• Title/Summary/Keyword: silica-sol

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Effective Liquid-phase Nitration of Benzene Catalyzed by a Stable Solid Acid Catalyst: Silica Supported Cs2.5H0.5PMo12O40

  • Gong, Shu-Wen;Liu, Li-Jun;Zhang, Qian;Wang, Liang-Yin
    • Bulletin of the Korean Chemical Society
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    • v.33 no.4
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    • pp.1279-1284
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    • 2012
  • Silica supported $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ catalyst was prepared through sol-gel method with ethyl silicate-40 as silicon resource and characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, nitrogen adsorption-desorption and potentiometric titration methods. The $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ particles with Keggin-type structure well dispersed on the surface of silica, and the catalyst exhibited high surface area and acidity. The catalytic performance of the catalysts for benzene liquid-phase nitration was examined with 65% nitric acid as nitrating agent, and the effects of various parameters were tested, which including temperature, time and amount of catalyst, reactants ratio, especially the recycle of catalyst was emphasized. Benzene was effectively nitrated to mononitro-benzene with high conversion (95%) in optimized conditions. Most importantly, the supported catalyst was proved has excellent stability in the nitration progress, and there were no any other organic solvent and sulfuric acid were used in the reaction system, so the liquid-phase nitration of benzene that we developed was an eco-friendly and attractive alternative for the commercial technology.

Characterization of SPAES Composite Membrane Using Silane Based Inorganics (실란계 복합화 무기물을 이용한 SPAES 복합막의 특성평가)

  • Woo, Chang Hwa;Kim, Deuk Ju;Nam, Sang Yong
    • Membrane Journal
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    • v.25 no.5
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    • pp.456-463
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    • 2015
  • In this study, we synthesize novel silane based inorganics for preparation of the polymer electrolyte membrane with high proton conductivity under high temperature condition and developed membranes are characterized. SPAES, hydrocarbon based polymer are synthesized and used as main polymeric material. We used sol-gel method to prepare inorganic material with high performance using silica, phosphate and zirconium. Three types of inorganics were prepared by control of the mole ration of each component. As a result of EDX analysis, the inorganic materials are well dispersed in the polymer membrane. The water uptake of the composite membrane is increased by introduction of the hydrophilic inorganic material in the membrane. When the content of the zirconium in the membrane is increased, the proton conductivity of the composite membrane shows the higher value than pure SPAES membrane at the high temperature. And the silica based inorganics effect to increase the proton conductivity under low temperature condition.

Nanosulfated Silica as a Potential Heterogeneous Catalyst for the Synthesis of Nitrobenzene

  • Khairul Amri;Aan Sabilladin;Remi Ayu Pratika;Ari Sudarmanto;Hilda Ismail;Budhijanto;Mega Fia Lestari;Won-Chun Oh;Karna Wijaya
    • Korean Journal of Materials Research
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    • v.33 no.7
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    • pp.265-272
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    • 2023
  • In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H2SO4/SiO2 as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO2 was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 ℃. SiO2 with a 200-mesh size was impregnated with 98 % H2SO4 by mixing for 1 h. The resulting 33 % (w/w) H2SO4/SiO2 catalyst was separated by centrifugation, dried, and calcined at 600 ℃. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 ℃ for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H2SO4/SiO2 could generate an average benzene conversion of 40.33 %.

Improvement of Photo-stability for p-Aramid Fibers by SiO2/TiO2 Sol-Gel Method (SiO2/TiO2 sol-gel법을 이용한 p-아라미드 섬유의 내광성 증진)

  • Lee, Young-Il;Jung, Min-Hyuck;Lee, Mun-Cheul
    • Textile Coloration and Finishing
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    • v.25 no.3
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    • pp.172-180
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    • 2013
  • Aramid fibers are being used increasingly in a wide range of application due to low density, high specific strength, high modulus, and high thermal resistance. But owing to its special physical and chemical structures, it is sensitive to absorb the ultraviolet light which will degrade the fiber's useful mechanical properties and structure. In this paper, the sol-gel technique was used to improve the photo-stability of p-aramid fibers. $TiO_2$, modified $SiO_2$/$TiO_2$ sol were used as coating solutions. The influence of the such coatings on the photo-stability of p-aramid fiber was investigated by an accelerated photo-ageing method using xenon lamp. The photo-stability of p-aramid fiber showed obvious improvement after the modified silica binding coating. But the amorphous $TiO_2$ sol coatings showed a negative effect. After 144h light exposure, the modified silane binder-coated fibers showed less degradation in mechanical properties with the retained tensile strength greater than about 70% of the original value.

Study for Organic(Bio)-Inorganic Nano-Hybrid OMC

  • Lee, Jung-Eun;Ji, Hong-Geun;Park, Yoon-Chang;Lee, Kyoung-Chul;Yoo, Eun-Ah
    • Proceedings of the SCSK Conference
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    • 2003.09a
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    • pp.178-191
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    • 2003
  • OMC is essentialiy necessary compound in sun goods as organic UV protecting products. But the skin-trouble problem is raising because of skin penetration of OMC. In this study, non-capsulated pure OMC was compared with Organic-Inorganic-Nano-hybrid OMC for skin penetration force and SPF degree. Organic- Inorganic Nano-Hybrid OMC is OMC trapped in the pore of the mesoporous silica synthesized by the sol-gel method after OMC is nanoemulsified in the system of the hydrogenated Lecithin/ Ethanol/caprylic/capric triglyceride/OMC/water. OMC- nano- emulsion was obtained by a microfluidizing process at 1000bar and then micelle size in the nanoemulsion solution is 100-200nm range. Mesoporous silica nano-hybrid OMC was prepared by the process; surfactant was added in dissolved OMC-Nanoemulsion, then the rod Micelle was formed. OMC-nanoemulsion was capsulated in this rod Micelle and then silica precursor was added in the OMC-nanoemulsion solution. Through the hydrolysis reaction of the silica precursor, mesoporous silica concluding OMC-Nanocapsulation was obtained. The nano-hybrid surface of this OMC-Nanoemulsion-Inorganic system was treated with polyalkyl-silane compound. OMC-Mesoporous silica Nano-hybrids coated with polyalkyl-silane compound show the higher sun protecting factor (SPF Analyzer: INDEX 10-15) than pure OMC and could reduce a skin penetration of OMC. The physico-chemical properties of these nano-hybrids measured on the SPF index, partical size, strcture, specific surface area, pore size, morphology, UV absorption, rate of the OMC dissolution using SPF Analyzer, Laser light scattering system, XRD, BET, SEM, chroma Meter, HPLC, Image analyzer, microfluidizer, UV/VIS. spectrometer.

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Preparation and Characterization of Sulfonated Poly(phthalazinone ether sulfone ketone) (SPPESK)/Silica Hybrid Membranes for Direct Methanol Fuel Cell Applications

  • Kim, Dae-Sik;Shin, Kwang-Ho;Park, Ho-Bum;Lee, Young-Moo
    • Macromolecular Research
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    • v.12 no.4
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    • pp.413-421
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    • 2004
  • Sulfonated poly(phthalazinone ether sulfone ketone) (SPPESK) membranes and sol-gel derived SPPESK/silica hybrid membranes have been investigated as potential polymer electrolyte membranes for direct methanol fuel cell (DMFC) applications. In comparison with the SPPESK membrane, the SPPESK/silica membranes exhibited higher water content, improved proton conductivity, and lower methanol permeability. Notably, the silica embedded in the membrane acted as a material for reducing the fraction of free water and as a barrier for methanol transport through the membrane. From the results of proton conductivity and methanol permeability studies, we suggest that the fractions of bound and free water should be optimized to obtain desirable proton conductivities and methanol permeabilities. The highly sulfonated PPESK hybrid membrane (HSP-Si) displayed higher proton conductivity (3.42 ${\times}$ 10$^2$ S/cm) and lower methanol permeability (4.15 ${\times}$ 10$\^$7/ $\textrm{cm}^2$/s) than those of Nafion 117 (2.54 ${\times}$ 10$^2$ S/cm; 2.36 ${\times}$ 10$\^$6/ $\textrm{cm}^2$/s, respectively) at 30$^{\circ}C$. This characteristic of the SPPESK/silica membranes is desirable for future applications related to DMFCs.

Silica Coating on Polymethylmethacrylate by Sol-Gel Process (졸-겔공정에 의해 Polymethylmethacrylate위에 실리카 코팅)

  • 이상근;양천회
    • Journal of the Korean Society of Safety
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    • v.12 no.4
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    • pp.79-85
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    • 1997
  • In order to improve the surface characteristics of polymethylmethacrylate(PMMA), oxide thin film coatings were applied using the sol-gel dip-coating technique. The $Si(OC_2H_5)_4$, tetra-ethyl-ortho-silicate(TEOS) was used as a starting material for $SiO_2$ coating. The hardness of the alkoxy-derived oxide-coated PMMA was increased from 190 MPa for non-coated PMMA with increasing film thickness. By optimizing the heating conditions and the hydrolysis conditions, a maximum apparent hardness obtained In the present study was achieved 310 MPa using the withdrawal velocity of 5cm/min and heat treatment at $90^{\circ}C$ for 5 hours, which is about 1.6 times larger than that of uncoated PMMA.

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SiO2/ZnS:Cu/ZnS Triplex Layer Coatings for Phosphorescence Enhancement

  • Zhang, Wen-Tao;Lee, Hong-Ro
    • Journal of the Korean institute of surface engineering
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    • v.41 no.4
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    • pp.169-173
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    • 2008
  • The objective of this study is to coat the $SiO_2$ layer uniformly on the ZnS:Cu phosphors by using Sol-Gel method. From results of SEM micrographs observation, XRD and XPS analysis, it could be confirmed that $SiO_2$ layer was relatively well coated on ZnS:Cu particles. $Ag_2S$ was used as a decoding chemical to analyze the dense and uniform coating performance of $SiO_2$ layer on phosphor particles. It could be concluded that phosphors synthesized from our two step replacement method showed strong blue peak comparing to other method and rather weak green peak also. Obtained particle size of phosphors were about 20m diameter. Luminescence properties of the phosphors were examined by photoluminescence spectra at the excitation wavelength of 270 nm.

Thermally Induced Mesophase Development in Ethanesilica Films via Macromolecular Templating Approach

  • Cho, Whirang;Char, Kook-Heon;Kwon, Su-Yong
    • Macromolecular Research
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    • v.17 no.9
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    • pp.697-702
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    • 2009
  • Mesoporous ethanesilica thin film was prepared using PEO-PLGA-PEO triblock copolymers as structure-directing agents and (1,2-bis(triethoxysilyl) ethane BTESE; bridged organosilicates) as inorganic precursors via one-step sol-gel condensation of ethanesilica precursors. The mesostructure of ethanesilica films is critically dependent on the processing experimental parameters after the hydrolyzed silica sol mixture was spin-cast. This study examined the effects of the block copolymer template/organosilica precursor ratio in the casting solution and aging period before calcination of the mesostructure. It was further demonstrated that mesoscopic ordering of organosilicate thin films is induced by the rearrangement of block copolymer template/organosilica hybrid during thermal decomposition of the PEO-PLGA-PEO triblock copolymer. The mesoporous structure and morphology were characterized by SAXS, TEM and solid-state NMR measurement.