To investigate the thermal properties of poly ( vinyltri ( phenylethynyl ) silane ) s ( PVTPES ) , vinyltri (phenylethynyl)silane (( Ph C�C )3—Si—CH�CH2 )(VTPES)was synthesized with vinyltrichlorosilane and phenylethynyl by Grignard reaction. Fourier transform infrared ( FT-IR ) and nuclear magnetic resonance (1H-NMR, 13C-NMR, 29Si-NMR) were used to characterize the molecular structure. Polymer of poly (vinyltri( phenylethynyl) silane) s was prepared by thermal polymerization of VTPES monomer and further characterized by TGA-DTG to get the corresponding thermal decomposition kinetic parameters. The results showed that the decomposition temperature at 5% weight loss ( Td5%) of the resin was about 550℃, and char yield (800 ℃) was approximately 80%. The Ea were 266.55 kJ/mol and 236.89 kJ/mol by Kissinger and Ozawa methods, respectively;the reaction order was 0.93 by Crane equation suggesting that the decomposition reaction was the first order reaction.%为研究聚乙烯基三苯乙炔基硅烷树脂的热性能，以苯乙炔和乙烯基三氯硅烷为原料，运用格利雅反应合成了乙烯基三苯乙炔基硅烷单体，并通过红外（ FT－IR）、核磁（1 H－NMR，13 C－NMR，29 Si－NMR）证实了合成产物．以此单体为原料，通过热聚合法制备了聚乙烯基三苯乙炔基硅烷树脂，并采用TGA－DTG研究该聚合物的热分解动力学，计算了相应动力学参数．结果表明：该树脂的热分解温度（Td5％）在550℃左右，800℃时聚合物的残炭率约80％；用Kissinger法和Ozawa法求得的聚合物热分解活化能分别为266．55和236．89 kJ／mol；用Crane法求得聚合物的热分解反应级数为0．93，近似为一级反应．
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