摘要
采用氧化亚铜和四甲基乙二胺复合体系催化丙烯腈与甲基二氯氢硅烷，硅氢加成反应合成了β-氰乙基甲基二氯硅烷。经质谱和核磁共振氢谱证实了其结构。考察了催化体系中水分、加料方式、催化剂中Cu/N配比、原料配比和反应温度对产物收率的影响。结果表明，较佳的工艺为：催化剂的水分处理方法为四甲基乙二胺用分子筛处理，氧化亚铜真空干燥脱水；加料方式为将四甲基乙二胺和氧化亚铜复合催化剂（Cu、N摩尔比为0.2）投入到反应瓶预热到100～110℃，缓慢将甲基二氯氢硅烷混合物和丙烯腈（摩尔比为1.2:1）从瓶底滴加到反应瓶中。在此条件下，β-氰乙基甲基二氯硅烷收率最高，可达73.1%。
Theβ-cyanoethylmethyldichlorosilane was successfully prepared by the hydrosilylation of acrylonitrile and methyl dichlo-rohydrosilane in the presence of tetramethyl ethylene diamine(TMEDA)and cuprous oxide(Cu2O)composite catalyst system.The stmcture ofβ-cyanoethylmethyldichlorosilane was confinmed by mass spectrometry and nuclear magnetic resonance spectroscopy.The impacts of the moisture in the catalytic system,the feeding way,the molar ratio of Cu to N of the catalyst,the ratio of the raw material,and the reaction temperatures on the yield of the product were investigated.The results showed that the optimal process conditions were proposed as following:moisture treatment methods of catalysts were TMEDA and cuprous oxide dehydrated by molecular sieve and vacuum drying respectively.Feeding way was that composite catalyst of TMEDA and cuprous oxide(mole ratio of Cu to N was0.2)were adding into the reaction bottle heating to100~110and then the mixture of acrylonitrile and methyl dichlorohydrosilane(molar ratio was1.2:1)was added dropwise from the bottom of the flask.Under this condition,the yield ofβ-cyanoethylmethyldichlorosilane reached the highest,up to73.1%.
作者
邓冬云
唐红定
Deng Dongyun;Tang Hongding(College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072;Zhejiang Zhongtian Fluorine & Silicone Material Co., Ltd, Quzhou, Zhejiang 324004)
出处
《化工生产与技术》
CAS
2016年第5期35-37,共3页
Chemical Production and Technology
关键词
β-氰乙基甲基二氯硅烷
硅氢加成反应
制备
氧化亚铜
四甲基乙二胺
丙烯腈
甲基二氯氢硅烷
β-cyanoethylmethyldichlorosilane
hydrosilylation
preparation
cuprous oxide
tetramethyl ethylenediamine (TMEDA)
acrylonitrile
methyl dichlohydrosilane
