共查询到20条相似文献,搜索用时 187 毫秒
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采用等体积浸渍法制备了不同负载量的固体酸催化剂SO42-/SnO2/SBA-15,利用X射线粉末衍射、N2吸附-脱附和透射电镜等手段对样品进行了表征,并考察了催化剂对4-叔丁基环己酮与乙二醇缩合反应的催化性能.结果表明,SO42-/SnO2催化剂负载于SBA-15后其催化性能明显改善.研究了SO42-/20%SnO2/SBA-15催化剂上部分酮类化合物与乙二醇及1,2-丙二醇的缩合反应,并考察了反应时间和催化剂用量等因素对反应性能的影响.在适宜的温和条件下,一些环酮类底物如环己酮、4-甲基环己酮和4-叔丁基环己酮等均可反应得到相应的缩醛化产物,且催化剂至少可循环使用4次. 相似文献
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在无溶剂条件下, 芳香醛与 5,5-二甲基-1,3-环己二酮或1,3-环己二酮经氨基磺酸锂催化缩合反应合成了氧杂蒽. 结果表明, 当催化剂用量为3%(摩尔分数)时, 在120 ℃反应 40~70 min, 产率高达 90% 以上. 此外, 探讨了该反应的氨基磺酸锂催化机理. 该合成方法具有操作简单, 反应时间短、 产率高及对环境友好等优点, 是现有氧杂蒽化合物合成方法的一个重要补充. 相似文献
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《中国科学:化学》2020,(2)
内酯化合物在医药、高分子等领域都有重要的应用.其中ε-己内酯是生物可降解材料聚己内酯(poly(ε-caprolactone))的单体以及聚酯的改性剂,目前年产量近10万吨,未来前景广阔.本文主要介绍了本课题组在分子氧氧化法合成内酯化合物特别是ε-己内酯方面所做的工作,以及国内外关于内酯化合物合成的研究进展以及展望.本课题组在传统的Baeyer-Villiger氧化环酮化合物制备内酯产物的研究基础上加以改进,分别从环己酮、K/A油(环己酮和环己醇的混合物)、环己烷出发,以氧气为氧化剂,一步反应得到ε-己内酯,较传统Baeyer-Villiger氧化法更加简单、高效、绿色环保,具有潜在的工业发展前景. 相似文献
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苯基磺酸官能化中孔硅基材料的制备及催化性能研究 总被引:7,自引:0,他引:7
通过溶胶-凝胶法制得了苯基聚硅氧烷, 进一步磺化制备了苯基磺酸官能化的中孔硅基催化材料, 并通过BET, SEM和固体核磁技术对其进行了表征. BET结果表明, 该催化剂比表面积为722 m2/g, 平均孔径为9.06 nm, 孔容0.59 mL/g. 13C CPMAS NMR和29Si CPMAS NMR表征显示磺酸基键合于苯环间位, 苯基以共价方式进入无机-有机杂化硅基材料的内部结构. 该固体酸的活性中心磺酸基在表面呈均匀分布, 在芳族羧酸和取代酚的直接酯化反应中表现出优异的催化性能. 相似文献
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苯磺酸修饰的层柱磷酸锆的制备及催化应用 总被引:1,自引:0,他引:1
以共缩合方法制备了一系列苯磺酸修饰的层柱磷酸锆材料,利用N2吸附、Si核磁共振、红外光谱和热重分析等方法对其结构进行了表征. 将其应用于对苯二酚与叔丁醇烷基化反应中,结果发现催化剂合成时的投料比对其催化性能有较大的影响,催化剂ZrP-0.4-2-10%-PhSO3H的催化性能最佳,反应4 h对苯二酚的转化率为85.4%,2-叔丁基对苯二酚得率达到58.5%. 酸性表征结果显示,催化剂活性与其表面可接触酸性位的数目密切有关. 该催化剂还具有较好的重复利用性能,反应3次后产物得率仅下降10%. 催化剂失活是由于磺酸基团的脱落或活性位被积碳覆盖所引起. 相似文献
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利用化学浸渍法将蔗糖负载到 SBA-15 介孔材料孔道内部, 高温炭化形成的多聚苯环经发烟硫酸气相磺化处理后, 得到磺酸基团功能化的新型碳-硅介孔复合材料. 发烟硫酸气相磺化处理是该材料合成的关键步骤. X 射线衍射、扫描电镜和氮气吸附结果表明, 碳-硅介孔复合材料经磺酸化处理保持了高度有序的介孔结构. 热重、傅里叶变换的红外光谱及吡啶吸附红外光谱结果证明, 磺酸功能基团成功的嫁接于碳-硅介孔复合材料孔道的内表面, 反应活性中心为 Br?nsted 酸, 酸密度在 0.09~0.70 mmol/g 可以有效调变. 当碳负载量为 35% 时, 该复合材料在生物柴油的绿色合成中显示出最优的催化性能, 且可重复使用 3 次以上. 相似文献
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苯及苯磺酸基官能化的中孔分子筛的合成及催化应用 总被引:3,自引:0,他引:3
近年来 ,通过对介孔分子筛 (如 MCM,HMS,MSU-X)结构及组成的化学“裁剪”,制备具有特定结构和表面性质的催化材料成为该领域的研究热点之一 [1~ 5] .许多文献报道了 MCM-4 1的有机官能化中孔材料的制备技术 [5~ 8] ,并将其应用于有机合成反应 ,取得了较好的结果 [7,8] .其中 MSU-X介孔分子筛结构具有三维排列“Worm-like”孔道特征 ,有利于物料传输 ;相对于 MCM-4 1分子筛在合成方面具有以中性表面活性剂作模板剂且模板剂容易去除等诸多优点[9] .本文采用非离子表面活性剂 C11— 15H2 3— 31(CH2 CH2 O) 9H(AEO9)为模板剂 ,… 相似文献
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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
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Christian W. Klampfl Wolfgang Buchberger Guenter Rieder Guenther K. Bonn 《Journal of chromatography. A》1997,770(1-2):23-28
A highly cross-linked porous poly(styrene-divinylbenzene) resin was reacted with sulfuric acid to give strong cation-exchange resins with capacities from 0.2 to 1.9 mequiv./g. The retention behavior of mono- and dicar☐ylic acids on these resins was compared with results obtained from silica-based cation exchangers functionalized with alkylsulfonic acid or phenylsulfonic acid groups. The contribution of different retention mechanisms like ion exclusion, hydrophobic interaction and adsorption to the separation of the analytes on these chromatographic supports was discussed. Additionally the applicability of silica-based cation exchangers was tested in the field of silage analysis. 相似文献
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《Comptes Rendus Chimie》2016,19(10):1247-1253
High surface area mesoporous silica based catalysts have been prepared by a simple hydrolysis/sol–gel process without using any organic template and hydrothermal treatment. A controlled hydrolysis of ethyl silicate-40, an industrial bulk chemical, as a silica precursor, resulted in the formation of very high surface area (719 m2/g) mesoporous (pore size 67 Å and pore volume 1.19 cc/g) silica. The formation of mesoporous silica has been correlated with the polymeric nature of the ethyl silicate-40 silica precursor which on hydrolysis and further condensation forms long chain silica species which hinders the formation of a close condensed structure thus creating larger pores resulting in the formation of high surface mesoporous silica. Ethyl silicate-40 was used further for preparing a solid acid catalyst by supporting molybdenum oxide nanoparticles on mesoporous silica by a simple hydrolysis sol–gel synthesis procedure. The catalysts showed very high acidity as determined by NH3-TPD with the presence of Lewis as well as Brønsted acidity. These catalysts showed very high catalytic activity for esterification; a typical acid catalyzed organic transformation of various mono- and di-carboxylic acids with a range of alcohols. The in situ formed silicomolybdic acid heteropoly-anion species during the catalytic reactions were found to be catalytically active species for these reactions. Ethyl silicate-40, an industrial bulk silica precursor, has shown a good potential for its use as a silica precursor for the preparation of mesoporous silica based heterogeneous catalysts on a larger scale at a lower cost. 相似文献
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Xu Y Xu S Emmler T Roelofs F Boettcher C Haag R Buntkowsky G 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(11):3311-3315
Mesoporous pure silicas and functionalized silica with a narrow pore size distribution centered at 3.8 nm were prepared by a novel template, amphiphilic dendritic polyglycerol. The resulting silica materials were characterized by electron microscopy; nitrogen adsorption; (1)H, (13)C, and (29)Si solid-state cross-polarization magic-angle spinning NMR spectroscopy. It was shown that the template could be completely removed from the pure and functionalized silica in an environmentally friendly way by means of a simple water extraction procedure. Furthermore, it was shown that these materials could be easily functionalized, for example, by employing aminopropyl groups. Thus, a new environmentally friendly pathway to this fascinating class of silica material has been opened. 相似文献
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Octyl-functionalized hybrid silica monolithic column for reversed-phase capillary electrochromatography 总被引:1,自引:0,他引:1
Yan LJ Zhang QH Feng YQ Zhang WB Li T Zhang LH Zhang YK 《Journal of chromatography. A》2006,1121(1):92-98
Hybrid silica monolithic stationary phase functionalized with octyl groups was synthesized by a two-step acid/base-catalyzed hydrolysis/co-condensation of tetraethoxysilane (TEOS) and n-octyltriethoxysilane (C(8)-TEOS). The influences of determining factors in the sol-gel process such as the monomer ratio and water content on the monolith formation were systematically investigated. An increase in the TEOS/C(8)-TEOS ratio in the polymerization mixture shifted the pore size distribution towards smaller pore diameter with larger pore volume. The optimal TEOS/C(8)-TEOS volume ratio was found to be 90/50, under which condition the median pore diameter of the monolith was around 1.0 microm with pore volume of 3.25 cm(3)/g. The chromatographic characteristics of the monolithic column prepared with the optimized fabrication condition were studied. Some aromatic compounds including alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs) and phenols were successfully separated on the octyl-functionalized silica monolithic column with high column efficiency up to 180,000 plates/m. 相似文献