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；TEOSHCl，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. The mesoporous silica MCM-41 with high crystallinity was synthesized by the route of S + X-I + with cetyl pyridinium bromide (CPBr) as template and tetraethoxysilane (TEOS) as silicon source under optimized operating conditions. Molecular sieve and its yield was improved. The process of molecular sieve stripper was optimized based on the results of TG-DTA. Meanwhile, the relative content of CPBr, TEOSHCl and H2O in the synthesized system was determined by XRD, The influence of the structure and the formation process of the structure are analyzed. It is found that the formation of the S + X-I + path of the MCM-41 structure undergoes the Lamellar → Hexagonal phase transfer process.