物理化学学报 >> 1998, Vol. 14 >> Issue (03): 243-248.doi: 10.3866/PKU.WHXB19980310

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MCM-41中孔SiO2分子筛合成新方法

张兆荣, 索继栓, 张小明, 李树本   

  1. 中国科学院兰州化学物理研究所羟基合成与选择氧化国家重点实验室，兰州 730000
  • 收稿日期:1997-06-30 修回日期:1997-10-07 发布日期:1998-03-15
  • 通讯作者: 李树本

A Novel Synthesis Method for MCM-41 Mesoporous Silica Molecular Sieves

Zhang Zhao-Rong, Suo Ji-Shuan, Zhang Xiao-Ming, Li Shu-Ben   

  1. State Key Laboratory for Oxo Synthesis and Selective Oxidation,Lanzhou Institute of Chemical Physics,Academia Sinica,Lanzhou 730000
  • Received:1997-06-30 Revised:1997-10-07 Published:1998-03-15
  • Contact: Li Shu-Ben

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摘要：

以溴代十六烷基吡啶（CPBr）为模板剂，正硅酸乙酯（TEOS）为硅源，在优化的操作条件下通过S＋X-I+路径合成了高结晶度的MCM－41中孔SiO2分子筛，并提高了其收率；以TG－DTA结果为基础，对分子筛脱模板剂的过程进行了优化; 同时以XRD对合成物系中CPBr, TEOS, HCl，H2O相对含量对MCM－41分子筛晶相结构的影响以及该结构的形成过程进行了分析，发现MCM－41结构沿S＋X-I+路径的形成经过了Lamellar→Hexagonal相转移历程.

关键词: 溴代十六烷基吡啶, 模板剂, MCM-41中孔SiO2分子筛, 合成

Abstract:

High quality MCM-41mesoporous silica molecular sieves were synthesized in high yield via improved S+X-I+ assembly pathway, by using cetylpyridinium bromide(CPBr) as template and tetraethyl orthosilicate(TEOS) as silica source. The calcination process of as-synthesized samples was optimized on the basis of TG-DTA results. Thus typical MCM-41 sample obtained was characterized by powder X-ray diffraction(XRD) and N2 adsorption-desorption techniques. The effects of CPBr, TEOS, HCl and H2O contents on the MCM-41 mesostucture, as well as the mechanistic steps involved in the formation of the mesophase were also investigated by XRD. It was found that. the titled crystal phase was developed through lamellar to hexagonal mesophase transformation.

Key words: Cetylpyridinium bromide, Template, MCM-41 mesoporous silica molecular sieve, Synthesis