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用十二烷基胺代替传统的季铵盐合成了中孔全硅分子筛HMS,并将硅钨杂多酸(SiW12)浸渍固载在HMS上.用XRD,FT-IR以及NH3-TPD等手段对HMS及不同负载量和焙烧温度的负载催化剂进行了表征.即使在固载量为50%的SiW12/HMS中,SiW12仍保持其Keggin结构并均匀分布在载体表面上,没有SiW12晶相生成.同时,在气-固相反应体系中研究了固载在HMS上的SiW12在合成乙酸丁酯中的催化性能.实验结果表明,200℃焙烧可以增强杂多酸与HMS内表面之间的相互作用,从而使其对酯化反应活性具有一定的影响,并且固载催化剂在较低反应温度下具有较高的酯化活性,且性能稳定,有一定的应用前景.
Mesopore all-silicon molecular sieve HMS was synthesized by using dodecylamine instead of the traditional quaternary ammonium salt, and impregnated with HMS on SiW12. XRD, FT-IR and NH3-TPD were used to characterize HMS and supported catalysts with different loadings and calcination temperatures. Even in SiW12 / HMS with a 50% loading, SiW12 retains its Keggin structure and is uniformly distributed on the surface of the support without SiW12 crystal phase formation. Meanwhile, the catalytic performance of SiW12 immobilized on HMS in the synthesis of butyl acetate was studied in a gas-solid reaction system. The experimental results show that the calcination at 200 ℃ can enhance the interaction between the heteropolyacid and the inner surface of HMS so that it has a certain influence on the esterification activity and the immobilized catalyst has a higher ester at the lower reaction temperature Activity, and stable performance, have certain application prospects.