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1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷的制备
引用本文:黄允河,何冰晓,陈关喜,吴清洲,冯建跃.1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷的制备[J].浙江大学学报(理学版),2016,43(4):416-419.
作者姓名:黄允河  何冰晓  陈关喜  吴清洲  冯建跃
作者单位:1. 浙江大学 化学系, 浙江 杭州 310027;
2. 浙江大学 分析测试中心, 浙江 杭州 310027
基金项目:浙江省重大科技专项重点工业项目(2013C01087)
摘    要:以二甲基氯硅烷和γ-氯丙烯为原料,经硅氢加成、水解缩合两步反应得到双官能团有机硅烷单体1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷,总产率为81.0%.对第1步硅氢加成反应进行了条件优化,确定最佳条件为:反应时间5 h,催化剂用量2×10-5 g·mL-1,反应物配比1∶1,此时产率可达83.8%;第2步水解缩合反应产率为96.7%.采用红外光谱、核磁共振、气相色谱-质谱联用等检测方法对产物进行了结构鉴定.

关 键 词:二甲基氯硅烷  γ-氯丙烯  1  3-双(γ-氯丙基)-1  1  3  3-四甲基二硅氧烷  硅氢加成  水解缩合  
收稿时间:2015-10-10

Preparation of 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane
HUANG Yunhe;HE Bingxiao;CHEN Guanxi;WU Qingzhou;FENG Jianyue.Preparation of 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane[J].Journal of Zhejiang University(Sciences Edition),2016,43(4):416-419.
Authors:HUANG Yunhe;HE Bingxiao;CHEN Guanxi;WU Qingzhou;FENG Jianyue
Institution:1. Department of Chemistry, Zhejiang University, Hangzhou 310027, China;
2. Center of Analysis and Measurement, Zhejiang University, Hangzhou 310027, China
Abstract:1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane is a reactive functional group terminated siloxane, which is synthesized using dimethylchlorosilane and allyl chloride as starting materials. Through hydrosilylation and hydrolytic condensation, 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane was prepared in a total yield of 81%. The optimal conditions of hydrosilylation were studied. The yield of hydrosilylation was 83.8% when the reaction time was 5 h, the amount of platinum catalyst was 2×10-5 g·mL-1 and the ratio of reactants was 1∶1. The yield of hydrolytic condensation was 96.7%. Additionally, IR, 1H NMR and gas chromatography-mass spectrometer were used to characterize the structure of target product.
Keywords:dimethylchlorosilane  allyl chloride  1  3-bis(γ-chloropropyl)-1  1  3  3-tetramethyldisiloxane  hydrosilylation  hydrolytic condensation
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