环己基甲基二氯硅烷的合成工艺

STUDY ON SYNTHETIC TECHNIQUE OF CYCLOHEXYLMETHYLDICHLOROSILANE

在一定的压力下,以甲基二氯硅烷(DCMS)和环己烯为原料、以硅氧烷铂配合物为催化剂,以苯甲醛为促进剂,进行了用氢硅烷化法合成环己基甲基二氯硅烷(CMCS)的工艺研究。考察了原料配比、反应温度、反应压力、催化剂用量、促进剂种类、反应时间等因素对CMCS收率的影响。得到合成CMCS的最佳工艺条件为:反应压力0.7-0.8MPa,n(环己烯):n(DCMS)=1.00:1.12,反应温度85-90℃,1mol环己烯用催化剂1.0mL,苯甲醛2.0mL,反应时间5-6h,CMCS收率89.6%,w(CMCS)=99.54%。用1HNMR、IR、MS对CMCS的结构进行了表征。

The cyclohexylmethyldichlorosilane(CMCS) was synthesized from dichloromethylsilane and cyclohexene(CH) via hydrosilylation with the complex of platinum and alkylsiloxanes as catalyst and benzaldehyde as promoter under pressure. The influencing factors such as molar ratio of raw materials, reaction temperature, reaction pressure, quantity of catalysts, type of promoter and reaction time on the yield of CMCS were studied. The optimum reaction conditions were found as follows: reaction pressure 0. 7-0. 8 MPa, molar ratio of cyclohexene to dichloromethylsilane 1. 00:1. 12, reaction temperature 85-90 ℃, amount of catalyst 1. 0 mL/mol CH, amount of benzaldehyde 2. 0 mL/mol CH and reaction time 5-6 h. The yield of CMCS is 89. 6% and the purity of CMCS analyzed by GC is 99. 54%. The structure of CMCS was characterized by FTIR, 1H NMR and MS.