significant effect on crystallinity and melting behavior of PP. Scanning electron microscopy images show that the nanomaterials were fine and uniformly dispersed within the polymer matrix. Furthermore, the addition of different nanoparticles to PP foam causes to increase the cell density, to reduce the cell sizes and to improve the cell sizes distribution. In this respect, the lowest cell sizes and the highest cell density are created by adding HA and MCM41-HA  nanopaticles to PP foams.

  13. Aliphatic Hydrocarbons from Lignocellulose by Pyrolysis over Cesium-Modified Amorphous Silica Alumina Catalysts

    NARCIS (Netherlands)

    Zabeti, M.; Sai Sankar Gupta, Karthick Babu; Raman, G.; Lefferts, Leon; Schallmoser, Stefan; Lercher, Johannes A.; Seshan, K.

    2015-01-01

    Cesium-modified amorphous silica alumina (Cs/ASA) is a promising catalyst for the production of hydrocarbons through pyrolysis of biomass. Catalytic pyrolysis of pinewood over Cs/ASA in a pyrolyzer system in conjunction with a gas chromatograph and mass spectrometer resulted in a 22% yield of

  14. STABLE SILICA-GRAFTED POLYMER-BOUND BULKY-PHOSPHITE MODIFIED RHODIUM HYDROFORMYLATION CATALYSTS

    NARCIS (Netherlands)

    JONGSMA, T; VANAERT, H; FOSSEN, M; CHALLA, G; VANLEEUWEN, PWNM

    1993-01-01

    The present study demonstrates that silica-grafted polymer-bound phosphite modified rhodium complexes can be used in continuous flow reactors. The hydroformylation of styrene was carried out at moderate pressure (p(CO/H-2) = 30 bar) and temperature (T = 100-degrees-C), yielding constant conversions

  15. Separation of metronidazole, its major metabolites and their conjugates using dynamically modified silica

    DEFF Research Database (Denmark)

    Thomsen, U. G.; Cornett, Claus; Tjornelund, J.

    1995-01-01

    -performance liquid chromatographic (HPLC) system for the simultaneous determination of metronidazole, its major metabolites and their glucuronic acid conjugates in biological fluids. The separation is performed using bare silica dynamically modified with N-cetyl-N,N,N-trimethylammonium bromide contained...

  16. Mesoporous silica obtained with methyltriethoxysilane as co-precursor in alkaline medium

    Czech Academy of Sciences Publication Activity Database

    Putz, A.-M.; Wang, K.; Len, A.; Plocek, Jiří; Bezdička, Petr; Kopitsa, G. P.; Khamova, T. V.; Ianasi, C.; Sacarescu, L.; Mitróová, Z.; Savii, C.; Yan, M.; Almásy, L.

    2017-01-01

    Roč. 424, SI 3 (2017), s. 275-281 ISSN 0169-4332. [International Conference on Physics of Advanced Materials (ICPAM) /9./. Cluj Napoca, 08.09.2016-14.09.2016] Institutional support: RVO:61388980 Keywords : Sol-gel process * mtes/teos * Hydrophobic silica * mcm-41 Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 3.387, year: 2016

  17. Chemical composition of silica-based biocidal modifier

    Directory of Open Access Journals (Sweden)

    Grishina Anna Nikolaevna

    2016-11-01

    Full Text Available Increase of the amount of fungi spores and micotixines causes the increase in the number of different diseases. Because of this, ensuring the biological safety in buildings is becoming more and more important today. The preferred way to guarantee the biological safety of a building is to employ modern building materials that prevent the settlement of the fungi colonies on the inner surfaces of walls. Such building materials can be produced using novel biocidal modifiers that allow controlling the number of microorganisms on the surface and in the bulk of a composite construction. The precipitation product of zinc hydrosilicates and sodium sulfate is one of the mentioned modifiers. Till now, the exact chemical composition of such precipitation product is controversial; it is obvious, though, that the efficacy of the biocidal modifier is mostly determined by the type of the copper compounds. In the present work an integrated approach is used for the investigation of the chemical composition of the biocidal modifier. Such an approach consists in the examination of the modifier’s composition by means of different, yet complementary, research methods: X-ray diffraction, infrared spectroscopy and DTA. It is shown that the chemical composition of the modifier mainly depends on the amount of precipitant. X-ray diffraction reveals that the major part of the modifier is represented by amorphous phase. Along with the increase of the precipitant’s amount the crystalline phase Zn4SO4(OH6•xH2O formation takes place. Such a crystalline phase is not appropriate as a component of the biocidal modifier. Another two methods - DTA and IR spectroscopy - reveal that the amorphous phase consists essentially of zinc hydrosilicates.

  18. Vulcanization characteristics and dynamic mechanical behavior of natural rubber reinforced with silane modified silica.

    Science.gov (United States)

    Chonkaew, Wunpen; Minghvanish, Withawat; Kungliean, Ulchulee; Rochanawipart, Nutthaya; Brostow, Witold

    2011-03-01

    Two silane coupling agents were used for hydrolysis-condensation reaction modification of nanosilica surfaces. The surface characteristics were analyzed using Fourier transform infrared spectroscopy (FTIR). The vulcanization kinetics of natural rubber (NR) + silica composites was studied and compared to behavior of the neat NR using differential scanning calorimetry (DSC) in the dynamic scan mode. Dynamic mechanical analysis (DMA) was performed to evaluate the effects of the surface modification. Activation energy E(a) values for the reaction are obtained. The presence of silica, modified or otherwise, inhibits the vulcanization reaction of NR. The neat silica containing system has the lowest cure rate index and the highest activation energy for the vulcanization reaction. The coupling agent with longer chains causes more swelling and moves the glass transition temperature T(g) downwards. Below the glass transition region, silica causes a lowering of the dynamic storage modulus G', a result of hindering the cure reaction. Above the glass transition, silica-again modified or otherwise-provides the expected reinforcement effect.

  19. Magnetic silica hybrids modified with guanidine containing co-polymers for drug delivery applications

    Energy Technology Data Exchange (ETDEWEB)

    Timin, Alexander S., E-mail: a_timin@mail.ru [Inorganic Chemistry Department, Ivanovo State University of Chemistry and Technology (ISUCT), 7, Sheremetevsky prosp., 153000 Ivanovo (Russian Federation); RASA Center in Tomsk, Tomsk Polytechnic University, 30, Lenin Avenue, 634500 Tomsk (Russian Federation); Khashirova, Svetlana Yu. [Kabardino-Balkar State University, ul. Chernyshevskogo 173, Nal' chik, 360004 Kabardino-Balkaria (Russian Federation); Rumyantsev, Evgeniy V.; Goncharenko, Alexander A. [Inorganic Chemistry Department, Ivanovo State University of Chemistry and Technology (ISUCT), 7, Sheremetevsky prosp., 153000 Ivanovo (Russian Federation)

    2016-07-01

    Guanidine containing co-polymers grafted onto silica nanoparticles to form core-shell structure were prepared by sol-gel method in the presence of γ-Fe{sub 2}O{sub 3} nanoparticles. The morphological features for uncoated and coated silica particles have been characterized with scanning electron microscopy. The results show that the polymer coated silicas exhibit spherical morphology with rough polymeric surface covered by γ-Fe{sub 2}O{sub 3} nanoparticles. The grafting amount of guanidine containing co-polymers evaluated by thermogravimetric analysis was in the range from 17 to 30%. Then, the drug loading properties and cumulative release of silica hybrids modified with guanidine containing co-polymers were evaluated using molsidomine as a model drug. It was shown that after polymer grafting the loading content of molsidomine could reach up to 3.42 ± 0.21 and 2.34 ± 0.14 mg/g respectively. The maximum drug release of molsidomine is achieved at pH 1.6 (approximately 71–75% release at 37 °C), whereas at pH 7.4 drug release is lower (50.4–59.6% release at 37 °C). These results have an important implication that our magneto-controlled silica hybrids modified with guanidine containing co-polymers are promising as drug carriers with controlled behaviour under influence of magnetic field. - Highlights: • Polymer coated silica hybrids containing γ-Fe{sub 2}O{sub 3} were prepared via sol–gel method. • Polymer grafting influences pH-response and surface properties of final products. • Molsidomine as a model drug was effectively loaded into polymer coated silicas. • The drug loading depends on the nature of grafted polymer and its content.

  20. Fabrication of the novel core-shell MCM-41@mTiO{sub 2} composite microspheres with large specific surface area for enhanced photocatalytic degradation of dinitro butyl phenol (DNBP)

    Energy Technology Data Exchange (ETDEWEB)

    Wei, Xiao-Na; Wang, Hui-Long, E-mail: hlwang@dlut.edu.cn; Li, Zhen-Duo; Huang, Zhi-Qiang; Qi, Hui-Ping; Jiang, Wen-Feng

    2016-05-30

    Graphical abstract: The mesoporous MCM-41@mTiO{sub 2} composite microspheres with core/shell structure, well-crystallized mesoporous TiO{sub 2} layer, high specific surface, large pore volume and excellent photocatalytic activity were synthesized by combining sol-gel and simple hydrothermal treatment. - Highlights: • The mesoporous MCM-41@mTiO{sub 2} composite was synthesized successfully. • The composite was facilely prepared by combining sol-gel and hydrothermal method. • The composite exhibited high photocatalytic degradation activity for DNBP. • The composite photocatalyst has excellent reproducibility. - Abstract: The mesoporous MCM-41@mTiO{sub 2} core-shell composite microspheres were synthesized successfully by combining sol-gel and simple hydrothermal treatment. The morphology and microstructure characteristics of the synthesized materials were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), N{sub 2} adsorption-desorption measurements, X-ray powder diffraction (XRD), UV–vis diffuse reflectance spectra (UV–vis/DRS) and Fourier transform infrared spectroscopy (FT-IR). The results indicate that the composite material possesses obvious core/shell structure, a pure mesoporous and well-crystallized TiO{sub 2} layer (mTiO{sub 2}), high specific surface area (316.8 m{sup 2}/g), large pore volume (0.42 cm{sup 3}/g) and two different pore sizes (2.6 nm and 11.0 nm). The photocatalytic activity of the novel MCM-41@mTiO{sub 2} composite was evaluated by degrading 2-sec-butyl-4,6-dinitrophenol (DNBP) in aqueous suspension under UV and visible light irradiation. The results were compared with commercial anatase TiO{sub 2} and Degussa P25 and the enhanced degradation were obtained with the synthesized MCM-41@mTiO{sub 2} composite under the same conditions, which meant that this material can serve as an efficient photocatalyst for the degradation of hazardous organic pollutants in wastewaters.

  1. Corundum ceramic materials modified with silica nanopowders: structure and mechanical properties

    International Nuclear Information System (INIS)

    Kostytsyn, M. A.; Muratov, D. S.; Lysov, D. V.; Chuprunov, K. O.; Yudin, A. G.; Leybo, D. V.

    2016-01-01

    Filtering elements are often used in the metallurgy of rare earth metals. Corundum ceramic is one of the most suitable materials for this purpose. The process of formation and the properties of nanomodified ceramic materials, which are proposed as filtering materials with tunable effective porosity, are described. A silica nanopowder is used as a porosity-increasing agent. Vortex layer apparatus is used for mixing of precursor materials. The obtained results show that nanomodification with the vortex layer apparatus using 0.04 wt. % silica nanopowder as a modifying agent leads to an increase in the compression strength of corundum ceramic by the factor of 1.5. (paper)

  2. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    Energy Technology Data Exchange (ETDEWEB)

    Popova, Margarita, E-mail: mpopova@orgchem.bas.bg [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Szegedi, Agnes [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Mavrodinova, Vesselina [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria); Novak Tušar, Natasa [National Institute of Chemistry, Ljubljana (Slovenia); Mihály, Judith; Klébert, Szilvia [Research Centre for Natural Sciences, Institute of Materials and Environmental Chemistry, Hungarian Academy of Sciences, 1117 Budapest, Magyar tudósok körútja 2. (Hungary); Benbassat, Niko; Yoncheva, Krassimira [Faculty of Pharmacy, 2 Dunav Str., 1000 Sofia (Bulgaria)

    2014-11-15

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol.

  3. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    International Nuclear Information System (INIS)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-01-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol

  4. Influence of Silane modified nano silica on the corrosion protection of zinc rich coating

    International Nuclear Information System (INIS)

    Nguyen Thuy Duong; To Thi Xuan Hang; Trinh Anh Truc; Pham Gia Vu; Bui Van Truoc; Thai Hoang

    2015-01-01

    Zinc rich coatings are the best effective primers for corrosion protection of carbon steel in aggressive conditions. For traditional zinc rich primer the zinc content is very high, more than 90 wt.%. The coating adhesion is decreased with the increase of zinc content, so that it is necessary to decrease the zinc content by using additives. In this study the nano silica modified by N-(2-Aminoethyl)-3-aminopropyltrimethoxysilane was prepared and incorporated in zinc rich epoxy coatings containing 85 wt.% zinc powder. The corrosion protection performance of coatings was evaluated by electrochemical impedance spectroscopy. The results obtained show that the presence of nano silica improved corrosion protection of zinc rich epoxy coating and the best protection was obtained with 3 wt.% nano silica. (author)

  5. Reactive Diazonium-Modified Silica Fillers for High-Performance Polymers.

    Science.gov (United States)

    Sandomierski, Mariusz; Strzemiecka, Beata; Chehimi, Mohamed M; Voelkel, Adam

    2016-11-08

    We describe a simple way of modification of three silica-based fillers with in situ generated 4-hydroxymethylbenzenediazonium salt ( + N 2 -C 6 H 4 -CH 2 OH). The rationale for using a hydroxyl-functionalized diazonium salt is that it provides surface-functionalized fillers that can react with phenolic resins. The modification of silica by diazonium salts was assessed using Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS). FTIR spectroscopy permitted the tracking of benzene ring breathing and C-C. The absence of the characteristic N≡N stretching vibration in the 2200-2300 cm -1 range indicates the loss of the diazonium group. XPS results indicate a higher C/Si atomic ratio after the diazonium modification of fillers and the presence of π-π* C1s satellite peaks characteristic of the surface-tethered aromatic species. Adhesion of aryl layers to the silicas is excellent because they withstand harsh thermal and organic solvent treatments. Phenolic resins (used, for example, as binders in abrasive products) were filled with diazonium-modified silicas at 10-25 wt %. The reactivity of the fillers toward phenolic resins was evaluated by the determination of the flow distance. After annealing at 180 °C, the diazonium-modified silica/phenolic resin composites were mechanically tested using the three-point flexural method. The flexural strength was found to be up to 35% higher than that of the composites prepared without any diazonium salts. Diazonium-modified silica with surface-bound -CH 2 -OH groups is thus ideal reactive filler for phenolic resins. Such filler ensures interfacial chemical reactions with the matrix and imparts robust mechanical properties to the final composites. This specialty diazonium-modified silica will find potential application as fillers in the composites for the abrasive industry. More generally, aryl diazonium salts are a unique new series of compounds for tailoring the surface properties of fillers

  6. Wettability of modified silica layers deposited on glass support activated by plasma

    Energy Technology Data Exchange (ETDEWEB)

    Terpiłowski, Konrad, E-mail: terpil@umcs.pl [Department of Physical Chemistry – Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Sklodowska University, Lublin (Poland); Rymuszka, Diana [Department of Physical Chemistry – Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Sklodowska University, Lublin (Poland); Goncharuk, Olena V.; Sulym, Iryna Ya.; Gun’ko, Vladimir M. [Chuiko Institute of Surface Chemistry, National Academy of Science of Ukraine, Kiev (Ukraine)

    2015-10-30

    Highlights: • New modified silica materials synthesis. • Support surface plasma activation. • Apparent surface free energy determination. • Equilibrium contact angle calculation. - Abstract: Fumed silica modified by hexamethyldisilazane [HDMS] and polydimethylsiloxane [PDMS] was dispersed in a polystyrene/chloroform solution. To increase adhesion between deposited silica layers and a glass surface, the latter was pretreated with air plasma for 30 s. The silica/polystyrene dispersion was deposited on the glass support using a spin coater. After deposition, the plates were dried in a desiccator for 24 h. Water advancing and receding contact angles were measured using the tilted plate method. The apparent surface free energy (γ{sub S}) was evaluated using the contact angle hysteresis approach. The surface topography was determined using the optical profilometry method. Contact angles changed from 59.7° ± 4.4 (at surface coverage with trimethylsilyl groups Θ = 0.14) to 155° ± 3.1 at Θ = 1. The value of γ{sub S} decreased from 51.3 ± 2.8 mJ/m{sup 2} (for the sample at the lowest value of Θ) to 1.0 ± 0.4 mJ/m{sup 2} for the most hydrophobic sample. Thus, some systems with a high degree of modification by HDMS showed superhydrophobicity, and the sliding angle amounted to about 16° ± 2.1.

  7. Bimetallic Nanocatalysts in Mesoporous Silica for Hydrogen Production from Coal-Derived Fuels

    Energy Technology Data Exchange (ETDEWEB)

    Kuila, Debasish [North Carolina Agricultural & Technical State Univ., Greensboro, NC (United States); Ilias, Shamsuddin [North Carolina Agricultural & Technical State Univ., Greensboro, NC (United States)

    2013-02-13

    In steam reforming reactions (SRRs) of alkanes and alcohols to produce H2, noble metals such as platinum (Pt) and palladium (Pd) are extensively used as catalyst. These metals are expensive; so, to reduce noble-metal loading, bi-metallic nanocatalysts containing non-noble metals in MCM-41 (Mobil Composition of Material No. 41, a mesoporous material) as a support material with high-surface area were synthesized using one-pot hydrothermal procedure with a surfactant such as cetyltrimethylammonium bromide (CTAB) as a template. Bi-metallic nanocatalysts of Pd-Ni and Pd-Co with varying metal loadings in MCM-41 were characterized by x-ray diffraction (XRD), N2 adsorption, and Transmission electron microscopy (TEM) techniques. The BET surface area of MCM-41 (~1000 m2/g) containing metal nanoparticles decreases with the increase in metal loading. The FTIR studies confirm strong interaction between Si-O-M (M = Pd, Ni, Co) units and successful inclusion of metal into the mesoporous silica matrix. The catalyst activities were examined in steam reforming of methanol (SRM) reactions to produce hydrogen. Reference tests using catalysts containing individual metals (Pd, Ni and Co) were also performed to investigate the effect of the bimetallic system on the catalytic behavior in the SRM reactions. The bimetallic system remarkably improves the hydrogen selectivity, methanol conversion and stability of the catalyst. The results are consistent with a synergistic behavior for the Pd-Ni-bimetallic system. The performance, durability and thermal stability of the Pd-Ni/MCM-41 and Pd-Co/MCM-41 suggest that these materials may be promising catalysts for hydrogen production from biofuels. A part of this work for synthesis and characterization of Pd-Ni-MCM-41 and its activity for SRM reactions has been published (“Development of Mesoporous Silica Encapsulated Pd-Ni Nanocatalyst for Hydrogen Production” in “Production and Purification of Ultraclean

  8. Titania-Coated Silica Alone and Modified by Sodium Alginate as Sorbents for Heavy Metal Ions

    Science.gov (United States)

    Kołodyńska, D.; Gęca, M.; Skwarek, E.; Goncharuk, O.

    2018-04-01

    The novel organic-inorganic biohybrid composite adsorbent was synthesized based on nanosized silica-titania modified with alginate within the development of effective adsorbent for heavy metal ions. Effects of metal species Cu(II), Zn(II), Cd(II), and Pb(II); concentrations; pH; temperature; and adsorption onto titania-coated silica (ST20) initial or modified by sodium alginate (ST20-ALG) were studied. The equilibrium and kinetic data of metal ions adsorption were analyzed using Langmuir and Freundlich adsorption models and kinetic models: pseudo first order, pseudo second order, intraparticle kinetic model, and Elovich. The maximum sorption capacities observed were higher for the ST20-ALG composite compared to the initial ST20 oxide for all studied metal ions, namely their values for ST20-ALG were 22.44 mg g- 1 for Cu(II) adsorption, 19.95 mg g- 1 for Zn(II), 18.85 mg g- 1 for Cd(II), and 32.49 mg g- 1 for Pb(II). Structure and properties of initial silica-titania ST20 and modified by sodium alginate ST20-ALG adsorbents were analyzed using nitrogen adsorption/desorption isotherms, ATR-FTIR, SEM-EDS, and pHpzc techniques.

  9. Effect of silica particles modified by in-situ and ex-situ methods on the reinforcement of silicone rubber

    International Nuclear Information System (INIS)

    Song, Yingze; Yu, Jinhong; Dai, Dan; Song, Lixian; Jiang, Nan

    2014-01-01

    Highlights: • In-situ and ex-situ methods were applied to modify silica particles. • In-situ method was more beneficial to preparing silica particles with high BET surface area. • Silicone rubber filled with in-situ modified silica exhibits excellent mechanical and thermal properties. - Abstract: In-situ and ex-situ methods were applied to modify silica particles in order to investigate their effects on the reinforcement of silicone rubber. Surface area and pore analyzer, laser particle size analyzer, Fourier-transform infrared spectroscopy (FTIR), contact-angle instrument, and transmission electron microscope (TEM) were utilized to investigate the structure and properties of the modified silica particles. Dynamic mechanical thermal analyzer (DMTA) was employed to characterize the vulcanizing behavior and mechanical properties of the composites. Thermogravimetric analysis (TGA) was performed to test the thermal stability of the composites. FTIR and contact angle analysis indicated that silica particles were successfully modified by these two methods. The BET surface area and TEM results reflected that in-situ modification was more beneficial to preparing silica particles with irregular shape and higher BET surface area in comparison with ex-situ modification. The DMTA and TGA data revealed that compared with ex-situ modification, the in-situ modification produced positive influence on the reinforcement of silicone rubber

  10. Hybrid thin films derived from UV-curable acrylate-modified waterborne polyurethane and monodispersed colloidal silica

    Directory of Open Access Journals (Sweden)

    C. H. Yang

    2012-01-01

    Full Text Available Hybrid thin films containing nano-sized inorganic domains were synthesized from UV-curable acrylate-modified waterborne polyurethane (WPU-AC and monodispersed colloidal silica with coupling agent. The coupling agent, 3-(trimethoxysilylpropyl methacrylate (MSMA, was bonded onto colloidal silica first, and then mixed with WPU-AC to form a precursor solution. This precursor was spin coated, dried and UV-cured to generate the hybrid films. The silica content in the hybrid thin films was varied from 0 to 30 wt%. Experimental results showed the aggregation of silica particles in the hybrid films. Thus, the silica domain in the hybrid films was varied from 30 to 50 nm by the different ratios of MSMAsilica to WPU-AC. The prepared hybrid films from the crosslinked WPU-AC/MSMA-silica showed much better thermal stability and mechanical properties than pure WPU-AC.

  11. Amperometric xanthine biosensors using glassy carbon electrodes modified with electrografted porous silica nanomaterials loaded with xanthine oxidase

    International Nuclear Information System (INIS)

    Saadaoui, Maroua; Sánchez, Alfredo; Díez, Paula; Raouafi, Noureddine; Pingarrón, José M.; Villalonga, Reynaldo

    2016-01-01

    Glassy carbon electrodes were modified with silica materials such as silica nanoparticles, mesoporous silica nanoparticles and mesoporous silica thin films with the aim to introduce scaffolds suitable for the immobilization of enzymes. Xanthine oxidase was selected as a model enzyme, and xanthine as the target analyte. A comparison of the modified electrodes showed the biosensor prepared with mesoporous silica nanoparticles to perform best. By using the respective biosensor, xanthine can be amperometrically determined (via measurement of enzymatically formed hydrogen peroxide) at a working voltage of 0.7 V (vs. Ag/AgCl) with a 0.28 μM detection limit. The biosensor was evaluated in terms of potential interferences, reproducibility and stability, and applied to the determination of fish freshness via sensing of xanthine. (author)

  12. Temperature-modified photonic bandgap in colloidal photonic crystals fabricated by vinyl functionalized silica spheres

    International Nuclear Information System (INIS)

    Deng Tiansong; Zhang Junyan; Zhu Kongtao; Zhang Qifeng; Wu Jinlei

    2011-01-01

    Graphical abstract: A thermal annealing procedure was described for fine modifying the photonic bandgap properties of colloidal photonic crystals, which were self-assembled from vinyl-functionalized silica spheres by a gravity sedimentation process. Highlights: → We described a thermal annealing procedure for fine modifying the photonic bandgap properties of colloidal photonic crystals. → The position of its stop band had more than 25% blue shift by annealing the sample from 60 to 600 deg. C. → The annealing temperature and the Bragg peak values have a linear relationship in the 120-440 deg. C range. → The effects provide a simple and controllable method for modifying the photonic bandgap properties of colloidal photonic crystals. - Abstract: A thermal annealing procedure for fine modifying the photonic bandgap properties of colloidal photonic crystals was described. The colloidal photonic crystals were assembled from monodisperse vinyl functionalized silica spheres by a gravity sedimentation process. The samples diffract light following Bragg's law combined with Snell's law. By annealing the sample at temperatures in the range of 60-600 deg. C, the position of its stop band shifted from 943 to 706 nm. It had more than 25% blue shift. In addition, the annealing temperature and the Bragg peak values have a linear relationship in the 120-440 deg. C range. Fourier transform infrared (FT-IR) spectra and thermo-gravimetric analysis (TGA) curves of vinyl functionalized silica spheres confirmed the above results. The effects provide a simple and controllable method for modifying the photonic bandgap properties of colloidal photonic crystals.

  13. Crystalline silica is a negative modifier of pulmonary cytochrome P-4501A1 induction

    Energy Technology Data Exchange (ETDEWEB)

    Battelli, L.A.; Ghanem, M.M.; Kashon, M.L.; Barger, M.; Ma, J.Y.C.; Simoskevitz, R.L.; Miles, P.R.; Hubbs, A.F. [NIOSH, Morgantown, WV (United States). Health Effects Laboratory Division

    2008-07-01

    Polycyclic aromatic hydrocarbons (PAHs) are products of incomplete combustion that are commonly inhaled by workers in the dusty trades. Many PAHs are metabolized by cytochrome P-4501A1 (CYP1A1), which may facilitate excretion but may activate pulmonary carcinogens. PAHs also stimulate their own metabolism by inducing CYP1A1. Recent studies suggest that respirable coal dust exposure inhibits induction of pulmonary CYP1A1 using the model PAH {beta}-naphthoflavone. The effect of the occupational particulate respirable crystalline silica was investigated on PAH-dependent pulmonary CYP1A1 induction. Male Sprague-Dawley rats were exposed to intratracheal silica or vehicle and then intraperitoneal {beta}-naphthoflavone, a CYP1A1 inducer, and/or phenobarbital, an inducer of hepatic CYP2B1, or vehicle. {beta}-Naphthoflavone induced pulmonary CYP1A1, but silica attenuated this {beta}-naphthoflavone-induced CYP1A1 activity and also suppressed the activity of CYP2B1, the major constituitive CYP in rat lung. The magnitude of CYP activity suppression was similar regardless of silica exposure dose within a range of 5 to 20 mg/rat. Phenobarbital and beta-naphthoflavone had no effect on pulmonary CYP2B1 activity. Both enzymatic immunohistochemistry and immunofluorescent staining for CYP1A1 indicated that sites of CYP1A1 induction were nonciliated airway epithelial cells, endothelial cells, and the alveolar septum. Our findings suggest that in PAH-exposed rat lung, silica is a negative modifier of CYP1A1 induction and CYP2B1 activity.

  14. Biosilica from Living Diatoms: Investigations on Biocompatibility of Bare and Chemically Modified Thalassiosira weissflogii Silica Shells

    Directory of Open Access Journals (Sweden)

    Stefania Roberta Cicco

    2016-12-01

    Full Text Available In the past decade, mesoporous silica nanoparticles (MSNs with a large surface area and pore volume have attracted considerable attention for their application in drug delivery and biomedicine. Here we propose biosilica from diatoms as an alternative source of mesoporous materials in the field of multifunctional supports for cell growth: the biosilica surfaces were chemically modified by traditional silanization methods resulting in diatom silica microparticles functionalized with 3-mercaptopropyl-trimethoxysilane (MPTMS and 3-aminopropyl-triethoxysilane (APTES. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy analyses revealed that the –SH or –NH2 were successfully grafted onto the biosilica surface. The relationship among the type of functional groups and the cell viability was established as well as the interaction of the cells with the nanoporosity of frustules. These results show that diatom microparticles are promising natural biomaterials suitable for cell growth, and that the surfaces, owing to the mercapto groups, exhibit good biocompatibility.

  15. Effects of partial replacement of silica with surface modified nanocrystalline cellulose on properties of natural rubber nanocomposites

    Directory of Open Access Journals (Sweden)

    Y. F. Luo

    2012-01-01

    Full Text Available Nanocrystalline cellulose was modified by 3-aminopropyl-triethoxysilane (KH550. The modified nanocrystalline cellulose (MNCC was further investigated to partially replace silica in natural rubber (NR composites via coagulation. NR/MNCC/silica and NR/nanocrystalline cellulose (NCC/silica nanocomposites were prepared. Through the comparison of vulcanization characteristics, processing properties of compounds and mechanical properties, compression fatigue properties, dynamic mechanical performance of NR/MNCC/silica and NR/NCC/silica nanocomposites, MNCC was proved to be more efficient than NCC. MNCC could activate the vulcanization process, suppress Payne effect, increase 300% modulus, tear strength and hardness, and reduce the heat build-up and compression set. Moreover, fine MNCC dispersion and strong interfacial interaction were achieved in NR/MNCC/silica nanocomposites. The observed reinforcement effects were evaluated based on the results of apparent crosslinking density (Vr, thermo-gravimetric (TG and scanning electron microscopic (SEM analyses of NR/MNCC/silica in comparison with NR/NCC/silica nanocomposites.

  16. 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.

  17. Simultaneous determination of hydroquinone and catechol at gold nanoparticles mesoporous silica modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Tashkhourian, J., E-mail: tashkhourian@susc.ac.ir [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Daneshi, M.; Nami-Ana, F. [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Behbahani, M.; Bagheri, A. [Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran (Iran, Islamic Republic of)

    2016-11-15

    Highlights: • An electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode was developed. • The electrode provides an accessible surface for simultaneous determination of hydroquinone and catechol. • Hydroquinone and catechol are highly toxic to both environment and human even at very low concentrations. - Abstract: A new electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode (AuNPs-MPS) was developed for simultaneous determination of hydroquinone and catechol. Morphology and structure of the AuNPs-MPS were characterized by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The electrochemical behavior of hydroquinone and catechol were investigated using square wave voltammetry and the results indicate that the electrochemical responses are improved significantly at the modified electrode. The observed oxidative peaks separation of about 120 mV made possible the simultaneous determination of hydroquinone and catechol in their binary-mixture. Under the optimized condition, a linear dynamic range of 10.0 μM–1.0 mM range for hydroquinone with the detection limit of 1.2 μM and from 30.0 μM–1.0 mM for catechol with the detection limit of 1.1 μM were obtained. The applicability of the method was demonstrated by the recovery studies of hydroquinone and catechol in spiked tap water samples.

  18. 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.

  19. 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.

  20. Impact behavior of f-silica and amine terminated polybutadiene co-acrylonitrile rubber modified novolac epoxy/Kevlar nanocomposites

    Science.gov (United States)

    Kavita, Pal, Vijayeta; Tiwari, R. K.

    2018-05-01

    In the present work, nano-fumed silica treated with 3-Glycidoxypropyl trimethoxy silane (f-silica) was used as a nanoreinforcement in the fabrication of amine terminated polybutadiene co-acrylonitrile rubber (ATBN) modified Kevlar/epoxy based nanocomposites. Nanocomposites with different f-silica loading (0, 0.5, 1.0 and 2.0 wt. %) and having same ATBN (10 wt. %) were made and characterized by Izod impact test for evaluating impact strength values. All the nanocomposites showed better impact strength than neat Kevlar/novolac epoxy based composite.

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

    Directory of Open Access Journals (Sweden)

    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.

  2. Electrochemistry and determination of epinephrine using a mesoporous Al-incorporated SiO{sub 2} modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Yanhong; Yang, Jinquan; Wu, Kangbing [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2008-05-30

    The potential application of Al-incorporated mesoporous SiO{sub 2} (denoted as Al-MCM-41) in electrochemistry as a novel electrode material was investigated. The peak currents of K{sub 3}[Fe(CN){sub 6}] remarkably increase and the peak potential separation obviously decreases at the mesoporous Al-MCM-41 modified carbon paste electrode (CPE). These phenomena suggest that the mesoporous Al-MCM-41 modified CPE possesses larger electrode area and electron transfer rate constant. Furthermore, the electrochemical behavior of epinephrine (EP) was investigated in different supporting electrolytes such as 0.01 mol L{sup -1} HClO{sub 4} and pH 7.0 phosphate buffer. It is found that the mesoporous Al-MCM-41 modified CPE exhibits catalytic ability to the oxidation of EP due to remarkable peak current enhancement and negative shift of peak potential. The electrochemical oxidation mechanism was also discussed. Finally, a novel electrochemical method was proposed for the determination of EP, which used to determine EP in urine samples. (author)

  3. Electrochemistry and determination of epinephrine using a mesoporous Al-incorporated SiO{sub 2} modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zeng Yanhong; Yang Jinquan [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China); Wu Kangbing [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China)], E-mail: kbwu@mail.hust.edu.cn

    2008-05-30

    The potential application of Al-incorporated mesoporous SiO{sub 2} (denoted as Al-MCM-41) in electrochemistry as a novel electrode material was investigated. The peak currents of K{sub 3}[Fe(CN){sub 6}] remarkably increase and the peak potential separation obviously decreases at the mesoporous Al-MCM-41 modified carbon paste electrode (CPE). These phenomena suggest that the mesoporous Al-MCM-41 modified CPE possesses larger electrode area and electron transfer rate constant. Furthermore, the electrochemical behavior of epinephrine (EP) was investigated in different supporting electrolytes such as 0.01 mol L{sup -1} HClO{sub 4} and pH 7.0 phosphate buffer. It is found that the mesoporous Al-MCM-41 modified CPE exhibits catalytic ability to the oxidation of EP due to remarkable peak current enhancement and negative shift of peak potential. The electrochemical oxidation mechanism was also discussed. Finally, a novel electrochemical method was proposed for the determination of EP, which used to determine EP in urine samples.

  4. Development of efficient amine-modified mesoporous silica SBA-15 for CO2 capture

    International Nuclear Information System (INIS)

    Zhang, Xiaoyun; Qin, Hongyan; Zheng, Xiuxin; Wu, Wei

    2013-01-01

    Graphical abstract: - Highlights: • A secondary amine AN-TEPA is used to modify the SBA-15. • CO 2 adsorption capacity (180.1 mg g −1 -adsorbent for 70% amine loading) is high. • The sorbent exhibits a high stability after 12 cycling runs. • The modified SBA-15 achieves complete desorption at low temperature (100 °C). - Abstract: A novel CO 2 sorbent was prepared by impregnating mesoporous silica, SBA-15, with acrylonitrile (AN)-modified tetraethylenepentamine (TEPA) in order to increase CO 2 adsorption capacity and improve cycling stability. The mesoporous silica with pre- and post-surface modification was investigated by X-ray diffraction characterization (XRD), N 2 adsorption–desorption test (N 2 -BET), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). The adsorption/desorption performance of S-TN (TN: AN modified TEPA) and S-TEPA was studied by dynamic adsorption. Test results showed that the solid base-impregnated SBA-15 demonstrated high CO 2 adsorption capacity (180.1 mg g −1 -adsorbent for 70% amine loading level). Compared to S-TEPA (24.1% decrease of initial capacity), S-TN with 50% amine loading exhibited improved cycling stability, 99.9% activity reserved (from initial 153.0 mg g −1 to 151.3 mg g −1 ) after 12 cycles of adsorption/desorption at 100 °C. A mechanism of molecular structure of the loaded amine was attributed to the improved performance

  5. Mesoporous Structure Control of Silica in Room-Temperature Synthesis under Basic Conditions

    Directory of Open Access Journals (Sweden)

    Jeong Wook Seo

    2015-01-01

    Full Text Available Various types of mesoporous silica, such as continuous cubic-phase MCM-48, hexagonal-phase MCM-41, and layer-phase spherical silica particles, have been synthesized at room temperature using cetyltrimethylammonium bromide as a surfactant, ethanol as a cosurfactant, tetraethyl orthosilicate as a silica precursor, and ammonia as a condensation agent. Special care must be taken both in the filtering of the resultant solid products and in the drying process. In the drying process, further condensation of the silica after filtering was induced. As the surfactant and cosurfactant concentrations in the reaction mixture increased and the NH3 concentration decreased, under given conditions, continuous cubic MCM-48 and layered silica became the dominant phases. A cooperative synthesis mechanism, in which both the surfactant and silica were involved in the formation of mesoporous structures, provided a good explanation of the experimental results.

  6. 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)

  7. ABTS-Modified Silica Nanoparticles as Laccase Mediators for Decolorization of Indigo Carmine Dye

    Directory of Open Access Journals (Sweden)

    Youxun Liu

    2015-01-01

    Full Text Available Efficient reuse and regeneration of spent mediators are highly desired for many of the laccases’ biotechnology applications. This investigation demonstrates that a redox mediator 2,2′-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS covalently attached to silica nanoparticles (SNPs effectively mediated dye decolorization catalyzed by laccase. Characteristics of ABTS-modified silica nanoparticles (ABTS-SNPs were researched by scanning electron microscopy and Fourier-transformed infrared spectroscopy. When ABTS and ABTS-SNPs were used as laccase mediators, the decolorization yields of 96 and 95% were, respectively, obtained for indigo carmine dye. The results suggest that ABTS immobilized on SNPs can be used as laccase mediators as they retain almost the same efficiency as the free ABTS. The oxidized ABTS-SNPs were regenerated by their reduction reaction with ascorbic acid. Decolorization efficiency of regenerated ABTS-SNPs and their initial forms were found to be almost equivalent. Six reuse cycles for spent ABTS-SNPs were run for the treatment of indigo carmine, providing decolorization yields of 96–77%. Compared with free mediator, the immobilized mediators have the advantage of being easily recovered, regenerated, and reused making the whole process environmentally friendly.

  8. Hyaluronic acid oligosaccharide modified redox-responsive mesoporous silica nanoparticles for targeted drug delivery.

    Science.gov (United States)

    Zhao, Qinfu; Geng, Hongjian; Wang, Ying; Gao, Yikun; Huang, Jiahao; Wang, Yan; Zhang, Jinghai; Wang, Siling

    2014-11-26

    A redox-responsive delivery system based on colloidal mesoporous silica (CMS) has been developed, in which 6-mercaptopurine (6-MP) was conjugated to vehicles by cleavable disulfide bonds. The oligosaccharide of hyaluronic acid (oHA) was modified on the surface of CMS by disulfide bonds as a targeting ligand and was able to increase the stability and biocompatibility of CMS under physiological conditions. In vitro release studies indicated that the cumulative release of 6-MP was less than 3% in the absence of glutathione (GSH), and reached nearly 80% within 2 h in the presence of 3 mM GSH. Confocal microscopy and fluorescence-activated cell sorter (FACS) methods were used to evaluate the cellular uptake performance of fluorescein isothiocyanate (FITC) labeled CMS, with and without oHA modification. The CMS-SS-oHA exhibited a higher cellular uptake performance via CD44 receptor-mediated endocytosis in HCT-116 (CD44 receptor-positive) cells than in NIH-3T3 (CD44 receptor-negative) cells. 6-MP loaded CMS-SS-oHA exhibited greater cytotoxicity against HCT-116 cells than NIH-3T3 cells due to the enhanced cell uptake behavior of CMS-SS-oHA. This study provides a novel strategy to covalently link bioactive drug and targeting ligand to the interiors and exteriors of mesoporous silica to construct a stimulus-responsive targeted drug delivery system.

  9. 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).

  10. Dual Mode Fluorophore-Doped Nickel Nitrilotriacetic Acid-Modified Silica Nanoparticles Combine Histidine-Tagged Protein Purification with Site-Specific Fluorophore Labeling

    OpenAIRE

    Kim, Sung Hoon; Jeyakumar, M.; Katzenellenbogen, John A.

    2007-01-01

    We present the first example of a fluorophore-doped nickel chelate surface- modified silica nanoparticle that functions in a dual mode, combining histidine-tagged protein purification with site-specific fluorophore labeling. Tetramethylrhodamine (TMR)-doped silica nanoparticles, estimated to contain 700–900 TMRs per ca. 23-nm particle, were surface modified with nitrilotriacetic acid (NTA), producing TMR-SiO2-NTA-Ni+2. Silica-embedded TMR retains very high quantum yield, is resistant to quenc...

  11. Photoresponsive Release from Azobenzene-Modified Single Cubic Crystal NaCl/Silica Particles

    Directory of Open Access Journals (Sweden)

    Xingmao Jiang

    2011-01-01

    Full Text Available Azobenzene ligands were uniformly anchored to the pore surfaces of nanoporous silica particles with single crystal NaCl using 4-(3-triethoxysilylpropylureidoazobenzene (TSUA. The functionalization delayed the release of NaCl significantly. The modified particles demonstrated a photocontrolled release by trans/cis isomerization of azobenzene moieties. The addition of amphiphilic solvents, propylene glycol (PG, propylene glycol propyl ether (PGPE, and dipropylene glycol propyl ether (DPGPE delayed the release in water, although the wetting behavior was improved and the delay is the most for the block molecules with the longest carbon chain. The speedup by UV irradiation suggests a strong dependence of diffusion on the switchable pore size. TGA, XRD, FTIR, and NMR techniques were used to characterize the structures.

  12. Removal of Parathion from Aqueous Media Through p-tert-Butylcalix[4]arene Based Modified Silica

    Directory of Open Access Journals (Sweden)

    Sibghatullah Memon

    2013-12-01

    Full Text Available This study explores, adsorption efficiency of p-tert-butylcalix[4]arene based modified silica to remove parathion from aqueous environment. The adsorption parameters, i.e. pH, concentration of pesticide solution, contact time and adsorbent dosage were optimized, as 10, 1 mg L-1, 40 min and 0.04 g, respectively. Langmuir, Freundlich and Dubinin-Radushkevich (D-R isotherm models were used to evaluate the adsorption mechanism. Adsorption constants values of these models suggest that the adsorption of parathion is favorable and were found to be best fit with Freundlich isotherm. From the kinetic study it can be predicted that adsorption of parathion follows Ho and McKay model (pseudo-second order. Thermodynamic parameters, enthalpy (ΔH, entropy (ΔS and Gibbs free energy (ΔG have also been evaluated and were found as -132.25, 0.45, -4.14 Jmol-1, respectively.

  13. Metal Recovery and Preconcentration by Edta and Dtpa Modified Silica Surfaces

    Directory of Open Access Journals (Sweden)

    Eveliina Repo

    2017-03-01

    Full Text Available This study focuses on the adsorption and preconcentration of various metals by silica gel surfaces modified with aminopolycarboxylic acids namely ethylenediaminetetraacetic acid or diethylenetriamine-pentaacetic acid. The adsorption performance of the studied materials was determined in mixed metal solutions and the adsorption isotherm studies were conducted for cobalt, nickel, cadmium, and lead. The results were modeled using various theoretical isotherm equations, which suggested that two different adsorption sites were involved in metal removal although lead showed clearly different adsorption behavior attributed to its lowest hydration tendency. Efficient regeneration of the adsorbents and preconcentration of metals was conducted with nitric acid. Results indicated that the metals under study could be analyzed rather accurately after preconcentration from both pure, saline and ground water samples.

  14. Mesoporous Silica Supported Au Nanoparticles with Controlled Size as Efficient Heterogeneous Catalyst for Aerobic Oxidation of Alcohols

    Directory of Open Access Journals (Sweden)

    Xuefeng Chu

    2015-01-01

    Full Text Available A series of Au catalysts with different sizes were synthesized and employed on amine group functionalized ordered mesoporous silica solid supports as catalyst for the aerobic oxidation of various alcohols. The mesoporous silica of MCM-41 supported Au nanoparticles (Au-1 exhibited the smallest particle size at ~1.8 nm with superior catalytic activities owing to the confinement effect of the mesoporous channels. Au-1 catalyst is also very stable and reusable under aerobic condition. Therefore, this presented work would obviously provide us a platform for synthesizing more size-controlled metal catalysts to improve the catalytic performances.

  15. Two emissive-magnetic composite platforms for Hg(II) sensing and removal: The combination of magnetic core, silica molecular sieve and rhodamine chemosensors

    Science.gov (United States)

    Mao, Hanping; Liu, Zhongshou

    2018-01-01

    In this paper, a composite sensing platform for Hg(II) optical sensing and removal was designed and reported. A core-shell structure was adopted, using magnetic Fe3O4 nanoparticles as the core, silica molecular sieve MCM-41 as the shell, respectively. Two rhodamine derivatives were synthesized as chemosensor and covalently immobilized into MCM-41 tunnels. Corresponding composite samples were characterized with SEM/TEM images, XRD analysis, IR spectra, thermogravimetry and N2 adsorption/desorption analysis, which confirmed their core-shell structure. Their emission was increased by Hg(II), showing emission turn on effect. High selectivity, linear working curves and recyclability were obtained from these composite samples.

  16. Dendritic silica nanomaterials (KCC-1) with fibrous pore structure possess high DNA adsorption capacity and effectively deliver genes in vitro.

    Science.gov (United States)

    Huang, Xiaoxi; Tao, Zhimin; Praskavich, John C; Goswami, Anandarup; Al-Sharab, Jafar F; Minko, Tamara; Polshettiwar, Vivek; Asefa, Tewodros

    2014-09-16

    The pore size and pore structure of nanoporous materials can affect the materials' physical properties, as well as potential applications in different areas, including catalysis, drug delivery, and biomolecular therapeutics. KCC-1, one of the newest members of silica nanomaterials, possesses fibrous, large pore, dendritic pore networks with wide pore entrances, large pore size distribution, spacious pore volume and large surface area--structural features that are conducive for adsorption and release of large guest molecules and biomacromolecules (e.g., proteins and DNAs). Here, we report the results of our comparative studies of adsorption of salmon DNA in a series of KCC-1-based nanomaterials that are functionalized with different organoamine groups on different parts of their surfaces (channel walls, external surfaces or both). For comparison the results of our studies of adsorption of salmon DNA in similarly functionalized, MCM-41 mesoporous silica nanomaterials with cylindrical pores, some of the most studied silica nanomaterials for drug/gene delivery, are also included. Our results indicate that, despite their relatively lower specific surface area, the KCC-1-based nanomaterials show high adsorption capacity for DNA than the corresponding MCM-41-based nanomaterials, most likely because of KCC-1's large pores, wide pore mouths, fibrous pore network, and thereby more accessible and amenable structure for DNA molecules to diffuse through. Conversely, the MCM-41-based nanomaterials adsorb much less DNA, presumably because their outer surfaces/cylindrical channel pore entrances can get blocked by the DNA molecules, making the inner parts of the materials inaccessible. Moreover, experiments involving fluorescent dye-tagged DNAs suggest that the amine-grafted KCC-1 materials are better suited for delivering the DNAs adsorbed on their surfaces into cellular environments than their MCM-41 counterparts. Finally, cellular toxicity tests show that the KCC-1-based

  17. Overcoming multiple gastrointestinal barriers by bilayer modified hollow mesoporous silica nanocarriers.

    Science.gov (United States)

    Wang, Ying; Zhao, Yating; Cui, Yu; Zhao, Qinfu; Zhang, Qiang; Musetti, Sara; Kinghorn, Karina A; Wang, Siling

    2018-01-01

    Oral administration of nanocarriers remains a significant challenge in the pharmaceutical sciences. The nanocarriers must efficiently overcome multiple gastrointestinal barriers including the harsh gastrointestinal environment, the mucosal layer, and the epithelium. Neutral hydrophilic surfaces are reportedly necessary for mucus permeation, but hydrophobic and cationic surfaces are important for efficient epithelial absorption. To accommodate these conflicting surface property requirements, we developed a strategy to modify nanocarrier surfaces with cationic cell-penetrating peptides (CPP) concealed by a hydrophilic succinylated casein (SCN) layer. SCN is a mucus-inert natural material specifically degraded in the intestine, thus protecting nanocarriers from the harsh gastric environment, facilitating their mucus permeation, and inducing exposure of CPPs after degradation for further effective transepithelial transport. Quantum dots doped hollow silica nanoparticles (HSQN) with a diameter around 180 nm was used as the nanocarrier and demonstrated as high as 50% loading efficacy of paclitaxel, a model drug with poor solubility and permeability. The dual layer modification strategy prevented premature drug leakage in stomach and maintained high mucus permeation (the trajectory spanned 9-fold larger area than single CPP modification). After intestinal degradation of SCN by trypsin, these nanocarriers exhibited strong interaction with epithelial membranes and a 5-fold increase in cellular uptake. Significant transepithelial transport and intestinal distribution were also observed for this dual-modified formulation. A pharmacokinetics study on the paclitaxel-loaded nanocarrier found 40% absolute bioavailability and 7.8-fold higher AUC compared to oral Taxol®. Compared with single CPP modified nanocarriers, our formulation showed increased in vivo efficacy and tumor accumulation of the model drug with negligible intestinal toxicity. In summary, sequential modification

  18. Thermal stability and surface acidity of mesoporous silica doubly doped by incorporation of sulfate and zirconium ions

    International Nuclear Information System (INIS)

    Salas, P.; Chen, L.F.; Wang, J.A.; Armendariz, H.; Guzman, M.L.; Montoya, J.A.; Acosta, D.R.

    2005-01-01

    A sulfated Si-Zr-MCM-41 solid with highly ordered mesostructure was synthesized through a templated synthesis route where the CTAB surfactant was used as template. During the synthesis procedure, various amounts of (NH 4 ) 2 SO 4 were added into the mixed solution of Zr and Si precursors to in situ sulfate the MCM-41 solids, aiming to enhance the acidity and thermal stability. The resultant materials showed a long-range ordered hexagonal arrangement with high surface area larger than 797 m 2 /g and an average pore size distributed at approximate 2.5-2.8 nm. The high-resolution TEM observations confirmed that the order of the mesostructure gained when the molar ratio of SO 4 2- /(ZrO 2 + SiO 2 ) increased from 0.1 to 0.3 but decreased as it reached 0.5, which is consistent with the results of 29 Si MAS-NMR and XRD analysis. Compared to Si-MCM-41, the (Q 2 + Q 3 )/Q 4 ratio derived from the NMR spectra of the Zr-doped sample was higher, indicating that zirconium atoms were incorporated into the silica framework. Unexpectedly, in situ sulfation does not enhance the surface Broensted acidity, most likely due to the sulfur retained within the bulk of the materials; however, it indeed improved the thermal stability of the solid and long-range order of the structure

  19. Visible Light Absorption of Binuclear TiOCoII Charge-Transfer UnitAssembled in Mesoporous Silica

    Energy Technology Data Exchange (ETDEWEB)

    Han, Hongxian; Frei, Heinz

    2007-01-30

    Grafting of CoII(NCCH3)2Cl2 onto mesoporous Ti-MCM-41 silicain acetonitrile solution affords binuclear Ti-O-CoII sites on the poresurface under complete replacement of the precursor ligands byinteractions with anchored Ti centers and the silica surface. The CoIIligand field spectrum signals that the Co centers are anchored on thepore surface in tetrahedral coordination. FT-infrared action spectroscopyusing ammonia gas adsorption reveals Co-O-Si bond modes at 831 and 762cm-1. No Co oxide clusters are observed in the as-synthesized material.The bimetallic moieties feature an absorption extending from the UV intothe visible to about 600 nm which is attributed to the TiIV-O-CoII?3TiIII-O-CoIII metal-to-metal charge-transfer (MMCT) transition. Thechromophore is absent in MCM-41 containing Ti and Co centers isolatedfrom each other; this material was synthesized by grafting CoII onto aTi-MCM-41 sample with the Ti centers protected by a cyclopentadienylligand. The result indicates that the appearance of the charge-transferabsorption requires that the metal centers are linked by an oxo bridge,which is additionally supported by XANES spectroscopy. The MMCTchromophore of Ti-O-CoII units has sufficient oxidation power to serve asvisible light electron pump for driving multi-electron transfer catalystsof demanding uphill reactions such as water oxidation.

  20. Thiol-modified gold nanoparticles deposited on silica support using dip coating

    International Nuclear Information System (INIS)

    Magura, Jozef; Zeleňáková, Adriana; Zeleňák, Vladimír; Kaňuchová, Maria

    2014-01-01

    Graphical abstract: - Highlights: • Thin layers of gold were deposited on glass substrate. • Layers were modified by two different ligands, 1,4-dithiothreitol and L-glutathione. • Red shift of SPR band was observed in spectra after modification of Au by thiols. • Charge transfer between Au and S atoms leads to ferromagnetic behaviour of samples. - Abstract: In our work, we have prepared thin layers of gold nanoparticles deposited via dip coating technique on silica glass substrate. The prepared thin layers were modified by two different ligands, namely 1,4-dithiothreitol (sample Au-DTT NPs) and L-glutathione (sample Au-GSH NPs). The spectral, structural and magnetic properties of the prepared samples were investigated. The modification of Au nanoparticles with thiol ligands leads to change of their plasmon resonance fields, as indicated by UV–vis spectra. The magnetic measurements showed that the magnetization of the samples is composed from two magnetic contributions: diamagnetic contribution and low field ferromagnetic contribution. Our experimental results show that the charge transfer between Au and S atoms gives rise to the ferromagnetic behaviour of prepared thin layers

  1. Multifunctional Amine Mesoporous Silica Spheres Modified with Multiple Amine as Carriers for Drug Release

    Directory of Open Access Journals (Sweden)

    Yan Li

    2018-01-01

    Full Text Available Mesoporous silica spheres were synthesized by using Stöber theory (MSN-40. Calcination of the mesostructured phase resulted in the starting solid. Organic modification with aminopropyl groups resulted in two MSN-40 materials: named MSN-NH2 and MSN-DQ-40, respectively. These two kinds of samples with different pore sizes (obtained from 3-[2-(2-aminoethylaminoethylamino]propyl-trimethox-ysilane (NQ-62 and modified NQ-62 showed control of the delivery rate of ibuprofen (IBU from the siliceous matrix. The obtained sample from modified NQ-62 has an increased loading rate and shows better control of the delivery rate of IBU than the obtained sample from NQ-62. These three solids were characterized using standard solid state procedures. During tests of in vitro drug release, an interesting phenomenon was observed: at high pH (pH 7.45, IBU in all carriers was released slowly; at low pH (pH 4.5, only a part of the IBU was slowly released from this carrier within 25 hours; most IBU was effectively confined in mesoporous material, but the remaining IBU was released rapidly and completely after 25 hours.

  2. 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.

  3. Synthesis of Polyurethane/Silica Modified Epoxy Polymer Based on 1,3-Propanediol for Coating Application

    Directory of Open Access Journals (Sweden)

    Lutviasari Nuraini

    2017-11-01

    Full Text Available Studies on the synthesis of polyurethane/silica modified epoxy polymer using 1,3-propanediol has been conducted. Synthesis of polymers made by reaction of tolonate and 1,3-propanediol (ratio NCO/OH=2.5 as the building blocks of polyurethane with diglycidyl ether bisphenol A (DGEBA epoxy and catalyst dibutyltin dilaurate (DBTL.The total weight of the polyurethane used was 20% (w/w of the total epoxy. Based on Fourier Transform Infrared (FTIR and 1H-Nuclear Magnetic Resonance (1H-NMR spectra indicated the existence of a new bond that is formed from the reaction of isocyanate group and hydroxyl group, where the hydroxyl groups derived from epoxy and 1,3-propanediol. The addition of silica (5, 10, and 15% w/w to epoxy into the epoxy-modified polyurethane has been carried out through sol-gel reaction of tetraethyl orthosilicate (TEOS. The isocyanate conversion rate for the addition of silica 5, 10, and 15% are 95.69; 100, and 100%, respectively. The morphology and element identification by Scanning Electron Microscopy/Energy Dispersive X-Ray Analysis (SEM/EDX, showed that Si element has been successfully added in the polymer. From the tensile strength and elongation analysis, also thermal stability analysis using Thermal Gravimetric Analyzer (TGA, the increase of silica amount into the polyurethane modified epoxy did not significantly affect to thermal properties, but decrease the tensile strength of the polymer.

  4. Microviscosity of supercooled water confined within aminopropyl-modified mesoporous silica as studied by time-resolved fluorescence spectroscopy.

    Science.gov (United States)

    Yamaguchi, Akira; Namekawa, Manato; Itoh, Tetsuji; Teramae, Norio

    2012-01-01

    The fluorescence dynamics of rhodamine B (RhB) immobilized on the pore surface of aminopropyl (AP)-modified mesoporous silica (diameter of the silica framework, 3.1 nm) was examined at temperatures between 293 and 193 K to study the microviscosity of supercooled water confined inside the pores. The mesoporous silica specimen with a dense AP layer (2.1 molecules nm(-2)) was prepared, and RhB isothiocyanate was covalently bound to part of the surface AP groups. The fluorescence lifetime of the surface RhB increased with decreasing temperature from 293 to 223 K, indicating that freezing of the confined water did not occur in this temperature range. The microviscosity of the supercooled confined water was evaluated from an analysis of the lifetime data based on a frequency-dependent friction model.

  5. Preparation and surface properties of mesoporous silica particles modified with poly(N-vinyl-2-pyrrolidone) as a potential adsorbent for bilirubin removal

    Energy Technology Data Exchange (ETDEWEB)

    Timin, Alexander, E-mail: a_timin@mail.ru [Inorganic Chemistry Department, Ivanovo State University of Chemistry and Technology (ISUCT), 7, Sheremetevsky prosp., 153000 Ivanovo (Russian Federation); Rumyantsev, Evgeniy, E-mail: evr@isuct.ru [Inorganic Chemistry Department, Ivanovo State University of Chemistry and Technology (ISUCT), 7, Sheremetevsky prosp., 153000 Ivanovo (Russian Federation); Lanin, Sergey N., E-mail: SNLanin@phys.chem.msu.ru [Chemistry Department, Physical Chemistry Division, Lomonosov Moscow State University, 1-3 Leninskie Gory, 119991 Moscow (Russian Federation); Rychkova, Sveta A. [Chemistry Department, Physical Chemistry Division, Lomonosov Moscow State University, 1-3 Leninskie Gory, 119991 Moscow (Russian Federation); Guseynov, Sabir S. [Krestov Institute of Solution Chemistry of Russian Academy of Sciences, 153000 Ivanovo (Russian Federation); Solomonov, Alexey V. [Inorganic Chemistry Department, Ivanovo State University of Chemistry and Technology (ISUCT), 7, Sheremetevsky prosp., 153000 Ivanovo (Russian Federation); Antina, Elena V. [Krestov Institute of Solution Chemistry of Russian Academy of Sciences, 153000 Ivanovo (Russian Federation)

    2014-10-15

    The surface of silica particles was modified with polyvinyl pyrrolidone (PVP) through sol–gel process. The different experimental techniques, i.e., thermogravimetric analysis (TGA and DTG), nitrogen adsorption, scanning electron microscopy (SEM), laser diffraction analysis (LDA), fourier transform spectroscopy (FTIR) are used to characterize the pure non-functionalized and functionalized silicas containing different amount of PVP. It was shown that PVP-modified silica samples have well developed porous structure; the values of specific surface area for PVP-modified silicas are in the range of 140–264 m{sup 2} g{sup −1}. While the non-functionalized silica shows the low surface area (S{sub BET} = 40 m{sup 2} g{sup −1}). The BJH analysis showed that PVP can be used as an effective agent to increase an average pore size and total pore volume. The results indicate that PVP functionalized silicas show a potential as effective adsorbents for bilirubin removal compared to other available adsorbents. - Highlights: • PVP functionalized silicas were synthesized via sol–gel method. • Modification of silica by PVP leads to the formation of mesoporous structure. • PVP functionalized mesoporous silicas demonstrate good adsorption properties for bilirubin removal.

  6. Determination of Copper in Different Ethanolic Matrices Using a Chloropropyl Silica Gel Modified with a Nanostructured Cubic Octa(3-aminopropyloctasilsesquioxane

    Directory of Open Access Journals (Sweden)

    Devaney Ribeiro Do Carmo

    2013-01-01

    Full Text Available The chloropropyl silica gel was modified with octa(3-aminopropyloctasilsesquioxane and characterized by Fourier transform infrared (FTIR spectroscopy, nuclear magnetic resonance (NMR, spectroscopies, and surface and area porosity. The specific sorption capacity of metallic ions (Cu2+ and Ni2+ increases in the following solvent order: water < ethanol 42% < ethanol < ketone. The high values of the constant (K in the order of 103 L mol−1 suggested the high adsorbent capacity of the modified silica (SGAPC for Cu2+ and Ni2+. SGAPC was applied to a separation column and shows recoveries of around 100% of copper in samples of sugar cane spirit, vodka, ginger brandy, and ethanol fuel.

  7. Electrochromatographic performance of graphene and graphene oxide modified silica particles packed capillary columns.

    Science.gov (United States)

    Zhao, Hongyan; Wang, Yizhou; Zhang, Danyu; Cheng, Heyong; Wang, Yuanchao

    2018-04-01

    Graphene oxide functionalized silica microspheres (GO@SiO 2 ) were synthesized based on condensation reaction between amino from aminosilica particles and carboxyl groups from GO. Reduction of GO@SiO 2 with hydrazinium hydroxide generated graphene modified silica particles (G@SiO 2 ). GO@SiO 2 and G@SiO 2 packed capillary columns for capillary electrochromatography were thereafter fabricated by pressure slurry packing with single-particle frits. GO of 0.3 mg/mL in dispersion solution for GO@SiO 2 synthesis was considered as a compromise between retaining and column efficiency whereas GO@SiO 2 of 20 mg/mL in slurries for column packing was chosen for a homogenous and tight bed. Optimum mobile phases were acquired considering both electroosmotic flow and resolution at an applied voltage of -6 kV as the following: acetonitrile/phosphate buffer (10 mM, pH 7.0), 75:25 (v/v) for polycyclic aromatic hydrocarbons and 50:50 (v/v) for aromatic compounds. A comparison was made between electrochromatographic performances for three PAHs (naphthalene, fluorene and phenanthrene) and three aromatic compounds of various polarities (toluene, aniline and phenol) on bare aminosilica, GO@SiO 2 and G@SiO 2 packed columns, which proved the contribution of alone or combinational actions of solvophobic effect and π-π electron stacking as well as hydrogen bonds to retaining behaviors by GO@SiO 2 and G@SiO 2 . Well over-run, over-day and over-column precisions (retention time: 0.3-1.4, 1.1-3.8 and 2.8-5.2%, respectively; peak area: 2.6-6.5, 4.8-8.3 and 6.5-12.6%, respectively) of GO@SiO 2 packed columns were a powerful proof for good reproducibility. Analytical characteristics of GO@SiO 2 packed capillary columns in CEC analysis of fresh water were evaluated with respect to linearity (R 2 = 0.9961-0.9989) over the range 0.1 to 100 mg/L and detection limits of 9.5 for naphthalene, 12.6 for fluorene and 16.2 μg/L for phenanthrene. Further application to fresh water increased the

  8. Facile and scalable preparation of highly wear-resistance superhydrophobic surface on wood substrates using silica nanoparticles modified by VTES

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Shanshan; Liu, Ming [College of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004 (China); Wu, Yiqiang, E-mail: wuyq0506@126.com [College of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004 (China); Hunan Provincial Collaborative Innovation Center for High-efficiency Utilization of Wood and Bamboo Resources, Central South University of Forestry and Technology, Changsha 410004 (China); Luo, Sha [College of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004 (China); Qing, Yan, E-mail: qingyan0429@163.com [College of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004 (China); Hunan Provincial Collaborative Innovation Center for High-efficiency Utilization of Wood and Bamboo Resources, Central South University of Forestry and Technology, Changsha 410004 (China); Chen, Haibo [College of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004 (China)

    2016-11-15

    Graphical abstract: Highly wear-resistance superhydrophobic surface on wood substrates was fabricated using silica nanoparticles modified by VTES. Display Omitted - Highlights: • Superhydrophobic surface on wood substrates was efficiently fabricated using nanoparticles modified by VTES. • The superhydrophobic surface exhibited a CA of 154° and a SAclose to 0°. • The superhydrophobic surface showed a durable and robust wear-resistance performance. - Abstract: In this study, an efficient, facile method has been developed for fabricating superhydrophobic surfaces on wood substrates using silica nanoparticles modified by VTES. The as-prepared superhydrophobic wood surface had a water contact angle of 154° and water slide angle close to 0°. Simultaneously, this superhydrophobic wood showed highly durable and robust wear resistance when having undergone a long period of sandpaper abrasion or being scratched by a knife. Even under extreme conditions of boiling water, the superhydrophobicity of the as-prepared wood composite was preserved. Characterizations by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy showed that a typical and tough hierarchical micro/nanostructure was created on the wood substrate and vinyltriethoxysilane contributed to preventing the agglomeration of silica nanoparticles and serving as low-surface-free-energy substances. This superhydrophobic wood was easy to fabricate, mechanically resistant and exhibited long-term stability. Therefore, it is considered to be of significant importance in the industrial production of functional wood, especially for outdoor applications.

  9. A comprehensive study of soft magnetic materials based on FeSi spheres and polymeric resin modified by silica nanorods

    International Nuclear Information System (INIS)

    Strečková, M.; Füzer, J.; Kobera, L.; Brus, J.; Fáberová, M.; Bureš, R.; Kollár, P.; Lauda, M.; Medvecký, Ĺ.; Girman, V.; Hadraba, H.; Bat'ková, M.; Bat'ko, I.

    2014-01-01

    A novel soft magnetic composite (SMC) based on spherical FeSi particles precisely covered by hybrid phenolic resin was designed. The hybrid resin including silica nano-rods chemically incorporated into the phenolic polymer matrix was prepared by the modified sol–gel method. A chemical bridge connecting silica nano-rods with the base polymeric net was verified by FTIR, 13 C and 29 Si NMR spectroscopy, whereas the shape and size of silica nano-rods were determined by TEM. It is shown that the modification of polymeric resin by silica nano-rods generally leads to the improved thermal and mechanical properties of the final samples. The hybrid resin serves as a perfect insulating coating deposited on FeSi particles and the core–shell particles can be further compacted by standard powder metallurgy methods in order to prepare final samples for mechanical, electric and magnetic testing. SEM images evidence negligible porosity, uniform distribution of the hybrid resin around FeSi particles, as well as, dimensional shape stability of the final samples after thermal treatment. The hardness, flexural strength and density of the final samples are comparable to the sintered SMCs, but they simultaneously exhibit much higher specific resistivity along with only slightly lower coercivity and permeability. - Highlights: • Soft magnetic composites are designed for electrotechnical applications. • Electroinsulating layer consists of phenolic resin modified with silica nano-rods. • NMR, FTIR and DSC analysis is used to characterize hybrid resin. • Spherical Fe–Si particles covered by hybrid resin form a core–shell composite. • Mechanical, electrical and magnetic properties are described in detail

  10. Proton Conductivity of Nafion/Ex-Situ Sulfonic Acid-Modified Stöber Silica Nanocomposite Membranes As a Function of Temperature, Silica Particles Size and Surface Modification

    Science.gov (United States)

    Muriithi, Beatrice; Loy, Douglas A.

    2016-01-01

    The introduction of sulfonic acid modified silica in Nafion nanocomposite membranes is a good method of improving the Nafion performance at high temperature and low relative humidity. Sulfonic acid-modified silica is bifunctional, with silica phase expected to offer an improvement in membranes hydration while sulfonic groups enhance proton conductivity. However, as discussed in this paper, this may not always be the case. Proton conductivity enhancement of Nafion nanocomposite membranes is very dependent on silica particle size, sometimes depending on experimental conditions, and by surface modification. In this study, Sulfonated Preconcentrated Nafion Stober Silica composites (SPNSS) were prepared by modification of Stober silica particles with mercaptopropyltriethoxysilane, dispersing the particles into a preconcentrated solution of Nafion, then casting the membranes. The mercapto groups were oxidized to sulfonic acids by heating the membranes in 10 wt % hydrogen peroxide for 1 h. At 80 °C and 100% relative humidity, a 20%–30% enhancement of proton conductivity was only observed when sulfonic acid modified particle less than 50 nm in diameter were used. At 120 °C, and 100% humidity, proton conductivity increased by 22%–42% with sulfonated particles with small particles showing the greatest enhancement. At 120 °C and 50% humidity, the sulfonated particles are less efficient at keeping the membranes hydrated, and the composites underperform Nafion and silica-Nafion nanocomposite membranes. PMID:26828525

  11. 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

  12. Radon exhalation rates of concrete modified with fly ash and silica fumes

    International Nuclear Information System (INIS)

    Amit Kumar; Chauhan, R.P.; Mehta, Vimal; Kant, K.

    2013-01-01

    The radiological impact of the environmental gas radon to the health of general public is of concern since many decades. Cement used for the construction blended with fly ash and silica fumes is recommended by Government in order to avoid the soil and environmental pollution. But these addition step-up the Indoor radon level in the dwelling due to radioactivity contents. The exhalation of radon from concrete blended with silica fumes and fly ash depends upon addition level, porosity, moisture and radioactivity content. In order to optimize the level of substitution of silica fumes and fly ash, measurements of radon exhalation rates from the concrete blended with different proportions of fly ash and silica fumes was carried out using active scintillation radon monitor. The effect of porosity, moisture, back diffusion and radioactivity content of the concrete on exhalation rates is studied. The measured exhalation rates were extrapolated for indoor radon concentration and effective dose equivalent using ICRP, 1987 recommendations. (author)

  13. Super-Hydrophobic/Icephobic Coatings Based on Silica Nanoparticles Modified by Self-Assembled Monolayers

    Directory of Open Access Journals (Sweden)

    Junpeng Liu

    2016-12-01

    Full Text Available A super-hydrophobic surface has been obtained from nanocomposite materials based on silica nanoparticles and self-assembled monolayers of 1H,1H,2H,2H-perfluorooctyltriethoxysilane (POTS using spin coating and chemical vapor deposition methods. Scanning electron microscope images reveal the porous structure of the silica nanoparticles, which can trap small-scale air pockets. An average water contact angle of 163° and bouncing off of incoming water droplets suggest that a super-hydrophobic surface has been obtained based on the silica nanoparticles and POTS coating. The monitored water droplet icing test results show that icing is significantly delayed by silica-based nano-coatings compared with bare substrates and commercial icephobic products. Ice adhesion test results show that the ice adhesion strength is reduced remarkably by silica-based nano-coatings. The bouncing phenomenon of water droplets, the icing delay performance and the lower ice adhesion strength suggest that the super-hydrophobic coatings based on a combination of silica and POTS also show icephobicity. An erosion test rig based on pressurized pneumatic water impinging impact was used to evaluate the durability of the super-hydrophobic/icephobic coatings. The results show that durable coatings have been obtained, although improvement will be needed in future work aiming for applications in aerospace.

  14. Mesoporous silica/polyacrylamide composite: Preparation by UV-graft photopolymerization, characterization and use as Hg(II) adsorbent

    Energy Technology Data Exchange (ETDEWEB)

    Saad, Ali, E-mail: ali.saad8803@gmail.com [Laboratory of Materials, Molecules and Applications, IPEST, University of Carthage, Sidi Bou Said road, B.P. 51, 2070 La Marsa (Tunisia); Faculté des Sciences de Tunis, Université El Manar, PO Box 248, El Manar II, 2092 Tunis (Tunisia); Univ Paris Diderot, Sorbonne Paris Cité, ITODYS, UMR 7086, CNRS, F-75013 Paris (France); Bakas, Idriss [Univ Paris Diderot, Sorbonne Paris Cité, ITODYS, UMR 7086, CNRS, F-75013 Paris (France); Laboratoire AQUAMAR, Equipe Matériaux Photocatalyse et Environnement, Faculté des Sciences, Université Ibn Zohr, B.P. 8106, Cité Dakhla, Agadir (Morocco); Piquemal, Jean-Yves; Nowak, Sophie [Univ Paris Diderot, Sorbonne Paris Cité, ITODYS, UMR 7086, CNRS, F-75013 Paris (France); Abderrabba, Manef, E-mail: abderrabbamanef@gmail.com [Laboratory of Materials, Molecules and Applications, IPEST, University of Carthage, Sidi Bou Said road, B.P. 51, 2070 La Marsa (Tunisia); Chehimi, Mohamed M., E-mail: chehimi@icmpe.cnrs.fr [Univ Paris Diderot, Sorbonne Paris Cité, ITODYS, UMR 7086, CNRS, F-75013 Paris (France); Université Paris Est, ICMPE (UMR7182), CNRS, UPEC, F-94320 Thiais (France)

    2016-03-30

    Graphical abstract: - Highlights: • Mesoporous silica/polyacrylamide nanocomposite adsorbent was prepared by UV-graft polymerization. • Polyacrylamide was successfully grafted onto the silanized mesoporous silica. • The Hg(II) adsorption capacity of the nanocomposite was as high as 177 mg g{sup −1} after 1 h at RT. • Adsorption process was found to fit pseudo second order kinetics and exothermic. - Abstract: MCM-41 ordered mesoporous silica was prepared, aminosilanized and grafted with polyacrylamide (PAAM) through in situ radical photopolymerization process. The resulting composite, denoted PAAM-NH{sub 2}-MCM-41, the calcined and silanized reference MCM-41s were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and N{sub 2} physisorption at 77 K. These complementary techniques brought strong supporting evidence for the silanization process followed by PAAM grafting. The surface composition was found to be PAAM-rich as judged by XPS. The composite was then employed for the uptake of Hg(II) from aqueous solutions. Adsorption was monitored versus pH, time, and temperature. The maximum adsorption capacity at 25 °C and pH 5.2 was 177 mg g{sup −1}. Kinetically, the equilibrium was reached within 60 min for a 100 mg L{sup −1} mercury solution. The adsorption of Hg(II) on PAAM-NH{sub 2}-MCM-41 composites followed second order kinetics. Thermodynamic parameters suggested that the favorable adsorption process is exothermic in nature and the adsorption is ascribed to a decrease in the degree of freedom of adsorbed ions which results in the entropy change. This work conclusively shows that mesoporous silica–polymer hybrid metal ion adsorbents (with robust silica–polymer interface) can be prepared in a simple way by in situ radical photopolymerization in the presence of

  15. Silica-gel modified with zirconium oxide as a novel 99Mo adsorbent 99mTc generators

    International Nuclear Information System (INIS)

    Salehi, H.; Mollarazi, E.; Abbasi, H.

    2010-01-01

    A new 99 Mo adsorbent has been prepared with modified silica gel with zirconium oxide (SiO 2 /ZrO 2 :Na 2 MoO 4 ) and used in technetium-99m generator. The adsorption behaviors of 99 Mo in the form of molybdate and 99m Tc in the form of pertechnetate on the new adsorbent was investigated showed that the adsorption capacity of molybdate on this generator was considerably higher than the usual generator with alumina column. Coating zirconium oxide on the surface of silica gel resulted in higher 99 Mo adsorption of this compound. 99m Tc is eluted with 0.9% NaCl, and the radionuclidic, radiochemical and chemical purities of the eluate were checked. This generator has a great potential as compared to the traditional alumina generators.

  16. Separation of pharmacologically active nitrogen-containing compounds on silica gels modified with 6,10-ionene, dextran sulfate, and gold nanoparticles

    Science.gov (United States)

    Ioutsi, A. N.; Shapovalova, E. N.; Ioutsi, V. A.; Mazhuga, A. G.; Shpigun, O. A.

    2017-12-01

    New stationary phases for HPLC are obtained via layer-by-layer deposition of polyelectrolytes and studied: (1) silica gel modified layer-by-layer with 6,10-ionene and dextran sulfate (Sorbent 1); (2) silica gel twice subjected to the above modification (Sorbent 2); and (3) silica gel modified with 6,10-ionene, gold nanoparticles, and dextran sulfate (Sorbent 3). The effect the content of the organic solvent in the mobile phase and the concentration and pH of the buffer solution have on the chromatographic behavior of several pharmacologically active nitrogen-containing compounds is studied. The sorbents are stable during the process and allow the effective separation of beta-blockers, calcium channel blockers, alpha-agonists, and antihistamines. A mixture of caffeine, nadolol, tetrahydrozoline, pindolol, orphenadrine, doxylamine, carbinoxamine, and chlorphenamine is separated in 6.5 min on the silica gel modified with 6,10-ionene, gold nanoparticles, and dextran sulfate.

  17. Synthesis and characterization of the superparamagnetic iron oxide nanoparticles modified with cationic chitosan and coated with silica shell

    International Nuclear Information System (INIS)

    Lewandowska-Łańcucka, Joanna; Staszewska, Magdalena; Szuwarzyński, Michał; Kępczyński, Mariusz; Romek, Marek; Tokarz, Waldemar; Szpak, Agnieszka; Kania, Gabriela; Nowakowska, Maria

    2014-01-01

    Highlights: • The new, facile methodology for synthesis of silica covered SPIONs is proposed. • The SPIONs was modified with cationic chitosan and coated with silica shell. • Negatively charged, rounded in shape particles of ca. 330 nm were obtained. • The product exhibits the superparamagnetic properties. • The product properties imply its potential applications in biomedicine areas. -- Abstract: Novel method for synthesis of superparamagnetic iron oxide nanoparticles (SPION) modified with a cationic chitosan (CCh) and coated with a silica shell, SPION-CCh-SiO 2 was developed. The process was carried out in two steps. In the first step the chitosan coated SPIONs were obtained by co-precipitation of Fe 2+ and Fe 3+ with ammonium hydroxide in aqueous solution of CCh. In the second one, the silica shell is formed on their surfaces. The formation of SPION-CCh-SiO 2 was achieved by direct decomposition of tetraethoxysilane (TEOS) adsorbed on a surface of SPION-CCh dispersed in aqueous phase under sonication and mechanical stirring at room temperature. The chemical composition and physicochemical properties of the materials were determined using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Dynamic Light Scattering (DLS) and zeta potential measurements. The morphology of the particles was evaluated by Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). Magnetic properties were confirmed using Atomic Force Microscopy/Magnetic Force Microscopy (AFM/MFM) and magnetization measurements. The resulting products are negatively charged, rounded in shape and exhibit the superparamagnetic properties what implies their potential applications in engineering and biomedicine areas

  18. Synthesis and characterization of the superparamagnetic iron oxide nanoparticles modified with cationic chitosan and coated with silica shell

    Energy Technology Data Exchange (ETDEWEB)

    Lewandowska-Łańcucka, Joanna, E-mail: lewandow@chemia.uj.edu.pl [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow (Poland); Staszewska, Magdalena; Szuwarzyński, Michał; Kępczyński, Mariusz [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow (Poland); Romek, Marek [Department of Cytology and Histology, Institute of Zoology, Jagiellonian University, Gronostajowa 9, 30-387 Krakow (Poland); Tokarz, Waldemar [Department of Solid State Physics, AGH University of Science and Technology, al. A. Mickiewicza 30, 30-059 Krakow (Poland); Szpak, Agnieszka; Kania, Gabriela; Nowakowska, Maria [Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow (Poland)

    2014-02-15

    Highlights: • The new, facile methodology for synthesis of silica covered SPIONs is proposed. • The SPIONs was modified with cationic chitosan and coated with silica shell. • Negatively charged, rounded in shape particles of ca. 330 nm were obtained. • The product exhibits the superparamagnetic properties. • The product properties imply its potential applications in biomedicine areas. -- Abstract: Novel method for synthesis of superparamagnetic iron oxide nanoparticles (SPION) modified with a cationic chitosan (CCh) and coated with a silica shell, SPION-CCh-SiO{sub 2} was developed. The process was carried out in two steps. In the first step the chitosan coated SPIONs were obtained by co-precipitation of Fe{sup 2+} and Fe{sup 3+} with ammonium hydroxide in aqueous solution of CCh. In the second one, the silica shell is formed on their surfaces. The formation of SPION-CCh-SiO{sub 2} was achieved by direct decomposition of tetraethoxysilane (TEOS) adsorbed on a surface of SPION-CCh dispersed in aqueous phase under sonication and mechanical stirring at room temperature. The chemical composition and physicochemical properties of the materials were determined using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Dynamic Light Scattering (DLS) and zeta potential measurements. The morphology of the particles was evaluated by Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). Magnetic properties were confirmed using Atomic Force Microscopy/Magnetic Force Microscopy (AFM/MFM) and magnetization measurements. The resulting products are negatively charged, rounded in shape and exhibit the superparamagnetic properties what implies their potential applications in engineering and biomedicine areas.

  19. 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.

  20. 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

  1. Physical Characteristics of Chitosan Based Film Modified With Silica and Polyethylene Glycol

    Directory of Open Access Journals (Sweden)

    F. Widhi Mahatmanti

    2014-07-01

    Full Text Available Recently, development of film materials is focused on finding the films with high chemical and physical stabilities. Organic based material such as chitosan produces films with low physical stability, and hence addition of inorganic materials necessary. In this research, the effect of silica and polyethylene glycol (PEG addition on the properties of chitosan based films has been investigated. Precursors used to produce films included chitosan with the deacetylation degree of 83% and sodium silicate solution as the silica source. A simple synthesis in a one-pot process was carried out by mixing 1%(w of chitosan solution in 2%(v/v acetate acid and sodium silicate solution (27% SiO2 in various composition ratios and casting the solution on a glass dish. The tensile strength and percentage of elongation decrease with increasing the silica content. The tensile strength tends to decline with addition of PEG, but the elongation percentage of the film increases. Hydrophilicity of the film decreases with the addition of silica and increases with the addition of PEG. The addition of silica and PEG does not change significantly the morphology of the film and functional groups indicating the domination of physical interaction among active sites in the film components.

  2. Chlorophyll a Covalently Bonded to Organo-Modified Translucent Silica Xerogels: Optimizing Fluorescence and Maximum Loading

    Directory of Open Access Journals (Sweden)

    M. A. García-Sánchez

    2016-07-01

    Full Text Available Chlorophyll is a pyrrolic pigment with important optical properties, which is the reason it has been studied for many years. Recently, interest has been rising with respect to this molecule because of its outstanding physicochemical properties, particularly applicable to the design and development of luminescent materials, hybrid sensor systems, and photodynamic therapy devices for the treatment of cancer cells and bacteria. More recently, our research group has been finding evidence for the possibility of preserving these important properties of substrates containing chlorophyll covalently incorporated within solid pore matrices, such as SiO2, TiO2 or ZrO2 synthesized through the sol-gel process. In this work, we study the optical properties of silica xerogels organo-modified on their surface with allyl and phenyl groups and containing different concentrations of chlorophyll bonded to the pore walls, in order to optimize the fluorescence that these macrocyclic species displays in solution. The intention of this investigation was to determine the maximum chlorophyll a concentration at which this molecule can be trapped inside the pores of a given xerogel and to ascertain if this pigment remains trapped as a monomer, a dimer, or aggregate. Allyl and phenyl groups were deposited on the surface of xerogels in view of their important effects on the stability of the molecule, as well as over the fluorescence emission of chlorophyll; however, these organic groups allow the trapping of either chlorophyll a monomers or dimers. The determination of the above parameters allows finding the most adequate systems for subsequent in vitro or in vivo studies. The characterization of the obtained xerogels was performed through spectroscopic absorption, emission and excitation spectra. These hybrid systems can be employed as mimics of natural systems; the entrapment of chlorophyll inside pore matrices indicates that it is possible to exploit some of the most

  3. Chlorophyll a Covalently Bonded to Organo-Modified Translucent Silica Xerogels: Optimizing Fluorescence and Maximum Loading.

    Science.gov (United States)

    García-Sánchez, M A; Serratos, I N; Sosa, R; Tapia-Esquivel, T; González-García, F; Rojas-González, F; Tello-Solís, S R; Palacios-Enriquez, A Y; Esparza Schulz, J M; Arrieta, A

    2016-07-22

    Chlorophyll is a pyrrolic pigment with important optical properties, which is the reason it has been studied for many years. Recently, interest has been rising with respect to this molecule because of its outstanding physicochemical properties, particularly applicable to the design and development of luminescent materials, hybrid sensor systems, and photodynamic therapy devices for the treatment of cancer cells and bacteria. More recently, our research group has been finding evidence for the possibility of preserving these important properties of substrates containing chlorophyll covalently incorporated within solid pore matrices, such as SiO₂, TiO₂ or ZrO₂ synthesized through the sol-gel process. In this work, we study the optical properties of silica xerogels organo-modified on their surface with allyl and phenyl groups and containing different concentrations of chlorophyll bonded to the pore walls, in order to optimize the fluorescence that these macrocyclic species displays in solution. The intention of this investigation was to determine the maximum chlorophyll a concentration at which this molecule can be trapped inside the pores of a given xerogel and to ascertain if this pigment remains trapped as a monomer, a dimer, or aggregate. Allyl and phenyl groups were deposited on the surface of xerogels in view of their important effects on the stability of the molecule, as well as over the fluorescence emission of chlorophyll; however, these organic groups allow the trapping of either chlorophyll a monomers or dimers. The determination of the above parameters allows finding the most adequate systems for subsequent in vitro or in vivo studies. The characterization of the obtained xerogels was performed through spectroscopic absorption, emission and excitation spectra. These hybrid systems can be employed as mimics of natural systems; the entrapment of chlorophyll inside pore matrices indicates that it is possible to exploit some of the most physicochemical

  4. Cu(II) recognition materials: Fluorophores grafted on mesoporous silica supports

    International Nuclear Information System (INIS)

    Kledzik, Krzysztof; Orlowska, Maja; Patralska, Dorota; Gwiazda, Marcin; Jezierska, Julia; Pikus, Stanislaw; Ostaszewski, Ryszard; Klonkowski, Andrzej M.

    2007-01-01

    There were designed and synthesized naphthalene and pyrene derivatives consisting of fluorophore group and of receptor fragment with donor N and O atoms. These fluorosensors were covalently attached by grafting carboxyl group to surfaces of silica xerogel or mesoporous silicas (MCM-41 and MCM-48) functionalized either with 3-aminopropyl or 3-glycidoxypropyl groups. The pyrene derivatives 2 and 3 covalently grafted on MCM-48 silica functionalized with 3-aminopropyl groups are potential recognition elements of a fluorescence chemical sensor. Fluorescence emission of the prepared recognition materials is quenched specifically owing to photoinduced electron transfer (PET) effect after coordination reactions with Cu(II) ions. Moreover, both the materials exhibit selectivity for Cu(II) ions in aqueous solutions in presence of such metal ions as: alkali, alkaline earth and transition. During UV irradiation the studied recognition elements undergo slowly photochemical degradation

  5. Thermogravimetric analyses and mineralogical study of polymer modified mortar with silica fume

    Directory of Open Access Journals (Sweden)

    Alessandra Etuko Feuzicana de Souza Almeida

    2006-09-01

    Full Text Available Mineral and organic additions are often used in mortars to improve their properties. Microstructural investigation concerning the effects of styrene acrylic polymer and silica fume on the mineralogical composition of high-early-strength portland cement pastes after 28 days of hydration are presented in this paper. Thermogravimetry and derivative thermogravimetry were used to study the interaction between polymers and cement, as well as the extent of pozzolanic reaction of the mortars with silica fume. Differential scanning calorimetry and X ray diffraction were used to investigate the cement hydration and the effect of the additions. The results showed that the addition of silica fume and polymer reduces the portlandite formation due to delaying of Portland cement hydration and pozzolanic reaction.

  6. Synthesis and Characterization of Hyaluronic Acid Modified Colloidal Mesoporous Silica Nanoparticles

    Science.gov (United States)

    Zhang, Wenbiao; Wang, Yu; Li, Zhen; Wang, Wanxia; Sun, Honghao; Liu, Mingxing

    2017-12-01

    The colloidal mesoporous silica nanoparticles functionalized with hyaluronic acid (CMS-HA) were successfully synthesized by grafting hyaluronic acid onto the external surface of the amino-functionalized mesoporous silica nanoparticles (CMS-NH2). Moreover, the paticle properties of CMS-HA were characterized by fourier transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS) and transmission electron microscopy (TEM). The nanomaterials were negatively charged and had a relatively uniform spherical morphology with about 100 nm in diameter, which could make it more compatible with blood. So the results suggested that the CMS-HA might be a critical nanomaterial for applying in target drug delivery system.

  7. Organically Modified Silica Nanoparticles Interaction with Macrophage Cells: Assessment of Cell Viability on the Basis of Physicochemical Properties.

    Science.gov (United States)

    Kumar, Dhiraj; Mutreja, Isha; Keshvan, Prashant C; Bhat, Madhusudan; Dinda, Amit K; Mitra, Susmita

    2015-11-01

    Silica nanoparticles have drawn a lot of attention for nanomedicine application, and this is attributed to their biocompatibility and ease of surface functionalization. However, successful utilization of these inorganic systems for biomedical application depends on their physicochemical properties. This study, therefore, discusses in vitro toxicity of organically modified silica nanoparticles on the basis of size, shape, and surface properties of silica nanoparticles. Spherical- and oval-shaped nanoparticles having hydroxyl and amine groups were synthesized in Tween 80 micelles using different organosilanes. Nanoparticles of similar size and morphology were considered for comparative assessment. "As-prepared" nanoparticles were characterized in terms of size, shape, and surface properties using ZetaSizer, transmission electron microscopy, and Fourier transform infrared to establish the above parameters. In vitro analysis in terms of nanoparticle-based toxicity was performed on J-774 (macrophage) cell line using propidium iodide-4',6-diamidino-2-phenylindol and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assays. Fluorescent dye-entrapped nanoparticles were used to visualize the uptake of the nanoparticles by macrophage cells. Results from cell studies suggested low levels of toxicity for different nanoparticle formulations studied, therefore are suitable for nanocarrier application for poorly soluble molecules. On the contrary, the nanoparticles of similar size and shape, having amine groups and low net negative charge, do not exhibit any in vitro cytotoxicity. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  8. 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

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

    Czech Academy of Sciences Publication Activity Database

    Zeleňák, V.; Badaničová, M.; Halamová, D.; Čejka, Jiří; Zukal, Arnošt; Murafa, Nataliya; Goerigk, G.

    2008-01-01

    Roč. 144, č. 2 (2008), s. 336-342 ISSN 1385-8947 R&D Projects: GA ČR GA203/08/0604 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z40320502 Keywords : mesoporous silica * hexagonal * amine * carbon dioxide Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.813, year: 2008

  10. Dihydrogenimidazole modified silica-sulfonated poly(ether ether ketone) hybrid materials as electrolyte membranes for direct ethanol fuel cells

    International Nuclear Information System (INIS)

    Roelofs, Kimball S.; Hirth, Thomas; Schiestel, Thomas

    2011-01-01

    The present study reports on dihydrogenimidazole modified inorganic-organic mixed matrix membranes for possible application as a proton exchange membrane in direct ethanol fuel cells. The polymeric phase consisted mainly of sulfonated poly(ether ether ketone) (sPEEK) with a sulfonation degree of 55%. The inorganic phase was built up from hydrophilic fumed silica particles interconnected with partially hydrolyzed and condensed tetraethoxysilane with a total inorganic loading of 27.3%. This inorganic phase was further modified with N-(3-triethoxysilylpropyl)-4,5-dihydroimidazole (DHIM), which consists of an hydrolyzable inorganic part and a functional organic group. The influence of the modifier on the mixed matrix system was studied by means of various modifier concentrations in various aqueous-ethanolic systems (water, 2 M and 4 M ethanol). Modifier concentration and ethanol concentration of the ethanol-water mixture exhibited significant but opposite effects on the liquid uptake of the mixed matrix membranes. The proton conductivity as well as the proton diffusion coefficient as a function of modifier content showed a linear decrease. The proton conductivity as a function of temperature showed Arrhenius behavior and the activation energy of the mixed matrix membranes was 43.9 ± 2.6 kJ mol -1 . High selectivity of proton diffusion coefficient to ethanol permeability coefficient was obtained with high modifier concentrations. At low modifier concentrations, this selectivity was dominated by ethanol permeation and at high modifier concentrations by proton diffusion. The main electrolyte properties can be optimized by setting the DHIM content in mixed matrix membrane. With this approach, tailor-made membranes can be prepared for possible application in direct ethanol fuel cells.

  11. Dihydrogenimidazole modified silica-sulfonated poly(ether ether ketone) hybrid materials as electrolyte membranes for direct ethanol fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Roelofs, Kimball S.; Hirth, Thomas [Fraunhofer Institute for Interfacial Engineering and Biotechnology, Nobelstr. 12, 70569 Stuttgart (Germany); Schiestel, Thomas, E-mail: Thomas.Schiestel@igb.fraunhofer.de [Fraunhofer Institute for Interfacial Engineering and Biotechnology, Nobelstr. 12, 70569 Stuttgart (Germany)

    2011-05-25

    The present study reports on dihydrogenimidazole modified inorganic-organic mixed matrix membranes for possible application as a proton exchange membrane in direct ethanol fuel cells. The polymeric phase consisted mainly of sulfonated poly(ether ether ketone) (sPEEK) with a sulfonation degree of 55%. The inorganic phase was built up from hydrophilic fumed silica particles interconnected with partially hydrolyzed and condensed tetraethoxysilane with a total inorganic loading of 27.3%. This inorganic phase was further modified with N-(3-triethoxysilylpropyl)-4,5-dihydroimidazole (DHIM), which consists of an hydrolyzable inorganic part and a functional organic group. The influence of the modifier on the mixed matrix system was studied by means of various modifier concentrations in various aqueous-ethanolic systems (water, 2 M and 4 M ethanol). Modifier concentration and ethanol concentration of the ethanol-water mixture exhibited significant but opposite effects on the liquid uptake of the mixed matrix membranes. The proton conductivity as well as the proton diffusion coefficient as a function of modifier content showed a linear decrease. The proton conductivity as a function of temperature showed Arrhenius behavior and the activation energy of the mixed matrix membranes was 43.9 {+-} 2.6 kJ mol{sup -1}. High selectivity of proton diffusion coefficient to ethanol permeability coefficient was obtained with high modifier concentrations. At low modifier concentrations, this selectivity was dominated by ethanol permeation and at high modifier concentrations by proton diffusion. The main electrolyte properties can be optimized by setting the DHIM content in mixed matrix membrane. With this approach, tailor-made membranes can be prepared for possible application in direct ethanol fuel cells.

  12. Silica-modified Fe-doped calcium sulfide nanoparticles for in vitro and in vivo cancer hyperthermia

    International Nuclear Information System (INIS)

    Wu, Steven Yueh-Hsiu; Yang, Kai-Chiang; Tseng, Ching-Li; Chen, Jung-Chih; Lin, Feng-Huei

    2011-01-01

    In this study, sulfide-based magnetic Fe-doped CaS nanoparticles modified with a silica layer were investigated for cancer hyperthermia. A polyvinyl pyrrolidone polymer was used as the coupling agent. The developed nanoparticles contained 11.6 wt% iron concentration, and their X-ray diffraction pattern was similar to those of CaS and Fe–CaS nanoparticles. The average particle size was approximately 47.5 nm and homogeneously dispersed in aqueous solutions. The major absorption bands of silica were observed from the FTIR spectrum. The magnetic properties and heating efficiency were also examined. The specific absorption ratio of nanoparticles at a concentration of 10 mg/mL at 37 °C in an ethanol carrier fluid was 37.92 W/g, and the nanoparticles would raise the temperature to over 45 °C within 15 min. A cytotoxicity analysis revealed that the nanoparticles had good biocompatibility, which indicated that the nanoparticles did not affect cell viability. The therapeutic effects of the nanoparticles were investigated using in vitro and animal studies. Cells seeded with nanoparticles and treated under an AC magnetic field revealed a percentage of cytotoxicity (60%) that was significantly higher from that in other groups. In the animal study, during a hyperthermia period of 15 days, tumor-bearing Balb/c mice that were subcutaneously injected with nanoparticles and exposed to an AC magnetic field manifested a reduction in tumor volume. The newly developed silica-modified Fe–CaS nanoparticles can thus be considered a promising and attractive hyperthermia thermoseed.

  13. Osseointegration properties of titanium dental implants modified with a nanostructured coating based on ordered porous silica and bioactive glass nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Covarrubias, Cristian, E-mail: ccovarrubias@odontologia.uchile.cl [Laboratory of Nanobiomaterials, Institute for Research in Dental Sciences, Faculty of Dentistry, University of Chile, Santiago (Chile); Mattmann, Matías [Laboratory of Nanobiomaterials, Institute for Research in Dental Sciences, Faculty of Dentistry, University of Chile, Santiago (Chile); Von Marttens, Alfredo [Department of Prosthesis, Faculty of Dentistry, University of Chile, Santiago (Chile); Caviedes, Pablo; Arriagada, Cristián [Laboratory of Cell Therapy, ICBM, Faculty of Medicine, University of Chile (Chile); Valenzuela, Francisco [Laboratory of Nanobiomaterials, Institute for Research in Dental Sciences, Faculty of Dentistry, University of Chile, Santiago (Chile); Rodríguez, Juan Pablo [Laboratory of Cell Biology, INTA, University of Chile, Santiago (Chile); Corral, Camila [Department of Restorative Dentistry, Faculty of Dentistry, University of Chile, Santiago (Chile)

    2016-02-15

    Graphical abstract: - Highlights: • The fabrication of a coating for osseointegration of titanium implant is presented. • The coating consists of nanoporous silica loaded with bioactive glass nanoparticles. • Coating accelerates the in vitro formation of apatite in simulated body fluid. • Coating promotes the osteogenic differentiation of stem cells. • Coating accelerates the formation of bone tissue in the periphery of the implant. - Abstract: The fabrication of a nanoporous silica coating loaded with bioactive glass nanoparticles (nBG/NSC) on titanium dental implant surface and its in vitro and in vivo evaluation is presented. The coating was produced by a combined sol–gel and evaporation induced self-assembly process. In vitro bioactivity was assessed in simulated body fluid (SBF) and investigating the osteogenic differentiation of human bone marrow mesenchymal stem cells (hBMSCs). A rat tibial model was employed to analyze the bone response to nBG/NSC-modified titanium implant surface in vivo. The nBG/NSC coating was confirmed at nano level to be constituted by a highly ordered nanoporous silica structure. The coating nanotopography in conjunction with the bioactivity of the BG particles accelerate the in vitro apatite formation and promote the osteogenic differentiation of hBMSCs in absence of osteogenic supplements. These properties accelerate the formation of bone tissue in the periphery of the implant after 3 weeks of implantation. Backscattered scanning electron microscopy images revealed the presence of gaps and soft tissue in the unmodified implant after 6 weeks, whereas the nBG/NSC-modified implant showed mature bone in intimate contact with the implant surface. The nBG/NSC coating appears promising for accelerating the osseointegration of dental implants.

  14. Osseointegration properties of titanium dental implants modified with a nanostructured coating based on ordered porous silica and bioactive glass nanoparticles

    International Nuclear Information System (INIS)

    Covarrubias, Cristian; Mattmann, Matías; Von Marttens, Alfredo; Caviedes, Pablo; Arriagada, Cristián; Valenzuela, Francisco; Rodríguez, Juan Pablo; Corral, Camila

    2016-01-01

    Graphical abstract: - Highlights: • The fabrication of a coating for osseointegration of titanium implant is presented. • The coating consists of nanoporous silica loaded with bioactive glass nanoparticles. • Coating accelerates the in vitro formation of apatite in simulated body fluid. • Coating promotes the osteogenic differentiation of stem cells. • Coating accelerates the formation of bone tissue in the periphery of the implant. - Abstract: The fabrication of a nanoporous silica coating loaded with bioactive glass nanoparticles (nBG/NSC) on titanium dental implant surface and its in vitro and in vivo evaluation is presented. The coating was produced by a combined sol–gel and evaporation induced self-assembly process. In vitro bioactivity was assessed in simulated body fluid (SBF) and investigating the osteogenic differentiation of human bone marrow mesenchymal stem cells (hBMSCs). A rat tibial model was employed to analyze the bone response to nBG/NSC-modified titanium implant surface in vivo. The nBG/NSC coating was confirmed at nano level to be constituted by a highly ordered nanoporous silica structure. The coating nanotopography in conjunction with the bioactivity of the BG particles accelerate the in vitro apatite formation and promote the osteogenic differentiation of hBMSCs in absence of osteogenic supplements. These properties accelerate the formation of bone tissue in the periphery of the implant after 3 weeks of implantation. Backscattered scanning electron microscopy images revealed the presence of gaps and soft tissue in the unmodified implant after 6 weeks, whereas the nBG/NSC-modified implant showed mature bone in intimate contact with the implant surface. The nBG/NSC coating appears promising for accelerating the osseointegration of dental implants.

  15. 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.

  16. Voltammetric Determination of Lead (II) and Cadmium (II) Using a Bismuth Film Electrode Modified with Mesoporous Silica Nanoparticles

    International Nuclear Information System (INIS)

    Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

    2014-01-01

    A new chemically modified glassy carbon electrode based on bismuth film coated mesoporous silica nanoparticles was developed and evaluated for reliable quantification of trace Pb 2+ and Cd 2+ by anodic stripping square wave voltammetry in natural water samples. Compared with conventional bismuth film electrodes or bismuth nanoparticles modified electrodes, this electrode exhibited significantly improved sensitivity and stability for Pb 2+ and Cd 2+ detection. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 2-150 μg L −1 with a detect limit of 0.2 μg L −1 for Pb 2+ , and 0.6 μg L −1 for Cd 2+ for 120s deposition. Good reproducibility was achieved on both single and equally prepared electrodes. In addition, scanning electron microscopy reveals that fibril-like bismuth structures were formed on silica nanoparticles, which could be responsible for the improved voltammetric performance due to the enhanced surface area. Finally, the developed electrode was applied to determine Pb 2+ and Cd 2+ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb 2+ and Cd 2+

  17. Mechanical and chemical properties of polyvinyl alcohol modified cement mortar with silica fume used as matrix including radioactive waste

    International Nuclear Information System (INIS)

    Dakroury, A. M.

    2007-01-01

    This paper discussed the mechanical and chemical properties of polyvinyl alcohol - modified cement mortar with silica fume to assess the safety for disposal of radioactive waste. The modified cement mortars containing polyvinyl alcohol (PVA) in the presence of 10 % silica fume (SF) .The chemical reaction between polymer and cement - hydrated product were investigated by the Infrared Spectral Technology, Differential Thermal Analysis and X-ray diffraction. The leaching of 137Cs from a waste composite into a surrounding fluid has been studied .The results shown that PVA increases the strength and decreases the porosity. The increase in strength duo to the interaction of PVA with cement , may be forming some new compound that fill the pores or improve the bond between the cement . The pozzolanic reaction of the SF increases the calcium silicate hydrates in the hardening matrix composites. There is distinct change in the refinement of the pore structure in cement composites giving fewer capillary pores and more of the finer gel pores

  18. Osseointegration properties of titanium dental implants modified with a nanostructured coating based on ordered porous silica and bioactive glass nanoparticles

    Science.gov (United States)

    Covarrubias, Cristian; Mattmann, Matías; Von Marttens, Alfredo; Caviedes, Pablo; Arriagada, Cristián; Valenzuela, Francisco; Rodríguez, Juan Pablo; Corral, Camila

    2016-02-01

    The fabrication of a nanoporous silica coating loaded with bioactive glass nanoparticles (nBG/NSC) on titanium dental implant surface and its in vitro and in vivo evaluation is presented. The coating was produced by a combined sol-gel and evaporation induced self-assembly process. In vitro bioactivity was assessed in simulated body fluid (SBF) and investigating the osteogenic differentiation of human bone marrow mesenchymal stem cells (hBMSCs). A rat tibial model was employed to analyze the bone response to nBG/NSC-modified titanium implant surface in vivo. The nBG/NSC coating was confirmed at nano level to be constituted by a highly ordered nanoporous silica structure. The coating nanotopography in conjunction with the bioactivity of the BG particles accelerate the in vitro apatite formation and promote the osteogenic differentiation of hBMSCs in absence of osteogenic supplements. These properties accelerate the formation of bone tissue in the periphery of the implant after 3 weeks of implantation. Backscattered scanning electron microscopy images revealed the presence of gaps and soft tissue in the unmodified implant after 6 weeks, whereas the nBG/NSC-modified implant showed mature bone in intimate contact with the implant surface. The nBG/NSC coating appears promising for accelerating the osseointegration of dental implants.

  19. Synthesis and Characterization of Meso porous Material Functionalized with Different Silylating Agent and Their Capability to Remove Cu2+

    International Nuclear Information System (INIS)

    Zaini Hamzah; Norhidayu Narawi; Hamizah Mohd Rasid; Amira Nazirah Mohd Yusoff

    2012-01-01

    Meso porous material MCM-41 with uniform hexagonally ordered pores in range of 2-10 nm was synthesized through hydrothermal method. The synthesis started from highly pure silica source known as Ludox which act as an active source of silica in the presence of organic surfactant (CTABr) as structure-directing agent. MCM-41 has been functionalized with the organic group known as 3-aminopropyltriethoxysilane (APTES), 3-mercaptopropyltrimethoxysilane (MPTMS), and chloropropyl triethoxysilane (CPTES) by co-condensation method in order to enhance the surface hydrophobicity of MCM-41. The increasing hydrophobicity will lead to efficient reaction specifically for organic reaction in organic solvent. The resulting materials were characterized with various techniques which are PXRD, FTIR, NMR, Elemental Analysis and AAS. The formation of uniform hexagonal framework of synthesized materials was shown in PXRD result. The functionalized groups of modified MCM-41 can be characterized via FTIR and 13 C-NMR results. The Elemental Analysis shows the percentage of nitrogen, carbon, hydrogen and sulphur in MCM-41 and functionalized MCM-41. From AAS, MCM-41 MPTMS has high capability for removal of Cu (II) in aqueous solution compared with others. (author)

  20. short communication mesoporous molecular sieve mcm-41

    African Journals Online (AJOL)

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    Department of Chemistry, School of Science, Alzahra University, Vanak, Tehran, Iran ... An efficient synthesis of 3,4-dihydro-2(1H)-pyrimidinones and -thiones using ... Some marine alkaloids recently isolated have been attributed to the.

  1. Evaluation of superparamagnetic and biocompatible properties of mesoporous silica coated cobalt ferrite nanoparticles synthesized via microwave modified Pechini method

    Energy Technology Data Exchange (ETDEWEB)

    Gharibshahian, M. [Faculty of New Sciences and Technologies, Semnan University, Semnan (Iran, Islamic Republic of); Mirzaee, O., E-mail: O_mirzaee@semnan.ac.ir [Faculty of Materials and Metallurgical Engineering, Semnan University, Semnan (Iran, Islamic Republic of); Nourbakhsh, M.S. [Faculty of New Sciences and Technologies, Semnan University, Semnan (Iran, Islamic Republic of)

    2017-03-01

    Cobalt ferrite nano particles were synthesized by Pechini sol-gel method and calcined at 700 °C in electrical and microwave furnace. The microwave calcined sample was coated with mesoporous silica by hydrothermal method. Characterization was performed by XRD, FESEM, TEM, VSM, BET and FTIR analysis. The cytotoxicity was evaluated by MTT assay with 3T3 fibroblast cells. The XRD and FTIR results confirmed spinal formation in both cases and verified the formation of silica coating on the nanoparticles. For microwave calcination, The XRD and SEM results demonstrated smaller and flat adhesion forms of nanoparticles with the average size of 15 nm. The VSM results demonstrated nearly superparamagnetic nanoparticles with significant saturation magnetization equal to 64 emu/g. By coating, saturation magnetization was decreased to 36 emu/g. Moreover, the BET results confirmed the formation of mesoporous coating with the average pore diameters of 2.8 nm and average pore volume of 0.82 cm{sup 3} g{sup −1}. Microwave calcined nanoparticles had the best structural and magnetic properties. - Highlights: • CoFe{sub 2}O{sub 4} nanoparticles were synthesized using the microwave modified Pechini method. • The Effect of calcination route and silica coating on NPs properties was studied. • The nearly superparamagnetic nanoparticles were achieved by microwave calcination. • MFC NPs had the best magnetic properties and MTT assay showed no toxicity for MFC-MSC NPs. • A useful scheme was designed to achieve biological superparamagnetic core/shell NPs.

  2. Autogenous Deformation and Change of the Relative Humidity in Silica Fume-Modified Cement Paste

    DEFF Research Database (Denmark)

    Jensen, Ole mejlhede; Hansen, Per Freiesleben

    1996-01-01

    Even during sealed curing and at a constant temperature a hardening cement paste will deform and the relative humidity within its pores will lower. This autogenous deformation and autogenous relative humidity change may be so significant that the cement paste cracks if the deformation is restrained....... This article focuses on the influence of silica fume addition on autogenous deformation and autogenous relative humidity change. Continuous measurement of autogenous deformation and autogenous relative humidity change for more than 1 year and 1« years, respectively, was performed. The investigations show...... thatsilica fume addition markedly increases the autogenous shrinkage as well as the autogenous relative humidity change....

  3. Influence of surface modified nanoilmenite/amorphous silica composite particles on the thermal stability of cold galvanizing coating

    Directory of Open Access Journals (Sweden)

    A.M. Al-Sabagh

    2018-03-01

    Full Text Available The present approach investigates the use of novel nanoilmenite/amorphous silica composite (NI/AS particles fabricated from ilmenite nanoparticles (FeTiO3 NPs and synthesized amorphous silica grains to improve thermal stability of the cold galvanizing coating. Transmission electron microscopic (TEM images demonstrated that both nanoilmenite and nanocomposite particles were of flaky-like nature and the average diameter of the particles is 20 nm. The lamellar shape of the nanocomposite and spherical nature of Zn-dust particles were illustrated by scanning electron microscopy (SEM micrographs. Different alkyd-based cold galvanizing coating formulations were modified using uniformly dispersing various amounts of the processed nanocomposite particles as a modifier to form some engineering nanocomposite coatings. Thermal stability of the nanocomposite and Zn-dust particles was determined by thermo-gravimetric analysis (TGA. From the obtained results it could be observed that the weight loss (% as a feature of the thermal stability in case of the nanocomposite particles was 2.9 compared to 85.9 for Zn-dust powder grains. Derivative thermo-gravimetric (DTG measurements were done under nitrogen atmosphere for the cured cold galvanizing coating samples heated from room temperature to 1000 °C. The obtained results revealed that the maximum decomposition temperature point in the third degradation step for 6% nanocomposite surface modified cured sample (CG-F was detected at 693 °C and was less value for unmodified conventional cold galvanizing coating (CG-A at 612 °C. The increase in thermal stability with increasing the concentration of nanocomposite particles could be mainly attributed to the interface surface interaction between the nanocomposite particles and alkyd resin matrix in which enhancing the inorganic-organic network stiffness by causing a reduction in the total free spaces and enhancement in the cross-linking density of the cured film

  4. Functionalized mesoporous silica nanoparticles for oral delivery of budesonide

    Energy Technology Data Exchange (ETDEWEB)

    Yoncheva, K., E-mail: krassi.yoncheva@gmail.com [Department of Pharmaceutical Technology, Faculty of Pharmacy, Medical University of Sofia, 2 Dunav Str., 1000 Sofia (Bulgaria); Popova, M. [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, Sofia (Bulgaria); Szegedi, A.; Mihaly, J. [Institute of Nanochemistry and Catalysis, Chemical Research Center, Hungarian Academy of Sciences, Pusztaszeri út. 59-67, 1025 Budapest (Hungary); Tzankov, B.; Lambov, N.; Konstantinov, S.; Tzankova, V. [Department of Pharmaceutical Technology, Faculty of Pharmacy, Medical University of Sofia, 2 Dunav Str., 1000 Sofia (Bulgaria); Pessina, F.; Valoti, M. [Dipartimento di Scienze della Vita, Universita di Siena, via Aldo Moro 2, Siena (Italy)

    2014-03-15

    Non-functionalized and amino-functionalized mesoporous silica nanoparticle were loaded with anti-inflammatory drug budesonide and additionally post-coated with bioadhesive polymer (carbopol). TEM images showed spherical shape of the nanoparticles and slightly higher polydispersity after coating with carbopol. Nitrogen physisorption and thermogravimetic analysis revealed that more efficient loading and incorporation into the pores of nanoparticles was achieved with the amino-functionalized silica carrier. Infrared spectra indicated that the post-coating of these nanoparticles with carbopol led to the formation of bond between amino groups of the functionalized carrier and carboxyl groups of carbopol. The combination of amino-functionalization of the carrier with the post-coating of the nanoparticles sustained budesonide release. Further, an in vitro model of inflammatory bowel disease showed that the cytoprotective effect of budesonide loaded in the post-coated silica nanoparticles on damaged HT-29 cells was more pronounced compared to the cytoprotection obtained with pure budesonide. -- Graphical abstract: Silica mesoporous MCM-41 particles were amino-functionalized, loaded with budesonide and post-coated with bioadhesive polymer (carbopol) in order to achieve prolonged residence of anti-inflammatory drug in GIT. Highlights: • Higher drug loading in amino-functionalized mesoporous silica. • Amino-functionalization and post-coating of the nanoparticles sustained drug release. • Achievement of higher cytoprotective effect with drug loaded into the nanoparticles.

  5. High-Yield and Sustainable Production of Phosphatidylserine in Purely Aqueous Solutions via Adsorption of Phosphatidylcholine on Triton-X-100-Modified Silica.

    Science.gov (United States)

    Zhang, Xiaoli; Li, Binglin; Wang, Jiao; Li, Huanyu; Zhao, Binxia

    2017-12-13

    Triton X-100 was covalently bound to a surface of silica and acted as an anchor molecule to facilitate the adsorption of phosphatidylcholine (PC) in a purely aqueous solution. The silica-adsorbed PC obtained was successfully used for phospholipase D (PLD)-mediated transphosphatidylation in the production of phosphatidylserine (PS). Organic solvents were completely avoided in the whole production process. The PC loading and PS yield reached 98.9 and 99.0%, respectively. Two adsorption models were studied, and the relevant parameters were calculated to help us understand the adsorption and reaction processes deeply. In addition, the silica-adsorbed PC provides a promising way to continuously biosynthesize PS. A packed-bed reactor was employed to demonstrate the process flow of the continuous production of PS. The recyclability and stability of the Triton-X-100-modified silica were excellent, as demonstrated by its use 30 times during continuous operation without any loss of the productivity.

  6. 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.

  7. Molecular insight into nanoscale water films dewetting on modified silica surfaces.

    Science.gov (United States)

    Zhang, Jun; Li, Wen; Yan, Youguo; Wang, Yefei; Liu, Bing; Shen, Yue; Chen, Haixiang; Liu, Liang

    2015-01-07

    In this work, molecular dynamics simulations are adopted to investigate the microscopic dewetting mechanism of nanoscale water films on methylated silica surfaces. The simulation results show that the dewetting process is divided into two stages: the appearance of dry patches and the quick contraction of the water film. First, the appearance of dry patches is due to the fluctuation in the film thickness originating from capillary wave instability. Second, for the fast contraction of water film, the unsaturated electrostatic and hydrogen bond interactions among water molecules are the driving forces, which induce the quick contraction of the water film. Finally, the effect of film thickness on water films dewetting is studied. Research results suggest that upon increasing the water film thickness from 6 to 8 Å, the final dewetting patterns experience separate droplets and striation-shaped structures, respectively. But upon further increasing the water film thickness, the water film is stable and there are no dry patches. The microscopic dewetting behaviors of water films on methylated silica surfaces discussed here are helpful in understanding many phenomena in scientific and industrial processes better.

  8. Cheap C18-modified silica monolith particles as HPLC stationary phase of good separation efficiency

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Ashraf; Ali, Faiz; Cheong, Woo Jo [Dept. of of Chemistry, Inha University, Incheon (Korea, Republic of)

    2015-06-15

    The columns packed with particles have a high efficiency but they are accompanied with a high column back pressure due to lower permeability, while the monolithic columns have a high permeability but they result in inferior separation efficiency for the analysis of small molecules in HPLC. In our laboratory,we have been using the pseudo-monolithic silica particles with C-18 ligand or polystyrene film. The column to column reproducibility was evaluated based on three columns made of three different batches of silica monolith particles, and better than 4.5% in N, and 1.6% in retention time were observed. The day to day reproducibility of a single column for three consecutive days was found better than 1.5% both in N and retention time. The van Deemter plots were derived for awide range of flow rates. The trends of van Deemter plots were similar to those of common patterns and the optimal flow rate was found to be 25 μL/min.

  9. Ultra-small dye-doped silica nanoparticles via modified sol-gel technique

    Science.gov (United States)

    Riccò, R.; Nizzero, S.; Penna, E.; Meneghello, A.; Cretaio, E.; Enrichi, F.

    2018-05-01

    In modern biosensing and imaging, fluorescence-based methods constitute the most diffused approach to achieve optimal detection of analytes, both in solution and on the single-particle level. Despite the huge progresses made in recent decades in the development of plasmonic biosensors and label-free sensing techniques, fluorescent molecules remain the most commonly used contrast agents to date for commercial imaging and detection methods. However, they exhibit low stability, can be difficult to functionalise, and often result in a low signal-to-noise ratio. Thus, embedding fluorescent probes into robust and bio-compatible materials, such as silica nanoparticles, can substantially enhance the detection limit and dramatically increase the sensitivity. In this work, ultra-small fluorescent silica nanoparticles (NPs) for optical biosensing applications were doped with a fluorescent dye, using simple water-based sol-gel approaches based on the classical Stöber procedure. By systematically modulating reaction parameters, controllable size tuning of particle diameters as low as 10 nm was achieved. Particles morphology and optical response were evaluated showing a possible single-molecule behaviour, without employing microemulsion methods to achieve similar results. [Figure not available: see fulltext.

  10. Heavy metals adsorption by novel EDTA-modified chitosan-silica hybrid materials.

    Science.gov (United States)

    Repo, Eveliina; Warchoł, Jolanta K; Bhatnagar, Amit; Sillanpää, Mika

    2011-06-01

    Novel adsorbents were synthesized by functionalizing chitosan-silica hybrid materials with (ethylenediaminetetraacetic acid) EDTA ligands. The synthesized adsorbents were found to combine the advantages of both silica gel (high surface area, porosity, rigid structure) and chitosan (surface functionality). The Adsorption potential of hybrid materials was investigated using Co(II), Ni(II), Cd(II), and Pb(II) as target metals by varying experimental conditions such as pH, contact time, and initial metal concentration. The kinetic results revealed that the pore diffusion process played a key role in adsorption kinetics, which might be attributed to the porous structure of synthesized adsorbents. The obtained maximum adsorption capacities of the hybrid materials for the metal ions ranged from 0.25 to 0.63 mmol/g under the studied experimental conditions. The adsorbent with the highest chitosan content showed the best adsorption efficiency. Bi-Langmuir and Sips isotherm model fitting to experimental data suggested the surface heterogeneity of the prepared adsorbents. In multimetal solutions, the hybrid adsorbents showed the highest affinity toward Pb(II). Copyright © 2011 Elsevier Inc. All rights reserved.

  11. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    Science.gov (United States)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-11-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound.

  12. Production of liquid alkanes by controlling reactivity of sorbitol hydrogenation with a Ni/HZSM-5 catalyst in water

    International Nuclear Information System (INIS)

    Zhang, Qing; Wang, Tiejun; Xu, Ying; Zhang, Qi; Ma, Longlong

    2014-01-01

    Graphical abstract: MCM-41-modified Ni/HZSM-5 catalyst was developed by impregnation method with high catalytic performance for sorbitol hydrogenation in water. Appropriate amount of MCM-41 addition can distinctly promote the improvement in the surface structure and modulation of acidic sites of the catalyst. The scission of C–O bond in the sorbitol molecule into liquid alkanes was easily carried out on the catalyst containing more Lewis acidic sites. - Highlights: • Ni/HZSM-5 promoted with MCM-41 is active for sorbitol hydrogenation to liquid alkanes. • Lewis acidic sites of Ni/HZSM-5 can be modulated by pure silica MCM-41. • MCM-41 added can distinctly decrease carbon deposition on the catalyst surface. - Abstract: Liquid fuels derived from renewable biomass are of great importance on the potential substitution for diminishing fossil fuels. The conversion of sorbitol (a product of biomass-derived glucose hydrogenation) into liquid alkanes such as pentane and hexane over the Ni/HZSM-5 catalysts with or without MCM-41 addition was investigated in the presence of hydrogen in water medium. The production distribution of sorbitol hydrogenation can be controlled by adjusting the acidity of the catalyst. The scission of C–C bond in the sorbitol molecule into light C 1 –C 4 alkanes was mainly carried out over Ni/HZSM-5 containing strong Brønsted acid sites, while C–O bond scission into heavier alkanes was dominated over the catalysts added by MCM-41 containing weak Lewis acid sites. The sorbitol conversion and total liquid alkanes selectivity were found to be 67.1% and 98.7% over 2%Ni/HZSM-5 modified by 40 wt% of MCM-41, whereas the corresponding value was 40% and 35.6% over 2%Ni/HZSM-5 in the absence of MCM-41. The effect of MCM-41 on the structure, acidity, and reducibility of Ni/HZSM-5 was investigated by using XRD, Py-IR, IR, and H 2 -TPR. Meanwhile, the resistance of carbon deposition over the catalyst modified by MCM-41 was studied by using TG

  13. Carbon Paste Electrode Modified with Carbamoylphosphonic Acid Functionalized Mesoporous Silica: A New Mercury-Free Sensor for Uranium Detection

    International Nuclear Information System (INIS)

    Yantasee, Wassana; Lin, Yuehe; Fryxell, Glen E.; Wang, Zheming

    2004-01-01

    This study reports a new approach for developing a uranium (U(VI)) electrochemical sensor that is mercury-free, solid-state, and has less chance for ligand depletion than existing sensors. A carbon-paste electrode modified with carbamoylphosphonic acid self-assembled monolayer on mesoporous silica was developed for uranium detection based on an adsorptive square-wave stripping voltammetry technique. Voltammetric responses for U(VI) detection are reported as a function of pH, preconcentration time, and aqueous phase U(VI) concentration. The uranium detection limit is 25 ppb after 5 minutes preconcentration and improved to 1 ppb after 20 minutes preconcentration. The relative standard deviations are normally less than 5%

  14. Organically Modified Silica with Pyrazole-3-carbaldehyde as a New Sorbent for Solid-Liquid Extraction of Heavy Metals

    Directory of Open Access Journals (Sweden)

    Smaail Radi

    2013-12-01

    Full Text Available A new chelating matrix, SiNP, has been prepared by immobilizing 1.5-dimethyl-1H-pyrazole-3-carbaldehyde on silica gel modified with 3-aminopropyl-trimethoxysilane. This new chelating material was well characterized by elemental analysis, FT-IR spectroscopy, cross polarization magic angle spinning solid state 13C-NMR, nitrogen adsorption-desorption isotherm, BET surface area, BJH pore size, and scanning electron microscopy (SEM. The new product exhibits good chemical and thermal stability as determined by thermogravimetry curves (TGA. The new prepared material was used as an adsorbent for the solid-phase extraction (SPE of Pb(II, Cd(II, Cu(II and Zn(II from aqueous solutions using a batch method, prior to their determination by flame atomic adsorption spectrometry. The adsorption capacity was investigated using kinetics and pH effects. Common coexisting ions did not interfere with separation and determination.

  15. Thermal stability and surface acidity of mesoporous silica doubly doped by incorporation of sulfate and zirconium ions

    Energy Technology Data Exchange (ETDEWEB)

    Salas, P. [Instituto Mexicano del Petroleo, Programa de Ingenieria Molecular, Eje Central Lazaro Cardenas No. 152, 07730 Mexico D.F. (Mexico)]. E-mail: psalas@imp.mx; Chen, L.F. [Departamento de Ingenieria Quimica, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico); Wang, J.A. [Laboratorio de Catalisis y Materiales, ESIQIE, Instituto Politecnico Nacional, Col. Zacatenco, 07738 Mexico D.F. (Mexico); Armendariz, H. [Instituto Mexicano del Petroleo, Programa de Ingenieria Molecular, Eje Central Lazaro Cardenas No. 152, 07730 Mexico D.F. (Mexico); Guzman, M.L. [Instituto Mexicano del Petroleo, Programa de Ingenieria Molecular, Eje Central Lazaro Cardenas No. 152, 07730 Mexico D.F. (Mexico); Montoya, J.A. [Instituto Mexicano del Petroleo, Programa de Ingenieria Molecular, Eje Central Lazaro Cardenas No. 152, 07730 Mexico D.F. (Mexico); Acosta, D.R. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, A. P. 20-364, 01000 Mexico D.F. (Mexico)

    2005-11-15

    A sulfated Si-Zr-MCM-41 solid with highly ordered mesostructure was synthesized through a templated synthesis route where the CTAB surfactant was used as template. During the synthesis procedure, various amounts of (NH{sub 4}){sub 2}SO{sub 4} were added into the mixed solution of Zr and Si precursors to in situ sulfate the MCM-41 solids, aiming to enhance the acidity and thermal stability. The resultant materials showed a long-range ordered hexagonal arrangement with high surface area larger than 797 m{sup 2}/g and an average pore size distributed at approximate 2.5-2.8 nm. The high-resolution TEM observations confirmed that the order of the mesostructure gained when the molar ratio of SO{sub 4} {sup 2-}/(ZrO{sub 2} + SiO{sub 2}) increased from 0.1 to 0.3 but decreased as it reached 0.5, which is consistent with the results of {sup 29}Si MAS-NMR and XRD analysis. Compared to Si-MCM-41, the (Q{sup 2} + Q{sup 3})/Q{sup 4} ratio derived from the NMR spectra of the Zr-doped sample was higher, indicating that zirconium atoms were incorporated into the silica framework. Unexpectedly, in situ sulfation does not enhance the surface Broensted acidity, most likely due to the sulfur retained within the bulk of the materials; however, it indeed improved the thermal stability of the solid and long-range order of the structure.

  16. Uptake and fate of surface modified silica nanoparticles in head and neck squamous cell carcinoma

    Directory of Open Access Journals (Sweden)

    Besic Gyenge Emina

    2011-08-01

    Full Text Available Abstract Background Head and neck squamous cell carcinoma (HNSCC is currently the eighth leading cause of cancer death worldwide. The often severe side effects, functional impairments and unfavorable cosmetic outcome of conventional therapies for HNSCC have prompted the quest for novel treatment strategies, including the evaluation of nanotechnology to improve e.g. drug delivery and cancer imaging. Although silica nanoparticles hold great promise for biomedical applications, they have not yet been investigated in the context of HNSCC. In the present in-vitro study we thus analyzed the cytotoxicity, uptake and intracellular fate of 200-300 nm core-shell silica nanoparticles encapsulating fluorescent dye tris(bipyridineruthenium(II dichloride with hydroxyl-, aminopropyl- or PEGylated surface modifications (Ru@SiO2-OH, Ru@SiO2-NH2, Ru@SiO2-PEG in the human HNSCC cell line UMB-SCC 745. Results We found that at concentrations of 0.125 mg/ml, none of the nanoparticles used had a statistically significant effect on proliferation rates of UMB-SCC 745. Confocal and transmission electron microscopy showed an intracellular appearance of Ru@SiO2-OH and Ru@SiO2-NH2 within 30 min. They were internalized both as single nanoparticles (presumably via clathrin-coated pits or in clusters and always localized to cytoplasmic membrane-bounded vesicles. Immunocytochemical co-localization studies indicated that only a fraction of these nanoparticles were transferred to early endosomes, while the majority accumulated in large organelles. Ru@SiO2-OH and Ru@SiO2-NH2 nanoparticles had never been observed to traffic to the lysosomal compartment and were rather propagated at cell division. Intracellular persistence of Ru@SiO2-OH and Ru@SiO2-NH2 was thus traceable over 5 cell passages, but did not result in apparent changes in cell morphology and vitality. In contrast to Ru@SiO2-OH and Ru@SiO2-NH2 uptake of Ru@SiO2-PEG was minimal even after 24 h. Conclusions Our study is the

  17. Anhydrous proton exchange membrane of sulfonated poly(ether ether ketone) enabled by polydopamine-modified silica nanoparticles

    International Nuclear Information System (INIS)

    Wang, Jingtao; Bai, Huijuan; Zhang, Haoqin; Zhao, Liping; Chen, Huiling; Li, Yifan

    2015-01-01

    Highlights: • The concept of acid/base pairs was employed to design anhydrous PEMs. • Polydopamine-modified silica particles were uniformly dispersed in SPEEK membrane. • The membranes displayed enhancement in both stability and anhydrous proton conductivity. - Abstract: Novel anhydrous proton exchange membrane is (PEM) facilely prepared by embedding dopamine-modified silica nanoparticles (DSiOis 2 ) into sulfonated poly (ether ether ketone) (SPEEK) polymer matrix. DSiO 2 bearing -NH 2 /-NH- groups are synthesized inspired by the bioadhesion principle, which are uniformly dispersed within SPEEK membrane due to the good interfacial compatibility. The interfacial electrostatic attractions render unique rearrangement of the nanophase-separated structure and the chain packing of the resultant hybrid membranes. As a result, the thermal and mechanical stabilities as well as structural stability of the hybrid membranes are enhanced when compared to SPEEK control membrane. On the other hand, induced by the attractions, acid–base pairs are formed at the SPEEK/DSiOarewere 2 interface, where fast proton transfer via Grotthuss mechanism is expected. These features confer much higher proton conductivities on the DSiO 2 -filled membranes under both hydrated and anhydrous conditions, compared to those of the SPEEK control membrane and SiO 2 -filled membranes. Particularly, the hybrid membrane with 15 wt% DSiO 2 achieve the highest conductivities of 4.52achieveachieved × 10 −3 S cm −1 at 120 °C under anhydrous condition, which is much higher than the SPEEK control membrane and the commercial Nafion membrane (0.1iswas × 10 −3 S cm −1 ). The membrane with 9 wt% DSiO 2 show an open cell potential of 0.98showshowed V and an optimum power density of 111.7 mW cm −2 , indicative of its potential application in fuel cell under anhydrous condition

  18. Determination of beryllium in water using silica gel chemically modified with aminophosphonic acid

    International Nuclear Information System (INIS)

    Zajtseva, G.N.; Strelko, V.V.

    2001-01-01

    Considered are methods of Be determination based on Be isolation from the solutions using aminophosphonic acid covalently bound on silica gel surface (APA-SiO 2 ) and subsequent photometric or atomic-absorption determination of Be in eluate ( the limit of Be determination is 0.00005 mg/l or 0.00008 mg/l, respectively). APA-SiO 2 high efficiency and a possibility of beryllium ions extraction from diluted solutions by means of sorbent small weighed portions is shown. High efficiency of the sorbent both for concentration and waters purification from beryllium is shown. Methods are tested in analysis of waste water. To assess the accuracy of the proposed methods, parallel determination of beryllium in tests by means of the additions method was carried out. The given data testify to a sufficient accuracy and reproducibility of the proposed methods [ru

  19. Development of TRPN dendrimer-modified disordered mesoporous silica for CO{sub 2} capture

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiaoyun; Zhang, Sisi; Qin, Hongyan; Wu, Wei, E-mail: wuweiupc@upc.edu.cn

    2014-08-15

    Highlights: • A novel series of TRPN dendrimers are synthesized. • Structurally disordered mesoporous silica was used to develop the CO{sub 2} adsorbent. • The CO{sub 2} adsorption capacity is relatively high. • The sorbent exhibits a high stability after 12 cycling runs. • The sorbent achieves complete desorption at low temperature (60 °C). - Abstract: A novel series of tri(3-aminopropyl) amine (TRPN) dendrimers were synthesized and impregnated on structurally disordered mesoporous silica (DMS) to generate CO{sub 2} adsorbents (TS). The physicochemical and adsorption properties of the adsorbents before and after dendrimer modification were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and N{sub 2} adsorption–desorption (N{sub 2}-BET) techniques. CO{sub 2} adsorption–desorption tests indicated that the sorbent demonstrates high CO{sub 2} adsorption capacity (138.1 mg g{sup −1} for G1 sample TS-G1-3CN-50 and 91.7 mg g{sup −1} for G2 sample TS-G2-6CN-50), and can completely desorb CO{sub 2} under vacuum at 60 °C. Its CO{sub 2} adsorption capacity at 25 °C increases with the amine loading, achieving the highest adsorption capacity (140.6 mg g{sup −1} for TS-G1-3CN) at 60%. The developed TS materials exhibited excellent cycling stability. After 12 consecutive adsorption–desorption runs, TS-G1-3CN-50 shows an adsorption capacity of 136.0 mg g{sup −1}, retaining 98.5% of its original value.

  20. Extraction of Silica from Cassava Periderm using Modified Sol-Gel ...

    African Journals Online (AJOL)

    Akorede

    6School of Chemical and Metallurgical Engineering, Faculty of Engineering and the Built ... glycol as capping agent in modified sol-gel method for ..... Effect of Organic Acid Treatment on the Properties of ... Journal of Analytical and Applied.

  1. Nanoparticles affect PCR primarily via surface interactions with PCR components: using amino-modified silica-coated magnetic nanoparticles as a main model

    Science.gov (United States)

    Nanomaterials have been widely reported to affect the polymerase chain reaction (PCR). However, many studies in which these effects were observed were not comprehensive, and many of the proposed mechanisms have been primarily speculative. In this work, we used amino-modified silica-coated magnetic n...

  2. l-Cysteine-modified silver-functionalized silica-based material as an efficient solid-phase extraction adsorbent for the determination of bisphenol A.

    Science.gov (United States)

    Li, Yuanyuan; Zhu, Nan; Li, Bingxiang; Chen, Tong; Ma, Yulong; Li, Qiang

    2018-02-01

    A new silver-functionalized silica-based material with a core-shell structure based on silver nanoparticle-coated silica spheres was synthesized, and silver nanoparticles were modified using strongly bound l-cysteine. l-Cysteine-silver@silica was characterized by scanning electron microscopy and FTIR spectroscopy. Then, a solid-phase extraction method based on l-cysteine-silver@silica was developed and successfully used for bisphenol A determination prior to HPLC analysis. The results showed that the l-cysteine-silver@silica as an adsorbent exhibited good enrichment capability for bisphenol A, and the maximum adsorption saturation was 20.93 mg/g. Moreover, a short adsorption equilibrium time was obtained due to the presence of silver nanoparticles on the surface of the silica. The extraction efficiencies were then optimized by varying the eluents and pH. Under the optimized conditions, good linearity for bisphenol A was obtained in the range from 0.4 to 4.0 μM (R 2  > 0.99) with a low limit of detection (1.15 ng/mL). The spiked recoveries from tap water and milk samples were satisfactory (85-102%) with relative standard deviations below 5.2% (n = 3), which indicated that the method was suitable for the analysis of bisphenol A in complex samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Selective removal mercury (Ⅱ) from aqueous solution using silica aerogel modified with 4-amino-5-methyl-1,2,4-triazole-3(4H)-thion

    Energy Technology Data Exchange (ETDEWEB)

    Tadayon, Fariba; Saber-Tehrani, Mohammad; Motahar, Shiva [Islamic Azad University, Tehran (Iran, Islamic Republic of)

    2013-03-15

    Silica aerogel surface modifications with chelating agents for adsorption/removal of metal ions have been reported in recent years. This investigation reported the preparation of silica aerogel (SA) adsorbent coupled with metal chelating ligands of 4-amino-5-methyl-1,2,4-triazole-3(4H)-thion (AMTT) and its application for selective adsorption of Hg(Ⅱ) ion. The adsorbent was characterized by Fourier transform infrared spectra (FTIR) and thermo gravimetric analysis (TGA) measurements, nitrogen physisorption and scanning electron microscope (SEM). Optimal experimental conditions including pH, temperature, adsorbent dosage and contact time have been established. Langmuir and Freundlich isotherm models were applied to analyze the experimental data. The best interpretation for the experimental data given by the Langmuir isotherm equation and the maximum adsorption capacity of the modified silica gel and silica aerogel was 142.85 and 17.24mgg⌃(-1), respectively. Thermodynamic parameters such as Gibbs free energy (ΔG{sup o}), standard enthalpy (ΔH{sup o}) and entropy change (ΔS{sup o}) were investigated. The adsorbed Hg(Ⅱ) on the SA-AMTT adsorbents could be completely eluted by 1.0M KBr solution and recycled at least four times without the loss of adsorption capacity. The results of the present investigation illustrate that modified silica aerogel with AMTT could be used as an adsorbent for the effective removal of Hg(Ⅱ) ions from aqueous solution.

  4. Use of rice husk ash as only source of silica in the formation of mesoporous materials Emprego da cinza da casca de arroz como única fonte de sílica na formação de materiais mesoporosos

    Directory of Open Access Journals (Sweden)

    A. J. Schwanke

    2013-03-01

    Full Text Available This paper reports the synthesis of molecular sieves similar to MCM-41 using rice husk ash as only source of silica. For comparison purposes, a standard synthesis was performed using aerosil 200 commercial silica. The rice husk silica was obtained by heating treatment at 600 ºC and leaching for 2 h in reflux with HCl 1mol.L-1 and used in the synthesis. The samples prepared were characterized by N2 adsorption, X-ray diffraction (XRD, scanning electronic microscopy (SEM and thermogravimetric analysis (TG. By type-IV adsorption isotherms, the formation of mesoporous materials was observed. XRD showed the formation of hexagonal unidirectional pore materials similar to MCM-41. By SEM, it could be observed that the rice husk has fibrous aspect and that synthesis using calcined and leached rice husk did not react entirely because silica was only partially dissolved.Este trabalho relata o estudo da síntese de peneiras moleculares semelhantes à MCM-41, empregando cinza da casca de arroz como única fonte de sílica. Para critérios de comparação uma síntese foi realizada com sílica comercial aerosil 200. A sílica da casca de arroz foi obtida mediante tratamento térmico a 600 ºC e lixiviação em refluxo por 2 h com HCl 1 mol/L e empregada na síntese. As amostras preparadas foram caracterizadas por adsorção de N2, difração de raios X, microscopia eletrônica de varredura (MEV e termogravimetria. Por meio das isotermas de adsorção, do tipo IV, observa-se a formação de material mesoporoso. Nos difratogramas de raios X é identificada a formação hexagonal unidirecional de poros, indicando que material apresenta semelhanças com a MCM-41. Por MEV observa-se que a casca de arroz possui aspecto fibroso e que a síntese empregando a casca de arroz calcinada e lixiviada não reagiu na sua totalidade devido a dissolução parcial da sílica.

  5. Sorption and Preconcentration of Lead on Silica Nanoparticles Modified with Resacetophenone

    Directory of Open Access Journals (Sweden)

    Anupreet Kaur

    2009-01-01

    Full Text Available The silica-resacetophenone (SiO2-RATP nanoparticles were used as a new sorbent for extraction of trace amounts of Pb(II by batch technique. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer SiO2-RATP was found to be 167.24 µ mol/g at optimum pH and the detection limit (3σ was 0.58 µg/L. The adsorption equilibrium of Pb(II on nanometer SiO2-RATP was achieved in 20 min. Adsorbed Pb(II was easily eluted with 5 mL of 0.5 M hydrochloric acid. The maximum preconcentration factor was 60. The method was applied for the determination of trace amounts of Pb(II in various natural water rivers.

  6. Solid phase extraction of uranium and thorium on octadecyl bonded silica modified with Cyanex 302 from aqueous solutions

    International Nuclear Information System (INIS)

    Nilchi, A.; Shariati Dehaghan, T.; Rasouli Garmarodi, S.

    2013-01-01

    A simple and reliable method for rapid extraction and determination of uranium and thorium using octadecyl-bonded silica modified with Cyanex 302 is presented. Extraction efficiency and the influence of various parameters such as aqueous phase pH, flow rate of sample solution and amount of extractant has been investigated. The study showed that the extraction of uranium and thorium increase with increasing pH value and was found to be quantitative at pH 6; and the retention of ions was not affected significantly by the flow rate of sample solution. The extraction percent were found to be 89.55 and 86.27 % for uranium and thorium, respectively. The maximal capacity of the cartridges modified by 30 mg of Cyanex 302 was found to be 20 mg of uranium and thorium. The method was successfully applied to the extraction and determination of uranium and thorium in aqueous solutions. The percentage recovery of uranium and thorium in a number of natural as well as seawater samples of Iran were also investigated and found to be in the range of 85-95%. (author)

  7. Comparison of bare and amino modified mesoporous silica@poly(ethyleneimine)s xerogel as indomethacin carrier: Superiority of amino modification.

    Science.gov (United States)

    Li, Jing; Xu, Lu; Wang, Hongyu; Yang, Baixue; Liu, Hongzhuo; Pan, Weisan; Li, Sanming

    2016-02-01

    The purpose of this study was to facilely develop amino modified mesoporous silica xerogel synthesized using biomimetic method (B-AMSX) and to investigate its potential ability to be a drug carrier for loading poorly water-soluble drug indomethacin (IMC). For comparison, mesoporous silica xerogel without amino modification (B-MSX) was also synthesized using the same method. The changes of characteristics before and after IMC loading were systemically studied using fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), small angle X-ray scattering (SAXS) and nitrogen adsorption/desorption analysis. The results showed that B-MSX and B-AMSX were spherical nanoparticles with mesoporous structure. Compared with B-MSX, IMC loading capacity of B-AMSX was higher because more drug molecules can be loaded through stronger hydrogen bonding force. DSC and SAXS analysis confirmed the amorphous state of IMC after being loaded into B-MSX and B-AMSX. The in vitro drug release study revealed that B-MSX and B-AMSX improved IMC release significantly, and B-AMSX released IMC a little faster than B-MSX because of larger pore diameter of IMC-AMSX. B-MSX and B-AMSX degraded gradually in dissolution medium evidenced by color reaction and absorbance value, and B-AMSX degraded slower than B-MSX due to amino modification. In conclusion, B-AMSX with superiority of higher loading capacity and enhanced dissolution release can be considered to be a good candidate as drug carrier for IMC. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Adsorption of H[Ru(III) Cl2(H2EDTA)] complex on modified silica gel surface with [3-(2-aminoethyl)aminopropyl] trimethoxysilane in ethanol solutions

    International Nuclear Information System (INIS)

    Lazarin, Angelica Machi; Sernaglia, Rosana Lazara

    1999-01-01

    Silica gel was functionalized with [3-(2-aminoethyl) aminopropyl] trimethoxysilane group (SF-AEATS) and the characterization by chemical analysis (N) and infrared spectroscopy confirmed the functionalization. The capacity of the modified silica to adsorb the complex Ru (III) EDTA from ethanolic solution was studied. The selectivity coefficients of the complex formed on the support obtained was τn), 2,07 x 10 4 L/mol and the average number of ligand bonded by one metal ion on the support (n) was ∼1. (author)

  9. Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

    2014-05-21

    In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

  10. 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.

  11. Synthesis and characterization of silica mesoporous material produced by hydrothermal continues pH adjusting path way

    Directory of Open Access Journals (Sweden)

    A. Salemi Golezani

    2016-08-01

    Full Text Available Mesoporous silica molecular sieves MCM-41 were synthesized under hydrothermal conditions. For this purpose, a solution with a molar coefficient of water, cetyltri-methyl ammonium bromide surfactants as template and sodium silicate as the source of SiO2 are used. Phase formation, morphology and gas absorption properties were investigated by XRD and BET analysis, respectively. The results showed that silica mesoporous material has been successfully synthesized. A favorable special surface and porosity volume together with regular arrangement of nano metric-hexagonal porosities were obtained from this synthesis. Thickness of the wall and average diameter of the pores are 0.8 nm and 4 nm, respectively.

  12. Application of mesoporous carbon and modified mesoporous carbon for treatment of DMF sewage

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Fang, E-mail: liufangfw@163.com; Gao, Ya; Zhang, Shuang; Yan, Xi; Fan, Fengtao; Zhao, Chaocheng; Sun, Juan [China University of Petroleum(East China), Department of Chemical Engineering (China)

    2016-02-15

    Mesoporous carbon (MC) was prepared in soft template, and potassium ferricyanide was added into MC to prepare the modified mesoporous carbon (MMC). TEM, SEM, FT-IR, and N{sub 2} adsorption–desorption were used to characterize the textural properties of mesoporous materials. The BET specific surface area, pore volume, and the pore size of MC and MMC were 607.6321 and 304.7475 m{sup 2}/g, 0.313552 and 0.603573 cm{sup 3}/g, and 5.4356 and 7.9227 nm, respectively. The adsorption capabilities of MC and MMC were compared with the silica mesoporous material MCM-41. The influences of different adsorption conditions were optimized. For MC, the optimums of adsorbent dose, DMF initial concentration, rotating speed, and pH were 0.002 mg/50 mL, 200 mg/L, 200 r/min, and 4, respectively. MMC showed the highest DMF adsorption capacity at adsorbent dose 0.002 g/50 mL, DMF initial concentration 1000 mg/L, rotating speed 1000 r/min, pH more than 9, and contact time of less than 20 min. Meanwhile for MC, MMC, Pseudo-second-order equation was used to fit adsorption kinetics data. And adsorption process could be well fitted by Langmuir and Freundlich adsorption isotherms of MC, MMC. The results showed that MMC was a perfect adsorbent for DMF, and it was easy to separation and recycle. The recycling property of MMC was still relatively better than other two adsorbents.

  13. Chemoselective Hydrogenation with Supported Organoplatinum(IV) Catalyst on Zn(II)-Modified Silica

    Energy Technology Data Exchange (ETDEWEB)

    Camacho-Bunquin, Jeffrey [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Ferrandon, Magali [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Sohn, Hyuntae [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Yang, Dali [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Liu, Cong [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Ignacio-de Leon, Patricia Anne [Energy Sciences Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Perras, Frédéric A. [Ames Laboratory, U.S. Department of Energy, Ames, Iowa 50010, United States; Pruski, Marek [Ames Laboratory, U.S. Department of Energy, Ames, Iowa 50010, United States; Department of Chemistry, Iowa State University, 2416 Pammel Drive, Ames, Iowa 50011, United States; Stair, Peter C. [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States; Department of Chemistry, Northwestern University, 2145 Sheridan Road, Evanston, Illinois 60208, United States; Delferro, Massimiliano [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S Cass Avenue, Lemont, Illinois 60439, United States

    2018-02-22

    Well-defined organoplatinum(IV) sites were grafted on a Zn(II)-modified SiO2 support via surface organometallic chemistry in toluene at room temperature. Solid-state spectroscopies including XAS, DRIFTS, DRUV-Vis, and solid-state (SS)NMR enhanced by dynamic nuclear polarization (DNP), as well as TPR-H2 and TEM techniques revealed highly dispersed (methylcyclopentadi-enyl)methylplatinum(IV) sites on the surface ((MeCp)PtMe/Zn/SiO2, 1). In addition, computational modelling suggests that the surface reaction of (MeCp)PtMe3 with Zn(II)-modified SiO2 support is thermodynamically favorable (ΔG = -12.4 kcal/mol), likely due to the increased acidity of the hydroxyl group, as confirmed by NH3-TPD and DNP-enhanced 17O{1H} SSNMR. In situ DRIFTS and XAS hydrogenation experiments reveal the formation of a surface Pt(IV)-H upon hydrogenolysis of Pt-Me groups. The heterogenized organoplatinum(IV)-H sites catalyze the selective partial hydrogenation of 1,3-butadiene to butenes (up to 95%) and the reduction of nitrobenzene derivatives to anilines (up to 100%) with excellent tolerance of reduction-sensitive func-tional groups (olefin, carbonyl, nitrile, halogens) under mild reaction conditions.

  14. Chemical design of pH-sensitive nanovalves on the outer surface of mesoporous silicas for controlled storage and release of aromatic amino acid

    International Nuclear Information System (INIS)

    Roik, N.V.; Belyakova, L.A.

    2014-01-01

    Mesoporous silicas with hexagonally arranged pore channels were synthesized in water–ethanol-ammonia solution using cetyltrimethylammonium bromide as template. Directed modification of silica surface with N-[N′-(N′-phenyl)-2-aminophenyl]-3-aminopropyl groups was realized by postsynthetic activation of halogenoalkylsilicas, which have surface uniformly or selectively distributed 3-chloropropyl groups, with 2-aminodiphenylamine in the liquid phase. Chemical composition of silica materials was estimated by IR spectroscopy and chemical analysis of the surface products of reactions. Characteristics of porous structure of MCM-41-type silicas were determined from X-ray and low-temperature nitrogen ad-desorption measurements. Release ability of synthesized silica carriers was established on encapsulation of 4-aminobenzoic acid in pore channels and subsequent delivery at pH=6.86 and pH=1.00. It was found that N-[N′-(N′-phenyl)-2-aminophenyl]-3-aminopropyl groups block pore entrances at neutral pH preventing 4-aminobenzoic acid release. At pH=1.00 repulsion of positively charged surface aromatic amino groups localized near pore orifices provides unhindered liberation of aromatic amino acid from mesoporous channels. - Graphical abstract: Blocking of pores with N-[N′-(N′-phenyl)-2-aminophenyl]-3-aminopropyl groups at pH=6.86 for storage of ABA and opening of pore entrances at pH=1.00 for unhindered ABA liberation. - Highlights: • Modification of MCM-41 with N-[N′-(N′-phenyl)-2-aminophenyl]-3-aminopropyl groups. • Study of release ability of synthesized silica carriers in relation to amino acid. • Controlled blocking and opening of pores by amino groups at pH change were performed. • Retention of amino acid at pH=6.86 and its liberation at pH=1.00 was proved

  15. Multifunctional PEG modified DOX loaded mesoporous silica nanoparticle@CuS nanohybrids as photo-thermal agent and thermal-triggered drug release vehicle for hepatocellular carcinoma treatment

    Science.gov (United States)

    Wu, Lingjie; Wu, Ming; Zeng, Yongyi; Zhang, Da; Zheng, Aixian; Liu, Xiaolong; Liu, Jingfeng

    2015-01-01

    The combination of a multi-therapeutic mode with a controlled fashion is a key improvement in nanomedicine. Here, we synthesized polyethylene glycol (PEG)-modified doxorubicin (DOX)-loaded mesoporous silica nanoparticle (MSN) @CuS nanohybrids as efficient drug delivery carriers, combined with photothermal therapy and chemotherapy to enhance the therapeutic efficacy on hepatocellular carcinoma (HCC). The physical properties of the nanohybrids were characterized by transmission electron microscopy (TEM), N2 adsorption and desorption experiments and by the Vis-NIR absorption spectra. The results showed that the doxorubicin could be stored in the inner pores of mesoporous silica nanoparticles; the CuS nanoparticles, which are coated on the surface of a mesoporous silica nanoparticle, could serve as efficient photothermal therapy (PTT) agents; the loaded drug release could be easily triggered by NIR irradiation. The combination of the PTT treatment with controlled chemotherapy could further enhance the cancer ablation ability compared to any of the single approaches alone. Hence, the reported PEG-modified DOX-loaded mesoporous silica nanoparticle@CuS nanohybrids might be very promising therapeutic agents for HCC treatment.

  16. Pepsin immobilized in dextran-modified fused-silica capillaries for on-line protein digestion and peptide mapping.

    Science.gov (United States)

    Stigter, E C A; de Jong, G J; van Bennekom, W P

    2008-07-07

    On-line digestion of proteins under acidic conditions was studied using micro-reactors consisting of dextran-modified fused-silica capillaries with covalently immobilized pepsin. The proteins used in this study differed in molecular weight, isoelectric point and sample composition. The injected protein samples were completely digested in 3 min and the digest was analyzed with micro-high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS). The different proteins present in the samples could be identified with a Mascot database search on the basis of auto-MS/MS data. It proved also to be possible to digest and analyze protein mixtures with a sequence coverage of 55% and 97% for the haemoglobin beta- and alpha-chain, respectively, and 35-55% for the various casein variants. Protease auto-digestion, sample carry-over and loss of signal due to adsorption of the injected proteins were not observed. The backpressure of the reactor is low which makes coupling to systems such as Surface Plasmon Resonance biosensors, which do not tolerate too high pressure, possible. The reactor was stable for at least 40 days when used continuously.

  17. Characteristics of Polysilicon Wire Glucose Sensors with a Surface Modified by Silica Nanoparticles/γ-APTES Nanocomposite

    Directory of Open Access Journals (Sweden)

    Jheng-Jia Jhuang

    2011-03-01

    Full Text Available This report investigates the sensing characteristics of polysilicon wire (PSW glucose biosensors, including thickness characteristics and line-width effects on detection limits, linear range and interference immunity with membranes coated by micropipette/spin-coating and focus-ion-beam (FIB processed capillary atomic-force-microscopy (C-AFM tip scan/coating methods. The PSW surface was modified with a mixture of 3-aminopropyl-triethoxysilane (γ-APTES and polydimethylsiloxane (PDMS-treated hydrophobic fumed silica nanoparticles (NPs. We found that the thickness of the γ-APTES+NPs nonocomposite could be controlled well at about 22 nm with small relative standard deviation (RSD with repeated C-AFM tip scan/coatings. The detection limit increased and linear range decreased with the line width of the PSW through the tip-coating process. Interestingly, the interference immunity ability improves as the line width increases. For a 500 nm-wide PSW, the percentage changes of the channel current density changes (ΔJ caused by acetaminophen (AP can be kept below 3.5% at an ultra-high AP-to-glucose concentration ratio of 600:1. Simulation results showed that the line width dependence of interference immunity was strongly correlated with the channel electrical field of the PSW biosensor.

  18. Natural silica sand modified by calcium oxide as a new adsorbent for uranyl ions removal from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Elhefnawy, O.A.; Elabd, A.A. [Nuclear and Radiological Regulatory Authority (NRRA), Cairo (Egypt). Nuclear Safeguards and Physical Protection Dept.

    2017-07-01

    Calcium oxide modified El-Zafarana silica sand (CMZS) was prepared as a new adsorbent for U(VI) removal from aqueous solutions in a series of batch experiments. The new adsorbent CMZS was characterized by different analysis techniques SEM, EDX, XRD, and FTIR. The influence of many parameters on the removal process like; effect of pH, contact time, U(VI) initial concentration and temperature on U(VI) removal were investigated. Kinetic experiments showed that U(VI) removal on CMZS followed pseudo-second-order kinetics model appropriately and the equilibrium data agreed well with the Langmuir isotherm model. Kinetics and isothermal data reveal the chemisorption process of U(VI) on CMZS. The thermodynamic parameters (ΔH {sup circle}, ΔS {sup circle}, ΔG {sup circle}) were evaluated from temperature dependent adsorption data and the U(VI) removal on CMZS was found to be endothermic and spontaneous in nature. U(VI) desorption from CMZS was studied by a simple acid treatment. The results indicate that CMZS is an effective adsorbent for U(VI) from aqueous solutions.

  19. Pepsin immobilized in dextran-modified fused-silica capillaries for on-line protein digestion and peptide mapping

    Energy Technology Data Exchange (ETDEWEB)

    Stigter, E.C.A. [Division of Biomedical Analysis, Department of Pharmaceutical Sciences, Faculty of Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands)], E-mail: e.c.a.stigter@uu.nl; Jong, G.J. de; Bennekom, W.P. van [Division of Biomedical Analysis, Department of Pharmaceutical Sciences, Faculty of Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands)

    2008-07-07

    On-line digestion of proteins under acidic conditions was studied using micro-reactors consisting of dextran-modified fused-silica capillaries with covalently immobilized pepsin. The proteins used in this study differed in molecular weight, isoelectric point and sample composition. The injected protein samples were completely digested in 3 min and the digest was analyzed with micro-high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS). The different proteins present in the samples could be identified with a Mascot database search on the basis of auto-MS/MS data. It proved also to be possible to digest and analyze protein mixtures with a sequence coverage of 55% and 97% for the haemoglobin {beta}- and {alpha}-chain, respectively, and 35-55% for the various casein variants. Protease auto-digestion, sample carry-over and loss of signal due to adsorption of the injected proteins were not observed. The backpressure of the reactor is low which makes coupling to systems such as Surface Plasmon Resonance biosensors, which do not tolerate too high pressure, possible. The reactor was stable for at least 40 days when used continuously.

  20. Highly sensitive sorption-luminescence determination of trace europium with preconcentration on silica chemically modified with iminodiacetic acid

    International Nuclear Information System (INIS)

    Voronina, R.D.; Zorov, N.B.

    2007-01-01

    Features of a sorption-luminescence method for the determination of trace europium were studied. The method includes the preliminary sorption of europium at pH 7.1 from solutions with silica chemically modified with iminodiacetic acid, the subsequent treatment of the sorbent with 2-thenoyltrifluoroacetone at pH 8.0, and the measurement of the intensity of luminescence of the surface three-component europium complex at 613 nm. The effect of moisture as the quencher of luminescence of the surface europium complex was studied, and techniques for its removal were proposed. Sorption in the static mode provides the detection limit of europium of 7 x 10 -5 g/ml. The calibration plot is linear in the range of two orders of magnitude of europium concentration in solutions. The relative standard deviation in the determination of 1.5 x 10 -2 μg/ml europium is 5%. In the dynamic mode of sorption from 1000 ml of an analyzed solution with the use of sorption-desorption, the detection limit of europium of 8 x 10 -7 μg/ml was attained [ru

  1. Adsorption of Pb(II) using silica gel composite from rice husk ash modified 3-aminopropyltriethoxysilane (APTES)-activated carbon from coconut shell

    Science.gov (United States)

    Yusmaniar, Purwanto, Agung; Putri, Elfriyana Awalita; Rosyidah, Dzakiyyatur

    2017-03-01

    Silica gel modified by 3-aminopropyltriethoxysilane (APTES) was synthesized from rice husk ash combined with activated carbon from coconut shell yielded the composite adsorbent. The composite was characterized by Fourier Transform Infra Red spectroscopy (FT-IR), Electron Dispersive X-Ray (EDX), Surface Area Analyzer (SAA) and adsorption test by Atomic Absorption Spectrometry (AAS). This composite adsorbent has been used moderately for the removal of lead ions from metal solutions and compared with silica gel modified APTES and activated carbon. The adsorption experiments of Pb -ions by adsorbents were performed at different pH and contact time with the same metal solutions concentration, volume solution, and adsorbent dosage. The optimum pH for the adsorption was found to be 5.0 and the equilibrium was achieved for Pb with 20 min of contact time. Pb ions adsorption by composite silica gel modified APTES-activated carbon followed by Langmuir isotherm model with qmax value of 46.9483 mg/g that proved an adsorbent mechanism consistent to the mechanism of monolayer formation.

  2. A rhenium complex doped in a silica molecular sieve for molecular oxygen sensing: Construction and characterization.

    Science.gov (United States)

    Yang, Xiaozhou; Li, Yanxiao

    2016-01-15

    This paper reported a diamine ligand and its Re(I) complex for potential application in oxygen sensing. The novelty of this diamine ligand localized at its increased conjugation chain which had a typical electron-withdrawing group of 1,3,4-oxadiazole. Electronic distribution of excited electrons and their lifetime were supposed to be increased, favoring oxygen sensing collision. This hypothesis was confirmed by single crystal analysis, theoretical calculation and photophysical measurement. It was found that this Re(I) complex had a long-lived emission peaking at 545 nm, favoring sensing application. By doping this complex into a silica matrix MCM-41, oxygen sensing performance and mechanism of the resulting composites were discussed in detail. Non-linear Stern-Volmer working curves were observed with maximum sensitivity of 5.54 and short response time of ~6 s. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. 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

  4. Different Effects of the Immunomodulatory Drug GMDP Immobilized onto Aminopropyl Modified and Unmodified Mesoporous Silica Nanoparticles upon Peritoneal Macrophages of Women with Endometriosis

    Directory of Open Access Journals (Sweden)

    Yuliya Antsiferova

    2013-01-01

    Full Text Available The aim of the present work was to compare in vitro the possibility of application of unmodified silica nanoparticles (UMNPs and modified by aminopropyl groups silica nanoparticles (AMNPs for topical delivery of immunomodulatory drug GMDP to the peritoneal macrophages of women with endometriosis. The absence of cytotoxic effect and high cellular uptake was demonstrated for both types of silica nanoparticles. The immobilization of GMDP on the UMNPs led to the suppression of the stimulatory effect of GMDP on the membrane expression of scavenger receptors SR-AI and SR-B, mRNAs expression of NOD2 and RAGE, and synthesis of proteolytic enzyme MMP-9 and its inhibitor TIMP-1. GMDP, immobilized onto AMNPs, enhanced the initially reduced membrane expression of SRs and increased NOD2, RAGE, and MMP-9 mRNAs expression by macrophages. Simultaneously high level of mRNAs expression of factors, preventing undesirable hyperactivation of peritoneal macrophages (SOCS1 and TIMP-1, was observed in macrophages incubated in the presence of GMDP, immobilized onto AMNPs. The effect of AMNPs immobilized GMDP in some cases exceeded the effect of free GMDP. Thus, among the studied types of silica nanoparticles, AMNPs are the most suitable nanoparticles for topical delivery of GMDP to the peritoneal macrophages.

  5. Different effects of the immunomodulatory drug GMDP immobilized onto aminopropyl modified and unmodified mesoporous silica nanoparticles upon peritoneal macrophages of women with endometriosis.

    Science.gov (United States)

    Antsiferova, Yuliya; Sotnikova, Nataliya; Parfenyuk, Elena

    2013-01-01

    The aim of the present work was to compare in vitro the possibility of application of unmodified silica nanoparticles (UMNPs) and modified by aminopropyl groups silica nanoparticles (AMNPs) for topical delivery of immunomodulatory drug GMDP to the peritoneal macrophages of women with endometriosis. The absence of cytotoxic effect and high cellular uptake was demonstrated for both types of silica nanoparticles. The immobilization of GMDP on the UMNPs led to the suppression of the stimulatory effect of GMDP on the membrane expression of scavenger receptors SR-AI and SR-B, mRNAs expression of NOD2 and RAGE, and synthesis of proteolytic enzyme MMP-9 and its inhibitor TIMP-1. GMDP, immobilized onto AMNPs, enhanced the initially reduced membrane expression of SRs and increased NOD2, RAGE, and MMP-9 mRNAs expression by macrophages. Simultaneously high level of mRNAs expression of factors, preventing undesirable hyperactivation of peritoneal macrophages (SOCS1 and TIMP-1), was observed in macrophages incubated in the presence of GMDP, immobilized onto AMNPs. The effect of AMNPs immobilized GMDP in some cases exceeded the effect of free GMDP. Thus, among the studied types of silica nanoparticles, AMNPs are the most suitable nanoparticles for topical delivery of GMDP to the peritoneal macrophages.

  6. 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.

  7. Formation of monodisperse mesoporous silica microparticles via spray-drying.

    Science.gov (United States)

    Waldron, Kathryn; Wu, Winston Duo; Wu, Zhangxiong; Liu, Wenjie; Selomulya, Cordelia; Zhao, Dongyuan; Chen, Xiao Dong

    2014-03-15

    In this work, a protocol to synthesize monodisperse mesoporous silica microparticles via a unique microfluidic jet spray-drying route is reported for the first time. The microparticles demonstrated highly ordered hexagonal mesostructures with surface areas ranging from ~900 up to 1500 m(2)/g and pore volumes from ~0.6 to 0.8 cm(3)/g. The particle size could be easily controlled from ~50 to 100 μm from the same diameter nozzle via changing the initial solute content, or changing the drying temperature. The ratio of the surfactant (CTAB) and silica (TEOS), and the amount of water in the precursor were found to affect the degree of ordering of mesopores by promoting either the self-assembly of the surfactant-silica micelles or the condensation of the silica as two competing processes in evaporation induced self-assembly. The drying rate and the curvature of particles also affected the self-assembly of the mesostructure. The particle mesostructure is not influenced by the inlet drying temperature in the range of 92-160 °C, with even a relatively low temperature of 92 °C producing highly ordered mesoporous microparticles. The spray-drying derived mesoporous silica microparticles, while of larger sizes and more rapidly synthesized, showed a comparable performance with the conventional mesoporous silica MCM-41 in controlled release of a dye, Rhodamine B, indicating that these spray dried microparticles could be used for the immobilisation and controlled release of small molecules. Copyright © 2013 Elsevier Inc. All rights reserved.

  8. Mesoporous silica nanoparticles for biomedical and catalytical applications

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Xiaoxing [Iowa State Univ., Ames, IA (United States)

    2011-01-01

    Mesoporous silica materials, discovered in 1992 by the Mobile Oil Corporation, have received considerable attention in the chemical industry due to their superior textual properties such as high surface area, large pore volume, tunable pore diameter, and narrow pore size distribution. Among those materials, MCM-41, referred to Mobile Composition of Matter NO. 41, contains honeycomb liked porous structure that is the most common mesoporous molecular sieve studied. Applications of MCM-41 type mesoporous silica material in biomedical field as well as catalytical field have been developed and discussed in this thesis. The unique features of mesoporous silica nanoparticles were utilized for the design of delivery system for multiple biomolecules as described in chapter 2. We loaded luciferin into the hexagonal channels of MSN and capped the pore ends with gold nanoparticles to prevent premature release. Luciferase was adsorbed onto the outer surface of the MSN. Both the MSN and the gold nanoparticles were protected by poly-ethylene glycol to minimize nonspecific interaction of luciferase and keep it from denaturating. Controlled release of luciferin was triggered within the cells and the enzymatic reaction was detected by a luminometer. Further developments by varying enzyme/substrate pairs may provide opportunities to control cell behavior and manipulate intracellular reactions. MSN was also served as a noble metal catalyst support due to its large surface area and its stability with active metals. We prepared MSN with pore diameter of 10 nm (LP10-MSN) which can facilitate mass transfer. And we successfully synthesized an organo sil