支链型硅烯炔树脂的合成与性能

Synthesis and Performances of Branched Silicon-containing Arylethyleneacetylene Resin

以二乙炔基苯(DEB)和甲基三氯硅烷(MTS)为原料,锌粉作催化剂,合成了一种支链型硅烯炔树脂(Branched Silicon-containing Arylethyleneacetylene Resin,BSA)。研究表明,最优反应条件为:物料摩尔配比二乙炔基苯比甲基三氯硅烷为9∶4,80℃温度下回流反应10h,合成树脂的产率达82.4%。树脂在130℃下就可发生固化交联反应,粘度较低,具有良好的加工性能;BSA树脂固化物具有良好的热稳定性,N2氛围下质量分解5%时的温度Td5达到567℃,800℃时质量残留率约为90%。

As a new method of silylation,zinc catalyst has the advantages of simple process,short production cycle,mild reaction condition.However,the thermal stability of the resin is lower than the product catalyzed by Grignard reagents due to terminal ethylene of resin.In order to improve the thermal stability and processing property,Branched Silicon-containing Arylethyleneacetylene Resin(BSA) was prepared by diethynylbenzene and methyltrichlorosilane catalyzed by zinc power.Based on the results of research,we concluded that the optimum reaction conditions:acetonitrile as solvent,temperature of 80℃and reaction time of 10 h,molar ratio of diethynylbenzene and methyltrichlorosilane of 9∶4,and the reaction yield reaches up to82.4%.BSA resin is easily processed and could be cured at the temperature of about 130℃.Cured BSA resin possess excellent thermal stability,the temperature at 5% weight loss is 567℃,and char yield of the cured resin at 800℃ under nitrogen is 90%.