十二烷基三甲氧基硅烷的合成

Synthesis of dodecyltrimethoxysilane

以三氯氢硅、1-十二碳烯为原料,在铂催化剂存在下合成出十二烷基三氯硅烷;并以溶剂法醇解得到十二烷基三甲氧基硅烷。考察了催化剂用量、原料配比、反应时间对加成反应的影响,溶剂、原料配比、温度等因素对醇解反应的影响。最佳反应条件为:在加成反应中,当铂催化剂与三氯氢硅的量之比为3.6×10-4∶1、三氯氢硅与1-十二碳烯的量之比为1.15∶1时,十二烷基三氯硅烷的收率达81%,反应在室温下无诱导期即可发生、且无需改变加料方式、反应时间短、副反应少、收率高;醇解反应采用溶剂法,将十二烷基三氯硅烷滴加到甲醇中,十二烷基三氯硅烷与甲醇的量之比为1∶3.2,底温控制在70℃,N2流量为80 mL/min,十二烷基三氯硅烷的滴加速度为1 mL/min,十二烷基三甲氧基硅烷的收率为85%。

The dodecyltrichlorosilane was prepared by the addition of trichlorosilane and HSiCl_3 catalyzed by platinum compound.Then dodecyltrimethoxysilane was synthesized by alcoholysis reation in the solvent.The effects of reaction conditions on the hydrosilylation and alcoholysis,such as amount of catalyst,material proportion and reaction temperature were reviewed.The optimum conditions for the hydrosilylation were that the mol-ration of platinum catalyst to methyldichlorosilane was 3.6×10^(-4):1,and the mol-ration of α-alkene to trichlorosilane was 1:1.15,the yield of dodecyltrichlorosilane reached 81%.The additive reaction could take place at room temperature without inducing time.When adding dodecyltrichlorosilane into methanol,the mol-ratio of dodecyltrichlorosilane and methanol was 1:3.2,the solvent was xylene,the reaction temperature was 70 ℃,the flow of N_2 was 80 mL/min and dropping rate was 1 mL/min,the yield of dodecyltrimethoxysilane was 85%.