摘要
以混合烷氧基硅烷和三甲基氯硅烷为原料,以盐酸为催化剂,采用水解-缩聚法制备了三甲基硅基封端同时包含乙烯基、氢、苯基的体型聚硅氧烷(无溶剂有机硅浸渍树脂),配合氯铂酸-乙烯基硅氧烷催化剂和抑制剂,配制无溶剂有机硅浸渍漆.研究了无溶剂有机硅浸渍树脂合成工艺中反应温度、反应时间、酸的浓度、水/烷氧基配比等因素对聚合物制备的影响规律.研究了硅乙烯基、苯基含量和硅氢/硅乙烯基配比对无溶剂有机硅浸渍树脂性能的影响规律.研究结果表明,最佳的制备工艺:水解温度为60℃,反应时间4 h,盐酸的质量分数为14%,水/烷氧基配比为0.5∶1.当硅乙烯基摩尔分数为7.8%,苯基摩尔分数为45%,硅氢/硅乙烯基配比为1.26∶1时,拉伸及弯曲性能最佳.采用红外、核磁、TGA等手段对无溶剂有机硅浸渍树脂进行结构表征和分析,并测试其机械、耐热和绝缘等性能.
Taking mixed alkoxysilane and trimethylchlorosilane as the raw materials,hydrochloric acid as the catalyst and trimethylsilyl as the end-capping agent,the bulk polysiloxane(solvent-free silicone impregnated resin)containing vinyl,hydrogen and phenyl groups was synthesized by hydrolysis-condensation method.Coupled with the catalysts and inhibitors of chloroplatinic acid-vinylsiloxane,solvent-free silicone impregnating varnish was prepared.The influences of some factors such as reaction temperature,reaction time,acid concentration and the mole ratio of water to alkoxy group on the synthesis of silicone impregnated varnish were studied.The effects of Si-Vi content,phenyl content,and molar ratio of Si-H to Si-Vi on the properties of solvent-free silicone impregnating resin were investigated.The results showed that the optimum preparation process was that hydrolysis temperature was 60℃,reaction time was 4 h,acid concentration was 14%,the molar ratio of water to alk-oxy group was 0.5∶1.When Si-Vi content was 7.8%,phenyl content was 45%,and the molar ratio of Si-H to Si-Vi was 1.26∶1,the tensile and bending properties were the best.The structure and analysis of solvent-free silicone impregnating varnish were performed by the means of IR,NMR and TGA,and the mechanical,heat-resistance and insulation properties were tested as well.
作者
侯新瑞
宋华锋
刘美辰
李美江
HOU Xinrui;SONG Huafeng;LIU Meichen;LI Meijiang(Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education,Hangzhou Normal University,Hangzhou 311121,China)
出处
《杭州师范大学学报（自然科学版）》
CAS
2020年第1期21-27,共7页
Journal of Hangzhou Normal University(Natural Science Edition)
基金
浙江省自然科学基金项目(LY17A010018).
关键词
水解-缩聚反应
无溶剂
有机硅浸渍树脂
制备
hydrolysis-polycondensation reaction
solvent-free
organosilicon impregnating varnish
preparation
