间氨基苯乙炔封端聚(间二乙炔基苯-甲基氢硅烷)树脂的合成及性能

摘要

A novel heat-resistant resin, m-aminophenylacetylene terminated poly ( m-dietheynylbenzene-methylsilane ) ( AP-SA) , was synthesized from m-dietheynylbenzene,dichloromethylsilane and m-aminophenylacetylene by using Grignard reagent and ammonolysis method.The structure of APSA was characterized by FT-IR、1H-NMR、13C-NMR and multiple detectors GPC/SEC.The curing behavior of APSA was analyzed by DSC and thermal stability of the cured resin was studied by TGA. Then the dependences between silicon content in the structure and properties of the resin were also discussed. The results show that APSAwith moderate viscosity can be easily processed.The cured resin exhibits excellent thermal stability,the Td5(5% mass loss temperature) and resi-due at 1000 ℃ are up to 634 ℃ and 90.1% under nitrogen,respectively.%以间二乙炔基苯、甲基氢二氯硅烷和间氨基苯乙炔为主要原料,通过格氏试剂法和氨解法,合成了一种耐高温间氨基苯乙炔封端聚(间二乙炔基苯-甲基氢硅烷)树脂(简称APSA树脂). 采用FT-IR、1 H-NMR、13 C-NMR和多检测GPC/SEC对树脂结构进行表征,利用DSC和TGA研究了树脂的固化行为和耐热性能,探讨了结构中硅元素含量对树脂性能的影响. 结果表明,APSA树脂常温下粘度适中,交联固化物具有优异的耐热性能,在N2 气氛下Td5(质量损失5%的温度)达634 ℃,1 000 ℃下的质量保留率为90.1%.