1,3-双(γ-氯丙基)-1,1,3,3-四甲基二硅氧烷的制备

Preparation of 1,3-bis(γ-chloropropyl)-1,1,3,3-tetramethyldisiloxane

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5h,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.

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 of81%.The optimal conditions of hydrosilylation were studied.The yield of hydrosilylation was 83.8% when the reaction time was 5h,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,1 H NMR and gas chromatography-mass spectrometer were used to characterize the structure of target product.