Study on the synthesis and thermal degradation of silicone resin containing silphenylene units
Study on the synthesis and thermal degradation of silicone resin containing silphenylene units
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含亚硅基单元有机硅树脂的合成及热降解研究
DOI：
10.1016/j.tca.2011.04.020
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发表时间：
2011-07-10
影响因子：
3.5
通讯作者：
Zhang, Changqiao
中科院分区：
文献类型：
--
作者：
Yang, Zhizhou;Feng, Lei;Zhang, Changqiao
以甲基三乙氧基硅烷和1，4-二（乙氧基二甲基硅基）苯为原料，采用共水解-缩聚法合成了含硅苯单元的有机硅树脂。其结构经傅立叶变换红外光谱（FTIR）和核磁共振（NMR）光谱证实。采用热分析结合红外光谱（TGA-FTIR）、傅立叶变换红外光谱（FTIR）和气相色谱-质谱（GC-MS）等技术研究了硅树脂在氮气气氛下的降解过程。在这些分析的基础上，降解过程分为三个阶段，340-430 ℃，430-675 ℃和675-820 ℃。结果表明，这三个阶段的降解机理是不同的。不同的降解机制提出了每个阶段。第一阶段的降解是由残留的Si-OH基团引起的。Si-C（6）H（4）-Si键的断裂是第二阶段的主要降解途径。第三阶段的重量损失是由于自由基反应引起的甲烷逸出。皇冠版权所有（C）2011由Elsevier BA/出版。All rights reserved.
Silicone resin containing silphenylene units was synthesized through a cohydrolysis-polycondensation method of methyltriethoxysilane and 1,4-bis(ethoxydimethylsilyl)benzene. Its structure was confirmed by Fourier-transformed infrared (FTIR) and nuclear magnetic resonance (NMR) spectra. The degradation under nitrogen atmosphere of the silicone resin was investigated by thermal analysis techniques combined with infrared spectroscopy (TGA-FTIR), FTIR and gas chromatograph-mass spectrometer (GC-MS). On the basis of these analyses, the degradation process was divided into three stages, 340-430 degrees C, 430-675 degrees C, and 675-820 degrees C. It was found that degradation mechanisms of these three stages were distinguishing. Different degradation mechanisms were proposed for each stage. The degradation of the first stage was caused by the residual Si-OH groups. The cleavage of Si-C(6)H(4)-Si bonds was the main degradation way of the second stage. The weight loss of the third stage resulted from the escape of methane caused by a radical reaction. Crown Copyright (C) 2011 Published by Elsevier BA/. All rights reserved.