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1.
TS-1分子筛的合成Ⅰ.29Si和1H NMR研究正硅酸乙酯的水解 总被引:2,自引:0,他引:2
利用29Si和1H NMR方法研究了TS-1分子筛合成过程中正硅酸乙酯(TEOS)的水解行为.1H NMR结果表明,TEOS在四丙基氢氧化铵(TPAOH)溶液中的水解速度快于在四乙基氢氧化铵(TEAOH)中的水解速度.TEOS水解后的29Si NMR谱显示,TEOS在TPAOH中水解产生的聚合硅酸根物种的分布与在TEAOH中的类似,都存在着单体、二聚、三聚及环聚等硅酸根物种的平衡,但TEOS-TEAOH体系中低聚硅酸根物种的浓度明显大于TEOS-TPAOH中的浓度.向水解后的样品中添加水,可促使多聚硅酸根物种转化为低聚物种.大量异丙醇的加入将导致单聚和二聚硅酸根物种的高聚.钛酸四丁酯加入到TEOS-TPAOH水解体系中得到的29Si NMR结果明显不同于TEOS-TEAOH水解体系. 相似文献
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The fluorescence and fluorescence-excitation spectra of fluorescein molecules during the sol-gel-xerogel transitions of tetraethyl orthosilicate (TEOS) solutions have been observed as functions of doped concentration, in the order of 10-2 and 10-5 mol dm-3, and of the sol-gel-xerogel transition time. It was shown that with a lower initial concentration only the cation was encapsulated in the pores of the silica xerogel state during the sol-gel reaction processes. On the other hand, with a high concentration four species, i.e., cation, monoanion, dianion, and dimer, were encapsulated in the silica xerogel during the sol-gel reaction processes. These results have the potential to open the way to the development of simultaneous multiple-band solid-state laser emitting materials. 相似文献
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A series of polymer-silica hybrid materials consisting of amino-terminated anionic waterborne-polyurethane (WPU) and inorganic silica particles have been prepared through a sol-gel process in the absence of an external catalyst. Typically, amino-terminated anionic WPU was first synthesized from polycaprolactone, dimethylol propionic acid, and 4,4′-methylenebis(cyclohexyl isocyanate) with specific molar ratios, followed by further reaction with triethylamine and triethylene tetramine to give as-prepared WPU. The WPU obtained was characterized by FTIR spectroscopy and gel permeation chromatography. Subsequently, a series of hybrid materials with different silica contents were prepared by performing sol-gel reactions with tetraethyl orthosilicate (TEOS) in an amino-terminated WPU matrix without the addition of an external catalyst. This was followed by examination by transmission electron microscopy and 29Si solid-state NMR. The terminated primary amine groups attached to the as-prepared WPU chains functioned as an internal base catalyst for the sol-gel process of TEOS. The effect of composition on the thermal stability, mechanical strength, surface wettability, and optical clarity of the hybrid materials was evaluated by the thermogravimetric analysis, dynamic mechanical analysis, contact angle measurement, and UV-visible transmission spectroscopy, respectively. 相似文献
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A novel method for synthesis of silica nanoparticles 总被引:7,自引:0,他引:7
Rao KS El-Hami K Kodaki T Matsushige K Makino K 《Journal of colloid and interface science》2005,289(1):125-131
A sequential method has been used, for the first time, to prepare monodisperse and uniform-size silica nanoparticles using ultrasonication by sol-gel process. The silica particles were obtained by hydrolysis of tetraethyl orthosilicate (TEOS) in ethanol medium and a detailed study was carried out on the effect of different reagents on particle sizes. Various-sized particles in the range 20-460 nm were synthesized. The reagents ammonia (2.8-28 mol L(-1)), ethanol (1-8 mol L(-1)), water (3-14 mol L(-1)), and TEOS (0.012-0.12 mol L(-1)) were used and particle size was examined under scanning electron microscopy and transmission electron microscopy. In addition to the above observations, the effect of temperature on particle size was studied. The results obtained in the present study are in agreement with the results observed for the electronic absorption behavior of silica particles, which was measured by UV-vis spectrophotometry. 相似文献
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Hybrid silica-PVA nanofibers via sol-gel electrospinning 总被引:1,自引:0,他引:1
Pirzada T Arvidson SA Saquing CD Shah SS Khan SA 《Langmuir : the ACS journal of surfaces and colloids》2012,28(13):5834-5844
We report on the synthesis of poly(vinyl alcohol) (PVA)-silica hybrid nanofibers via sol-gel electrospinning. Silica is synthesized through acid catalysis of a silica precursor (tetraethyl orthosilicate (TEOS) in ethanol-water), and fibers are obtained by electrospinning a mixture of the silica precursor solution and aqueous PVA. A systematic investigation on how the amount of TEOS, the silica-PVA ratio, the aging time of the silica precursor mixture, and the solution rheology influence the fiber morphology is undertaken and reveals a composition window in which defect-free hybrid nanofibers with diameters as small as 150 nm are obtained. When soaked overnight in water, the hybrid fibers remain intact, essentially maintaining their morphology, even though PVA is soluble in water. We believe that mixing of the silica precursor and PVA in solution initiates the participation of the silica precursor in cross-linking of PVA so that its -OH group becomes unavailable for hydrogen bonding with water. FTIR analysis of the hybrids confirms the disappearance of the -OH peak typically shown by PVA, while formation of a bond between PVA and silica is indicated by the Si-O-C peak in the spectra of all the hybrids. The ability to form cross-linked nanofibers of PVA using thermally stable and relatively inert silica could broaden the scope of use of these materials in various technologies. 相似文献
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Kazunori Matsui Takayuki Kaneko Yasunori Yaginuma Masaru Ryu 《Journal of Sol-Gel Science and Technology》1997,9(3):273-277
A spin probe TEMPOL (4-hydroxy-2,2,6,6-tetramethylpiperidinyl-1-oxy) was dissolved in a tetraethyl orthosilicate sol-gel reaction
system and measured by electron spin resonance spectroscopy at 295 K. The nitrogen hyperfine coupling constant was from 1.64–1.66
mT in the sol-gel solutions. The values were sensitive to the ethanol-to-water ratio of the solutions. The hyperfine coupling
constant in the xerogels was 1.70 mT, which was almost the same as that in water, indicating that the probe molecules were
trapped in silica pores with water adsorbed on the silica surfaces. The motion of TEMPOL in the xerogels was considerably
slower than in the sol-gel solutions. The local viscosity estimated was from 70–90 cP. The ESR spectra of TEMPOL were altered
during the sol-gel process, indicating that adsorbed water on the silicas surfaces has an important role for trapping organic
molecules in sol-gel glasses. 相似文献
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A organically modified molecularly imprinted silica (MIS), selective for methylxanthines, was prepared using a simple sol-gel procedure. Caffeine was used as template; 3-aminopropyltrimethoxysilane (APTMS) as functional monomer and tetraethyl orthosilicate (TEOS) as reticulating agent. The material was packed on solid-phase extraction (SPE) cartridges and evaluated with aqueous test samples, natural water and human urine; a quantitative method for methylxanthines in water, using SPE cartridges packed with the MIS coupled with HPLC-UV was developed. The MIS was highly specific for methylxanthines, with an imprinting factor of (20.5+/-1.9). The analytical method resulted in detection limits of 85 microgL(-1) for theobromine, 44 microgL(-1) for theophylline and 53 microgL(-1) for caffeine. 相似文献
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Two layered silica protective film made by a spray-and-dip coating method on 304 stainless steel 总被引:1,自引:0,他引:1
Taejin Hwang HeungYeol Lee Hohyeong Kim GyunTak Kim 《Journal of Sol-Gel Science and Technology》2010,55(2):207-212
The silica coating has attracted much attention because of its superior corrosion resistance with almost no harm to human
health and to the environment. In this study, a two layered silica film was tried to get an enhanced corrosion resistance.
The silica film was prepared on the hairline finish 304 stainless steel surfaces by-a-spray- and subsequent-dip-coating process.
The spray coating solution was prepared by mixing sodium silicate solution, silica colloid, tetraethyl orthosilicate (TEOS),
methyltriethoxysilane (MTES), ethanol, and distilled water. Then the solution was sprayed onto the stainless steel surface,
and was dried and heat treated. The dip coating solution was prepared by a simple mixing of TEOS and acidic water into ethanol,
and the prior spray coated sample was dipped into the solution. The outer dip coated layer was intended to cover spray coated
rough and porous layer and hence to enhance the corrosion resistance. A homogeneous and crack free surface was successfully
obtained after the dip coating. The prepared silica film was characterized using scanning electron microscopy, potentiodynamic
polarization scan, and electrochemical impedance spectroscopy. The two layered film showed an enhanced corrosion resistance.
The enhancement was attributed to a protecting effect of the dip coated layer where the diffusion of ionic species was successfully
impeded. 相似文献
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GUO Bin GAO Jian-gang CHEN Da-zhu LIU Jian-ping HE Ping-sheng ZHANG Qi-jin 《高等学校化学研究》2005,21(5):606-610
The sol-gel transition process of PMMA/SiO2 hybrid materials was first studied by means of the dynamic torsional vibration method. The different stages of the transition can be described by the change of torque. The temperature-dependent measurement of the gel time( tg ) gives the possibility to determine the apparent activation energy.( Ea ) of this transition according to Flory's gelation theory. The non-equilibrium thermodynamic fluctuation theory was used to predict the transition behavior. The isothermal transition experiments on hybrid sols with different TEOS(tetraethyl orthosilicate) contents were carried out. The results show that the Ea of a hybrid sol is higher than that of a non- hybrid sol of a TEOS-water-ethanol system. The increasing of TEOS content in a hybrid sol has no obvious effect on the Ea value, but it can enhance the sol-gel .reaction rate. 相似文献
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Qi Zhao Yingcong Wei Chuangjiang Ni Yumei Zhang Baijun Liu Zhaoyan Sun Haiming Xie Wei Hu Liang Liang 《Journal of polymer science. Part A, Polymer chemistry》2019,57(21):2190-2200
Study on proton exchange membrane (PEM) with the aim toward excellent battery performance of PEM for fuel cells has attracted increasing attention. In this work, nanocellulose (CNC) aminated by KH792 noted as NN was prepared. CNC or NN/sulfophenylated poly(ether ether ketone ketone) (sPEEKK) nanocomposite membrane (SN) or (SNN) were produced by solution mixing. SNN was further coated with tetraethyl orthosilicate (TEOS) to obtain SNNT. The properties of sPEEKK, SN, SNN, and SNNT membranes were thoroughly investigated. The proton conductivity of SN4 was 0.22 S·cm?1 at 90 °C, while a proton conductivity of 0.30 S·cm?1 was obtained for SNN4, and an even higher value of 0.36 S·cm?1 at 90 °C was obtained for the TEOS‐coated SNN4 (SNN4T). Meanwhile, SNN4T showed high thermal stability, and its Td5 was as high as 318.2 °C. Furthermore, the composite membrane coated with TEOS also presented excellent oxidative stability. The mass of SNN2T after treated in Fenton agent for 1 h at 80 °C was still retained 96.2%, and it was not fully dissolved until 11 h. It was illustrated that aminated CNC/sPEEKK nanocomposite membranes coated with TEOS is a kind of promising materials as PEMs for fuel cells. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 2190–2200 相似文献
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含氟高分子/SiO_2杂化疏水材料的制备及涂层表面性质 总被引:1,自引:0,他引:1
采用自由基溶液聚合与溶胶-凝胶法相结合的方法制备了含氟高分子/SiO2杂化疏水材料.通过甲基丙烯酸十二氟庚酯(FA)与乙烯基三乙氧基硅烷(VTES)共聚合成了含氟硅共聚物(PFAS),进一步通过原硅酸乙酯(TEOS)与PFAS共聚物溶液共水解缩聚制备了具有含氟侧基的碳碳主链高分子和硅氧网络的含氟高分子/SiO2杂化疏水材料.研究结果表明,SiO2组分含量提高可以显著增加杂化材料薄膜的涂敷厚度,改善其耐久性能,而对杂化材料疏水性能的影响不大. 相似文献
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采用蔗糖为碳源, 正硅酸乙酯(TEOS)为硅源, 分别以草酸、硝酸铁、硝酸镍为催化剂, 用溶胶-凝胶法制备碳化硅前驱体, 考察了制备过程中催化剂的种类以及反应温度和时间对凝胶形成的影响. 发现以硝酸铁为催化剂最有利于凝胶的形成, 碳/硅物质的量比为4的前驱体在氩气气氛1350 ℃下加热10 h, 碳热还原反应趋于完成. 以该条件下合成的多孔碳化硅(比表面积133 m2·g-1)作为催化剂载体, 通过等量浸渍法获得Pt/SiC催化剂, 将其应用于一氧化碳氧化的模型反应中. 研究结果表明该催化剂有较好的催化活性和稳定性. 引入镍助剂的PtNi/SiC催化剂能进一步提高一氧化碳催化氧化反应的活性. 相似文献
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In situ small-angle X-ray scattering (SAXS) is used to investigate the influence of alcohol identity and content on silicalite-1 growth from clear solutions at 368 K. Several tetraalkyl orthosilicates (Si(OR)4, R = Me, Pr, and Bu) are used to synthesize silicalite-1 from clear solution mixtures comparable to those previously investigated (i.e. 1:0.36:20 TEOS:TPAOH:H2O (TEOS = tetraethyl orthosilicate; TPAOH = tetrapropylammonium hydroxide), 368 K). All TPAOH-organosiloxane mixtures studied form silica nanoparticles after aging at room temperature for 24 h. Full-profile fitting analysis of the SAXS data indicates the particles are ellipsoidal and is inconsistent with the presence of "nanoslabs" or "nanoblocks". Synthesis using TEOS as the silica source have an induction period of approximately 7.5 h and a growth rate of 1.90 +/- 0.10 nm/h at 368 K. Changing the silica source to tetramethyl orthosilicate (TMOS) does not change the induction period; however the particle growth rate is decreased to 1.65 +/- 0.09 nm/h at 368 K. Variable-temperature SAXS measurements for syntheses with TEOS and TMOS show the activation energy for silicalite-1 growth is 60.0 +/- 2.9 and 73.9 +/- 2.8 kJ/mol, respectively, indicating the alcohol identity does influence the growth rate. By mixing tetrapropyl orthosilicate (TPOS) with TEOS (1.6:1.0 molar ratio) as the silica source, the precursor solution shows a shorter induction period (6.0 h) and a faster particle growth rate (2.16 +/- 0.06 nm/h). The alcohol identity effect is more pronounced when other organocations (e.g. alkyltripropylammonium cations) are used to make silicalite-1 at 368 K. Removing ethanol from the precursor solution decreases the induction period to approximately 4.5 h and increases the particle growth rate to 2.99 +/- 0.13 nm/h. Mixtures with 2 equiv of ethanol have an induction period and particle growth rate of 6.0 h and 2.04 +/- 0.03 nm/h, respectively. The results demonstrate the alcohol identity and content influence silicalite-1 growth kinetics. One possible explanation is varying the alcohol identity and content changes the strength of the hydrophobic hydration of the structure-directing agent and the water-alcohol interaction, resulting in less efficient interchange between clathrated water molecules and solvated silicate species. 相似文献
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Dongming Qi Chao Lin Hongting Zhao Hu Liu 《Journal of Dispersion Science and Technology》2017,38(1):70-74
In this study, monodispersed SiO2 nanoparticles with controllable size ranging from 20 to 100 nm have been successfully prepared by using a Stöber sol-gel process. The particle size, distribution, and morphology were examined by dynamic light scattering (DLS) and transmission electron microscopy (TEM). In order to accurately regulate the particle size, the effects of various reaction parameters on the particle size and morphology of SiO2 nanoparticles were systematically investigated. It was found that, to some extent, the SiO2 particle size increased linearly with the increase of ammonia or water content, as well as the decrease of reaction temperature, while nearly kept constant with the increase of tetraethyl orthosilicate (TEOS). Based upon the results, an empirical formula has been developed to model/predict the particle size of the SiO2 nanoparticles over a wide range of various reaction conditions. 相似文献
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LI Ying-xiu ZHU Lian-de ZHU Guo-yi State Key Lab of Electroanalytical Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun P.R. ChinaZHAO Chun College of Chemistry Jilin University Changchun P 《高等学校化学研究》2002,18(1):12-15
IntroductionIn recent years chemiluminescence (CL)biosensor prepared by immobilization of a sensitivereagent such as peroxidase or oxidase onto a solidmatrix has attracted much attention due to the highsensitivity of the chemiluminescent reaction of thesensitive reagent even with a simple instrument.Generally,CL biosensors can be divided into twocategories.One consists of hydrogen peroxide sen-sors prepared by immobilizing a kind of peroxidaseonto a suitable solid support[1,2 ] ,and the immo… 相似文献
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苯基修饰的疏水微孔二氧化硅膜的制备与表征 总被引:2,自引:0,他引:2
采用苯基三乙氧基硅烷(PTES)和正硅酸乙酯(TEOS)作为前驱体,通过溶胶-凝胶法制备了苯基修饰的SiO2膜材料。利用扫描电镜、N2吸附、视频光学接触角测量仪、热重分析、红外光谱等测试手段对膜的孔结构以及疏水性能进行了表征,最后还研究了修饰后膜材料在室温条件下的单组份气体渗透和分离性能。结果表明,随着PTES加入量的增大,膜材料的疏水性逐渐增强,当PTES/TEOS和H2O/TEOS的化学计量比分别达到0.6和9.6时,膜材料对水的接触角达到115±0.5°,仍保持良好的微孔结构,其孔体积为0.17cm3/g,孔径为0.4-0.5nm。室温下氢气在修饰后SiO2膜的输运既遵循发生在微孔孔道的表面扩散机理也遵循发生在较大孔道或者微缺陷的努森扩散机理,膜材料的H2渗透率达到1.49×10-6mol?m-2?Pa-1?s-1,H2/CO2 和H2/SF6的理想分离系数分别达到4.64和365.59 相似文献
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Elham Noori Mehdi Bazarganipour Masoud Salavati-Niasari Tahereh Gholami 《Journal of Cluster Science》2013,24(4):1171-1180
Silica nanostructures were synthesized on the basis of modified Stöber procedure via a sonochemical method and the reaction between tetraethyl orthosilicate (TEOS), ethylenediamine (en) and methanol in water, in the attendance of Schiff-base ligand (H2Salen) as capping agent. The effects of synthesis parameters such as: sonochemical irradiation time, sonochemical power and molar aspect ratio of Schiff-base ligand to TEOS were considered to achieve optimum situation. It was established that particle size, morphology and phase of the products could be affected by these parameters. The as synthesized silica nanostructures were characterized by X-ray powder diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, ultraviolet–visible spectroscopy, and X-ray energy dispersive spectroscopy. 相似文献