聚(甲基苯基-间乙炔基硅烷)树脂的合成及热稳定性能

Synthesis and Thermal Stability of Poly(Methyl-Phenyl-Diethynyl) Resin

以甲基氢二乙炔基硅烷、甲基氢二氯硅烷和二苯基二氯硅烷为主要原料,通过格氏试剂与二氯硅烷的缩合反应,合成了一种硅炔杂化耐高温树脂聚(甲基苯基-间乙炔基硅烷)(PMPS)。采用傅里叶变换红外光谱、核磁共振和凝胶渗透色谱对其结构进行了表征;利用傅里叶变换红外光谱和差示扫描量热技术分析了树脂的固化行为;采用热重分析考察了树脂固化产物的热稳定性能。结果表明,PMPS树脂的数均相对分子质量为1140,相对分子质量分布系数为1.34,常温下黏度适中,具有良好的加工性能。树脂通过硅氢加成反应和Diels-Alder反应形成交联网络结构,固化产物具有良好的热稳定性,在空气和氮气气氛中失重5%时的温度(Td5)高于550℃,1000℃的质量保留率大于65%。

A novel kind of high temperature-resistant hybrid resin,poly( methyl-phenyl-diethynyl)( PMPS),was prepared by condensation of dichlorosilanes and organic magnesium Grignard regents. The structure of PMPS was characterized by FT-IR,1H-NMR,13C-NMR and GPC. The curing behavior of PMPS was investigated by FT-IR and DSC,the thermal stability of the cured resin was studied by TGA. The results show that the number average molecular weight and distribution coefficient of PMPS are 1140 and 1. 34,respectively. PMPS has moderate viscosity,cured at a relative low temperature and can be easily processed. The resin can form crosslinked network structure through hydrosilylation reaction and Diels-Alder reaction,the cured PASB resins have excellent thermal stability,the temperature of 5% mass loss( Td5) is up to 550 ℃ in nitrogen and air respectively,and the residue at 1000 ℃ is up to 65%.