高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (12): 2332.

• 研究论文 • 上一篇    下一篇

表面含磺酸基的介孔分子筛催化剂SBA-15-SO3H的制备及其催化性能

袁兴东1,2, 沈健1, 李国辉2, 周敬来2, 金知晚3, 朴尚颜3   

  1. 1. 抚顺石油学院石油化工系, 抚顺113001;
    2. 中国科学院山西煤炭化学研究所, 太原030001;
    3. 韩国化学研究院, 分子工程催化中心, 大田305600
  • 收稿日期:2002-02-19 出版日期:2002-12-24 发布日期:2002-12-24
  • 通讯作者: 袁兴东(1966年出生),男,博士,教授,主要从事石油化工催化剂研究.E-mail:yuanxdong@sina.com E-mail:yuanxdong@sina.com

Prepararion of Highly Active Esterification Catalyst SBA-15 Mesoporous Silica Functionalized with Sulfonic Acid Group

YUAN Xing-Dong1,2, SHEN Jian1, LI Guo-Hui2, ZHOU Jing-Lai2, KIM Ji-Man3, PARK Sang-Eon3   

  1. 1. Department of Petrochemical Technology, Fushun Petroleum Institute, Fushun 113001, China;
    2. Institute of Coal Chemistry, Chienese Acadamy of Sciences, Taiyuan 030001, China;
    3. Catalysis Center for Molecular Engineering, Korea Research Institute of Chemical Technology(KRICT), PO Box 107, Yusong Taejon 305-600, Korea
  • Received:2002-02-19 Online:2002-12-24 Published:2002-12-24

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摘要： 采用直接和后合成两种方法制备出含磺酸基的介孔分子筛SBA-15-SO3H,用XRD和红外光谱分析制备过程中催化剂结构和组成的变化.结果表明,两种方法制备出的含磺酸基的催化剂都保持了SBA-15分子筛的完整晶体结构,并含有质子酸中心—SO3H;固体核磁共振表征结果证明,两种方法都使MPTMS存在于分子筛的表面;用N2吸附-脱附测定了它们的比表面积、孔径和孔容;TGA分析认为,MPTMS在分子筛表面的热稳定性大于300℃,酸碱滴定结果说明,直接法获得的催化剂的酸中心多于后合成法.酯化反应结果表明,直接法合成的催化剂比后合成法具有更高的稳定性,且简便、快捷、高效.

关键词: 介孔分子筛, SBA-15, 固体酸, 磺酸, 表面改性, 多相催化剂, 酯化

Abstract: Well-ordered, mesoporous, hybrid SBA-15 materials containing alkyl(methyl) and sulfonic acid group were prepared by post and direct-synthesis methods in the presence of triblock copolymer P123 as the structure-directing agent under acid conditions. The materials have been characterized by powder X-ray diffraction,nitrigon gas sorption(BET), FTIR, themogravimetric weight loss(TGA) and solid state 29Si MAS NMR. XRD result shows the two kinds of catalysts have the SBA-15 structure characters (hexagonal, p6mm). FTIR and 29Si-MAS-NMR results show the surface of SBA-15 functionalized by the organic-silica group and the acid site is B acid site. BET shows them has a large surface area and large pore size. TGA shows they have a higher thermal stability than sulfonic acid resin. They are efficient catalysts for the esterification of methanol with oleic acid. The d-SBA-15-SO3H catalyst has a higher hydrothermal stability and hydrophobicity than p-SBA-15-SO3H. The d-SBA-15-SO3H can be reused many times, and the activity can retain stable. The direct synthesis method is more simple, convenient and efficient comparison with the post synthesis method.

Key words: Mesoporous zeolite, SBA-15, Solid acid, Sulfonic acid, Surface modification, Heterogeneous catalyst, Esterification

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