引用本文: | 谭德新,王艳丽,邢宏龙,唐玲,史铁钧.聚乙烯基三苯乙炔基硅烷的制备及热性能分析[J].材料科学与工艺,2015,23(2):63-67.DOI:10.11951/j.issn.1005-0299.20150211. |
| TAN Dexin,WANG Yanli,XING Honglong,TANG Ling,SHI Tiejun.Preparation and thermal properties of polyvinyl(triphenylethynyl)silane[J].Materials Science and Technology,2015,23(2):63-67.DOI:10.11951/j.issn.1005-0299.20150211. |
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摘要: |
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(1H-NMR, 13C-NMR, 29Si-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. |
关键词: 苯乙炔 乙烯基三氯硅烷 格利雅反应 乙烯基三苯乙炔基硅烷 热分解动力学 |
DOI:10.11951/j.issn.1005-0299.20150211 |
分类号:TQ323 |
基金项目:国家自然科学基金资助项目(2,5);安徽省高校自然科学基金重点项目(KJ2013A087, KJ2013A095);安徽理工大学博士基金项目. |
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Preparation and thermal properties of polyvinyl(triphenylethynyl)silane |
TAN Dexin1, WANG Yanli2, XING Honglong1, TANG Ling1, SHI Tiejun3
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(1.School of Chemical Engineering, Anhui University of Science and Technology, Huainan 232001, China; 2.School of Materials Science and Engineering, Anhui University of Science and Technology, Huainan 232001, China; 3.School of Chemical Engineering, Hefei University of Technology, Hefei 230009, China)
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Abstract: |
To investigate the thermal properties of poly(vinyltri(phenylethynyl)silane)s (PVTPES) , vinyltri(phenylethynyl)silane((PhCC)3 —Si—CHCH2)(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. |
Key words: phenylethynylene vinyltrichlorosilane grignard reaction vinyltri(phenylethynyl)silane thermal decomposition kinetics |