硅氢加成法合成环己基甲基二甲氧基硅烷  

Synthesis of Cyclohexylmethyldimethoxysilane by Hydrosilylation Method

作　　者：韦正友[1] 余茂宽 陈少永[1] 张利民[1] 陶兆林[1] 

机构地区：[1]蚌埠医学院公共课程部,安徽蚌埠233003 [2]安徽富博精细化工股份有限公司质控部,安徽蚌埠233030

出　　处：《精细化工》2003年第2期98-100,114,共4页Fine Chemicals

基　　金：安徽省教委自然科学研究计划资助项目 ( 98JL174)~~

摘　　要：对环己基甲基二甲氧基硅烷 (CMMS) (合成聚丙烯的助催化剂 )的合成进行了研究。以环己烯和甲基氢二氯硅烷 (DCMS)为原料 ,在硅氧烷铂配合物催化下制得中间体环己基甲基二氯硅烷 (CMCS) ,再与甲醇反应 ,制备终产物CMMS。合成中间体最佳工艺条件为 :反应温度 80～ 90℃ ,n(环己烯 )∶n(DCMS) =1 0 0∶1 2 2 ,1mol环己烯用催化剂 0 80mL ,叔丁醇 1 0mL ,反应时间 4h ,收率 87 9%;终产物的合成条件为 :第一阶段反应室温下进行 ,n(甲醇 )∶n(CMCS) =1 2 2∶1 0 0 ;第二阶段反应温度≤ 40℃ ,n(甲醇 )∶n(CMCS) =5 0 0∶1 0 0 ,通过减压及用甲醇作为氯化氢吸收剂 ,分液操作 ,除去反应副产物氯化氢。残留产品中的氯化氢用甲醇钠溶液中和 ,得目标产物CMMS ,收率 73 5 %,w(CMMS) =99 2 5 %(GC)。用IR、GC -MS对CMMS的结构进行了表征。本工艺操作简便 ,原料价廉易得 ,成本较低 ,适于工业化生产。Synthesis of the title compound (CMMS) as a cocatalyst for synthesis of polypropylene was studied.Thus, with cyclohexene and dichloromethylsilane as starting materials,via hydrosilylation under the catalysis of platinum complex of alkylsiloxanes,the intermediate cyclohexylmethyldichlorosilane (CMCS) was formed which then reacted with methanol to give the final product CMMS.The optimum reaction conditions were as follows. For the intermediate,with 82.0 g cyclohexene,the mole ratio of cyclohexene to dichloromethylsilane was 1.00∶1.22, the reaction temperature was 80-90 ℃,the amount of the catalyst was 0.80 mL,the amount of tertiary butanol was 1.0 mL,and the reaction time was 4 h.The yield of CMCS was 87.9%.For the final product, the mole ratio of methanol to CMCS was 1.22∶1.00 in the first-stage reaction at room temperature and then 5.00∶1.00 in the second-stage reaction at ≤40 ℃ liquid temperature under reduced pressure .The hydrogen chloride formed was absorbed in methanol in the upper layer and was removed.The remaining hydrogen chloride in the separated alkoxysilane was neutralized with sodium methoxide.The yield of CMMS was 73.5% and the mass fraction by GC was 99.25%.The structure of CMMS was characterized by IR and GC-MS.This method provides a better way to obtain CMMS and is simple,mild and suitable for industrial production due to its low cost.

关 键 词：硅氢加成法 合成 环己基甲基二甲氧基硅烷 环己基甲基二氯硅烷 

分 类 号：TQ264.14[化学工程—有机化工]