共查询到20条相似文献,搜索用时 109 毫秒
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XRD粉末衍射法研究全微波合成的MCM-41介孔分子筛 总被引:23,自引:0,他引:23
MCM41是Mobil公司九十年代开发的具有规整孔道的介孔分子筛,其潜在的应用前景已引起人们广泛关注[1,2]。目前,MCM41介孔分子筛的合成多为水热法[3]。该法操作较为繁琐,耗能费时,整个合成过程最快也需5~7天。1988年ChuP.[4]以专利形式报道了微波技术在分子筛合成中的应用,但对合成的具体细节未作任何描述。宋天佑[5]、Cundy[6]等人在晶化阶段采用微波辐射法分别合成了NaX和MCM41介孔分子筛,但其有机模板剂的脱除(简称“脱模”)过程仍采用传统的高温焙烧法。作者首次采用全微波辐射… 相似文献
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新型MCM-41-β-沸石中孔-微孔复合分子筛 总被引:27,自引:0,他引:27
MCM-41是1992年由Mobil公司首次合成,具有可调的规整孔道结构,孔径大小为1.6~10nm的六方中孔分子筛[1,2],β-沸石是具有三维十二元环孔道,一条线性通道孔径为0.57nm×0.75nm,另一条由两种线性通道相交形成的弯曲通道,孔径... 相似文献
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以十六烷基三甲基省化铵(CTAB)作模板剂,研究了水热体系中孔MCM-41分子筛的合成条件。在H2O/Si介于12-100,Si/Al介于10-∞,CTAB/Si介于0.08-0.2时,可以合成出MCM-41分子筛,在国入煤油等混合烃的合成体系中,可以合成出孔径大于4nmdisplay structure 相似文献
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在凝胶体系NaX(F、Cl、Br)Na2OAl2O3SiO2CTAB(十六烷基三甲基溴化铵)H2O中,研究了水热合成中孔MCM41的合成条件。实验证明,在398K下晶化8~16d,NaX/SiO2介于0.01~0.05时,均可合成出MCM41分子筛;NaF的加入,可以加快MCM41分子筛的晶化速度;NaBr的加入,对形成MCM41分子筛有阻碍作用。采用XRD、SEM、TGDTA和N2吸附对合成样品加以表征,证明合成样品具有介孔分子筛特性。 相似文献
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MCM-41分子筛的合成及129Xe核磁共振的研究 总被引:5,自引:0,他引:5
Purely siliceous MCM-41 with a narrow pore-size distribution, different pore size, high surface area was synthesized . As prepared, calcined and catalytically tested MCM-41 materials have been comprehensively characterized by N2 adsorption/desorption at 77K and 129Xe NMR. By adding mesitylene during the synthesis, the pore size of MCM-41 was enlarged to 5.2nm. The chemical shift in 129Xe NMR spectroscopy of adsorbed xenon indicates that the MCM-41 is one dimensional pore channels . 相似文献
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Romanenko KV Py X d'Espinose de Lacaillerie JB Lapina OB Fraissard J 《The journal of physical chemistry. B》2006,110(7):3055-3060
(129)Xe NMR has been used to study a series of homologous activated carbons obtained from a KOH-activated pitch-based carbon molecular sieve modified by air oxidation/pyrolysis cycles. A clear correlation between the pore size of microporous carbons and the (129)Xe NMR of adsorbed xenon is proposed for the first time. The virial coefficient delta(Xe)(-)(Xe) arising from binary xenon collisions varied linearly with the micropore size and appeared to be a better probe of the microporosity than the chemical shift extrapolated to zero pressure. This correlation was explained by the fact that the xenon collision frequency increases with increasing micropore size. The chemical shift has been shown to vary very little with temperature (less than 9 ppm) for xenon trapped inside narrow and wide micropores. This is indicative of a smooth xenon-surface interaction potential. 相似文献
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K. V. Romanenko O. B. Lapina X. Py J. Fraissard 《Russian Journal of General Chemistry》2008,78(11):2171-2181
Despite the extensive use of 129Xe NMR for characterization of high surface-to-volume porous solids, particularly zeolites, this method has not been widely used to explore the properties of microporous carbon materials. In this study, commercial amorphous carbons of different origin (produced from different precursors) and a series of activated carbons obtained by successive cyclic air oxidation/pyrolysis treatments of a single precursor were examined. Models of 129Xe chemical shift as a function of local Xe density, mean pore size, and temperature are discussed. The virial coefficient arising from binary xenon collisions, σXe-Xe, varied linearly with the mean pore size given by N2 adsorption analysis; σXe-Xe appeared to be a better probe of the mean pore size than the chemical shift extrapolated to zero pressure, σS. 相似文献
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Cr/MCM-41催化剂的结构特征及其纳米尺寸孔内聚乙烯的形成 总被引:5,自引:0,他引:5
合成了纯硅MCM-41,并以浸渍法在表面负载烯烃聚合催化活性中心---过渡金属元素Cr;通过对所得Cr/MCM-41样品的结构特征及Cr物种的存在形成进行XRD,低温N2吸附,FTIR,Raman,^2^9SiNMR等表征发现,Cr/MCM-41具有良好的长程有序结构、较高的比表面积及均一的孔径分布。负载于MCM-41表面的Cr物种通过与羟基的相互作用分散于载体孔道内。Cr负载量较低时,Cr物种主要以孤立态存在,随着Cr含量增加,出现聚合态的Cr物种。Cr/MCM-41的一维孔道内,不仅可进行乙烯的聚合形成聚乙烯,而且反应后MCM-41的长程结构保持不变。 相似文献
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Xenon porometry is a method in which porous material is immersed in a medium and the properties of the material are studied by means of 129Xe nuclear magnetic resonance (NMR) of xenon gas dissolved in the medium. For instance, the chemical shift of a particular signal (referred to as signal D) arising from xenon inside small pockets formed in the pores during the freezing of the confined medium is highly sensitive to the pore size. In the present study, we show that when naphthalene is used as the medium the pore size distribution of the material can be determined by measuring a single one-dimensional spectrum near room temperature and converting the chemical shift scale of signal D to the pore radius scale by using an experimentally determined correlation. A model has been developed that explains the curious behavior of the chemical shift of signal D as a function of pore radius. The other signals of the spectra measured at different temperatures have also been identified, and the influence of xenon pressure on the spectra has been studied. For comparison, 129Xe NMR spectra of pure xenon gas adsorbed to porous materials have been measured and analyzed. 相似文献
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Benjamin D. Egleston Konstantin V. Luzyanin Michael C. Brand Rob Clowes Michael E. Briggs Rebecca L. Greenaway Andrew I. Cooper 《Angewandte Chemie (International ed. in English)》2020,59(19):7362-7366
Control of pore window size is the standard approach for tuning gas selectivity in porous solids. Here, we present the first example where this is translated into a molecular porous liquid formed from organic cage molecules. Reduction of the cage window size by chemical synthesis switches the selectivity from Xe‐selective to CH4‐selective, which is understood using 129Xe, 1H, and pulsed‐field gradient NMR spectroscopy. 相似文献
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Michele Mauri Matteo Farina Giorgio Patriarca Roberto Simonutti K. Thomas Klasson 《International Journal of Polymer Analysis and Characterization》2015,20(2):119-129
Pecan shell-based biochar is utilized as a filtration medium, sequestrant for metallic ions, soil conditioner, and other applications. One process for creating the biochar involves the use of phosphoric acid at high temperature in a partial oxygen atmosphere to produce a highly porous carbonaceous material. In this work, we found 129Xe NMR to be an excellent technique to study micropores in biochar. Thus, the 129Xe chemical shift in biochar was found to vary linearly with the xenon pressure; from the data an estimate of about 8–9 Å could be proposed for the average pore diameter in pecan shell-based biochar. Through saturation recovery and 2-D NMR exchange experiments, information on the exchange between free versus bound xenon was obtained. Furthermore, correlations of 129Xe NMR data with the carbonization process conditions were made. 相似文献
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Moudrakovski IL Wang LQ Baumann T Satcher JH Exarhos GJ Ratcliffe CI Ripmeester JA 《Journal of the American Chemical Society》2004,126(16):5052-5053
Hyperpolarized (HP) 129Xe NMR was used for the first time to probe the geometry and interconnectivity of pores in RF aerogels and to correlate them with the [resorcinol]/[catalyst] (R/C) ratio. We have demonstrated that HP 129Xe NMR is an ideal method for accurately measuring the volume-to-surface-area (Vg/S) ratios for soft mesoporous materials without using any geometric models. The Vg/S parameter, which is related both to the geometry and the interconnectivity of the porous space, has been found to correlate strongly with the R/C ratio and exhibits an unusually large span: an increase in the R/C ratio from 50 to 500 results in about 5-fold rise in Vg/S. Unlike conventional techniques, HP 129Xe NMR spectroscopy probes the geometry and interconnectivity of the nano- or mesopores in soft materials, providing new insights into the pore structure. 相似文献
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Huang SJ Huh S Lo PS Liu SH Lin VS Liu SB 《Physical chemistry chemical physics : PCCP》2005,7(16):3080-3087
An extensive study has been made on a series of multifunctional mesoporous silica materials, prepared by introducing two different organoalkoxysilanes, namely 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane (AEPTMS) and 3-cyanopropyltriethoxysilane (CPTES) during the base-catalyzed condensation of tetraethoxysilane (TEOS), using the variable-temperature (VT) hyperpolarized (HP) 129Xe NMR technique. VT HP-129Xe NMR chemical shift measurements of adsorbed xenon revealed that surface properties as well as functionality of these AEP/CP-functionalized microparticles (MP) could be controlled by varying the AEPTMS/CPTES ratio in the starting solution during synthesis. Additional chemical shift contribution due to Xe-moiety interactions was observed for monofunctional AEP-MP and CP-MP as well as for bifunctional AEP/CP-MP samples. In particular, unlike CP-MP that has a shorter organic backbone on the silica surface, the amino groups in the AEP chain tends to interact with the silanol groups on the silica surface causing backbone bending and hence formation of secondary pores in AEP-MP, as indicated by additional shoulder peak at lower field in the room-temperature 129Xe NMR spectrum. The exchange processes of xenon in different adsorption regions were also verified by 2D EXSY HP-129Xe NMR spectroscopy. It is also found that subsequent removal of functional moieties by calcination treatment tends to result in a more severe surface roughness on the pore walls in bifunctional samples compared to monofunctional ones. The effect of hydrophobicity/hydrophilicity of the organoalkoxysilanes on the formation, pore structure and surface property of these functionalized mesoporous silica materials are also discussed. 相似文献