含硼多乙烯基有机硅树脂的制备及耐热性能研究  

Preparation of boron-containing polyvinyl silicone resin and study on its heat resistance

作　　者：王永生 邓建国[1] 武元鹏[2] 马春彦[1] 纪兰香[1] 白小峰[1] WANG Yongsheng;DENG Jianguo;WU Yuanpeng;MA Chunyan;JI Lanxiang;BAI Xiaofeng(Institute of Chemical Materials,China Academy of Engineering Physics,Mianyang 621000,China;School of Materials Science and Engineering,Southwest Petroleum University,Chengdu 610500,China)

机构地区：[1]中国工程物理研究院化工材料研究所,四川绵阳621000 [2]西南石油大学材料科学与工程学院,成都610500

出　　处：《功能材料》2020年第7期7045-7050,共6页Journal of Functional Materials

基　　金：四川省重点研发项目资助(2018GZ0539)。

摘　　要：以二苯基二甲氧基硅烷、苯基三甲氧基硅烷和4-联苯硼酸为原料,采用水解-缩合的方法制备不同硼含量的苯基乙烯基杂化硅树脂预聚体(BSiR),并与含氢硅油交联剂在铂催化剂作用下硅氢加成固化得到新型的耐高温有机硅材料-聚硼硅氧烷(PBS)。采用红外光谱、核磁共振、凝胶渗透色谱、热重分析等方法对杂化硅树脂预聚体和固化物进行表征,考察了反应时间、反应温度、组分比例等因素对合成的影响。结果表明,反应温度75℃,反应时间6 h,合成硅树脂的重均相对分子质量Mw为80246 g/mol,数均相对分子质量Mn为99437 g/mol,分布宽度D值为1.24。以该硅树脂预聚体为基料制备的固化物在500℃下失重仅5%。Using diphenyldimethoxysilane,phenyltrimethoxysilane and 4-biphenylboronic acid as raw materials,phenylvinyl hybrid silicone resin prepolymers(BSiR)with different boron contents were prepared by hydrolysis-condensation method.And a new type of high temperature resistant silicone material-polyborosiloxane(PBS)was prepared by hydrosilylation and solidification with the hydrogen-containing silicone oil cross-linking agent under the action of platinum catalyst.Infrared spectroscopy,nuclear magnetic resonance,gel permeation chromatography,and thermogravimetric analysis were used to characterize the hybrid silicone resin prepolymers and cured products.The effects of reaction time,reaction temperature,and component ratio on the synthesis were investigated.The results showed that when the reaction temperature was 75℃and the reaction time was 6 h.the weight average molecular weight Mw of the synthetic silicone resin was 80246 g/mol,the number average molecular weight Mn was 99437 g/mol,and the distribution width D was 1.24.The weight loss of the cured product prepared by using the silicone prepolymer as a base material was only 5%at 500℃.

关 键 词：掺硼有机硅树脂 水解-缩合 4-联苯硼酸 热稳定性 

分 类 号：TQ324.21[化学工程—合成树脂塑料工业]