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21.
Berquier Jean-Marc Nael Pascal Jupille Jacques Jacquiod Catherine 《Journal of Sol-Gel Science and Technology》2000,19(1-3):83-87
Fourier Transform Infrared transmission spectroscopy is used to characterize surfactant-templated silica films on glass. The calcination process is followed in situ and evidence for the removal of the surfactant along the Hoffman reaction is given. Once calcined, the surface of the pores of the mesoporous films is proven by deuteration experiment to be hydroxylated. Bands are attributed to isolated and hydrogen-bonded silanols. Silylation reaction with hexamethyldisilazane only occurs with isolated silanol groups. 相似文献
22.
表面含磷酸的介孔分子筛P-SBA-15的合成及其性能评价 总被引:4,自引:1,他引:4
采用后合成法,将磷酸固载在纯硅介孔分子筛SBA-15表面上。利用X射线衍射(XRD)、红外光谱(IR)、氮气吸附 脱咐法(BET)分析方法表征催化剂的物理性能。结果表明,催化剂P-SBA-15在高温焙烧后保持了稳定的介孔分子筛SBA-15结构,该催化剂的比表面积和孔径分别为605.45m2/g和5.576nm(磷硅摩尔比5%)。选用十一碳烯酸与异丙醇的酯化反应对催化剂P-SBA-15的催化反应性能进行评价,同时与其他几种微孔沸石分子筛催化剂催化性能相比表明,磷酸改性的介孔分子筛P SBA 15是合成十一烯酸异丙酯较为理想的固体酸催化剂,考察了催化剂的稳定性。 相似文献
23.
采用阳离子表面活性剂十六烷基三甲基溴化铵为模板剂,以正硅酸乙酯为硅源,以硫酸铝为铝源,水热合成了以催化油浆窄馏分为添加剂的高比表面积Al-MCM-41介孔分子筛,并利用XRD,HREM,TG-DTA及N2吸附-脱附等测试手段对合成样品进行了表征.合成的Al-MCM-41分子筛的比表面积和孔体积分别达到1295m2/g和1.5cm3/g,其平均孔径为4.3nm.重点研究了Al-MCM-41分子筛结晶度、晶胞参数、比表面积、孔体积及平均孔径等结构性质随催化油浆窄馏分添加量及其组成的变化规律,并从合成机理上进行了解释. 相似文献
24.
Mechanism of hierarchical porosity development in MFI zeolites by desilication: the role of aluminium as a pore-directing agent 总被引:2,自引:0,他引:2
Groen JC Peffer LA Moulijn JA Pérez-Ramírez J 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(17):4983-4994
The role of the concentration and the nature of aluminium in the creation of hierarchical porosity in both commercial and synthesized MFI zeolites have been investigated through controlled mesoporosity development by desilication in alkaline medium. Framework aluminium controls the process of framework silicon extraction and makes desilication selective towards intracrystalline mesopore formation. An optimal molar Si/Al ratio in the range 25-50 has been identified; this leads to an optimal mesoporosity centred around 10 nm and mesopore surface areas of up to 235 m(2) g(-1) while preserving the intrinsic crystalline and acidic properties. At lower framework Si/Al ratios the relatively high Al content inhibits Si extraction and hardly any mesopores are created, while in highly siliceous ZSM-5 unselective extraction of framework Si induces formation of large pores. The existence of framework Al sites in different T positions that are more or less susceptible to the alkaline treatment, and the occurrence of re-alumination, are tentative explanations for the remarkable behaviour of Al in the desilication process. The presence of substantial extra framework Al, obtained by steam treatment, inhibits Si extraction and related mesopore formation; this is attributed to re-alumination of the extraframework Al species during the alkaline treatment. Removal of extraframework Al species by mild oxalic acid treatment restores susceptibility to desilication, which is accompanied by formation of larger mesopores due to the enhanced Si/Al ratio in the acid-treated zeolite. 相似文献
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26.
Gun'ko VM Villiéras F Leboda R Marciniak M Charmas B Skubiszewska-Zi&ecedil;ba J 《Journal of colloid and interface science》2000,230(2):320-327
Adsorbents synthesized by grafting of titania onto mesoporous silica gel surfaces at different temperatures were studied by means of nitrogen adsorption–desorption and water desorption. The pore size distribution f(Rp) of titania/silica gel depends on the titania concentration (CTiO2) and the temperature of titania synthesis. Nonuniformity of TiO2 phase is maximal at a low CTiO2 value (3.2 wt.% anatase deposited at 473 K), and two peaks of the fractal dimension distribution f(D) are observed at such a concentration of titania, but at larger CTiO2 values, only one f(D) peak is seen. More ordered filling of pores and adsorption sites by nitrogen, reflecting in the shape of adsorption energy distributions f(E) at different pressures of adsorbate, is observed for adsorbent with titania (rutile+anatase) grafted on silica gel at a higher temperature (673 K). 相似文献
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Two simple modification methods for ordered mesoporous silicas were examined and compared. MCM-41 molecular sieve was physically coated with 4-cyano-4-biphenyl [4(4-pentenyloxy)]benzoate (CBPB) and chemically modified using trimethylethoxysilane. The structural and surface properties of the obtained materials were characterized using elemental analysis, thermogravimetry and nitrogen adsorption over a wide pressure range.It was shown that the pore size of the MCM-41 material was not decreased significantly after the coating procedure, even for high loadings of CBPB. Moreover, low pressure adsorption measurements indicated that significant fractions of the MCM-41 surface were not covered by CBPB, even for high CBPB loadings, which suggests that the attained coverage may be very nonuniform. The chemical bonding procedure led to a marked decrease in the pore size and change of surface properties.It was demonstrated that nitrogen adsorption measurements provide a means of a thorough characterization of modified MCM-41 materials, allowing to estimate the surface area, pore volume and pore size distribution. Moreover, low pressure adsorption data can be used to qualitatively or semiquantitatively assess the surface coverage of the coated/bonded organic groups, which may be used to estimate the uniformity of the coverage and therefore, the usefulness of the modification procedure. 相似文献
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30.
介孔分子筛MSU-1的合成 总被引:1,自引:0,他引:1
MSU X介孔分子筛具有三维立体交叉排列的蠕虫状孔道结构,有利于客体分子在其孔道内扩散[1]。目前合成MSU X的原料[2 4]TEOS水解速度慢,合成过程较易控制,但价高、易燃、有刺激性。本文采用文献[5 7]法,以水玻璃、A(EO)9为原料,在酸性至近中性的范围里合成了MSU 1介孔分子筛,与TEOS为原料的MSU 1合成进行了比较,考察了pH值和不同类型表面活性剂(脂肪醇聚氧乙烯醚和烷基酚聚氧乙烯醚)对产物结构性质的影响。1 实验部分1 1 试剂和仪器水玻璃(SiO2%≈26、Na2O%≈8),工业级,青岛海洋化工厂生产;脂肪醇聚氧乙烯醚非离子表面活性… 相似文献