聚十二烷基三苯乙炔基硅烷树脂的制备与热性能
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O633. 2

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国家自然科学基金项目(面上项目,重点项目,重大项目)


Preparation and thermal perperty of Polydodecyl(triphenylethynyl)silane resin
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The National Natural Science Foundation of China (General Program, Key Program, Major Research Plan)

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    摘要:

    以镁条、溴乙烷、苯乙炔和十二烷基三氯硅烷为原料,通过格氏反应成功制备十二烷基三苯乙炔基硅烷(DTPES)。采用傅里叶变换红外光谱(FT-IR)和核磁共振波谱(1H-NMR、13C-NMR和29Si-NMR)对DTPES单体结构进行表征;根据非等温差示扫描量热法(DSC)确定单体的固化工艺;借助热聚合法制备聚十二烷基三芳炔基硅烷树脂(PDTPES),并通过热重(TG)和微分热重(DTG)分析研究了PDTPES树脂的热稳定性;采用六种方法(Kissinger、Ozawa、Friedman、Vyazonvkin-Weight、Cosat-Redfern和Achar法)计算得到PDTPES树脂热分解Ea为181.51 kJ/mol,指前因子A为9.65?1011s-1,并求得了热分解动力学方程。

    Abstract:

    Dodecyl (triphenylethynyl) silane (DTPES) was synthesized via Grignard reaction of Dodecyl trichlorosilane and phenyl acetylene in the presence of magnesium and ethyl bromide. Its chemical structure was characterized by nuclear magnetic resonance spectroscopy (1H-NMR 13C-NMR, and 29Si-NMR) and Fourier transform infrared spectroscopy (FT-IR). Its curing process was obtained by Differential Scanning Calorimetry (DSC) and the corresponding Polydodecyl(triphenylethynyl)silane resin (PDTPES) was also synthesized by thermal polymerization. The thermal decomposition behavior was analyzed by TG and DTG and the corresponding kinetic parameters and curing mechanism were discussed by six well-known kinetic methods, i.e., Kissinger, Ozawa, Friedman, Vyazonvkin-Weight, Coast-Redfern and Achar methods. Results show that the average thermal decomposition activation energy Ea was 181.51 kJ/mol and the pre-exponential factor A was 9.65?1011s-1, and the thermal decomposition kinetics equation was also proposed.

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王艳丽,谭德新.聚十二烷基三苯乙炔基硅烷树脂的制备与热性能[J].精细化工,2019,36(2):

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  • 收稿日期:2018-04-17
  • 最后修改日期:2018-07-30
  • 录用日期:2018-08-03
  • 在线发布日期: 2019-02-18
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