摘要
以三甲氧基硅烷与γ-氯丙烯为原料,以自制多羰基配位钌的氯化物为催化剂合成了γ-氯丙基三甲氧基硅烷。考察了溶剂环境、催化剂用量、反应温度、加料方式、物料配比及反应时间等对反应产物的影响。较佳的反应条件为:在无溶剂环境下,温度为75~95℃,钌催化剂用量为40×10-6,三甲氧基硅烷与γ-氯丙烯的量之比为1. 05~1. 15∶1,采用γ-氯丙烯滴入三甲氧基硅烷的加料方式,保温2 h。此条件下,γ-氯丙基三甲氧基硅烷的收率达96%。
The synthesis of γ -chloropropyltrimethoxy silane from trimethoxysilane and γ -chloropropene was studied. The effects of solvent environment, amount of catalyst, reaction temperature, feeding sequence, material ratio and reaction time on the reaction products were discussed. The results show that the temperature ranges from 75℃ to 95℃ in the solvent-free environment. When the amount of ruthenium catalyst was 40μg/g, the molar ratio of trimethoxysilane to γ -chloropropene was 1.05, 1.15∶ 1, the target yield of γ -chloropropyltrimethoxy silane was 96%, which was synthesized by dropping γ -chloropropene into trimethoxysilane.
作者
刘成刚
刘文辉
张先亮
张波
黄驰
廖俊
王晓玲
LIU Cheng-gang 1,2 , LIU Wen-hui 3 , ZHANG Xian-liang 1 , ZHANG Bo 2 ,HUANG Chi 1,4 , LIAO Jun 4 , WANG Xiao-ling 1 ,4(1. College of Chemistry and Molecular Sciences, National Demonstration Center for Experimental Chemistry Education(Wuhan University), Wuhan University,Wuhan 430072, Hubei;2. Hubei Wuda Silicone New Material Co., Ltd., Wuhan 430072, Hubei;3. Jianghe Chemical Factory of CSSG, Yuan'an 444200, Hubei;4. Hubei Military-Civilian Integration and Co-Innovation Center of Aerospace Power and Materials Technology, Wuhan 430072, Hubei)
出处
《有机硅材料》
CAS
2018年第5期345-349,共5页
Silicone Material
基金
国家自然科学基金项目(51572201)
国家"基础学科拔尖学生培养试验计划"(20160210)
武汉大学实验中心开放实验项目(WHU-2018-XYKF-10)