Synthesis and Characterization of Polysiloxane Containing p-Silphenylene Prepared by Ring-Opening Polymerization and Dehydration Condendation

Qiang HUANG; Ming KANG; Zheng GU; Qing-xia HAN; Yu-hong HUANG

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Synthesis and Characterization of Polysiloxane Containing p-Silphenylene Prepared by Ring-Opening Polymerization and Dehydration Condendation

更新时间：2022-09-18

- Synthesis and Characterization of Polysiloxane Containing p-Silphenylene Prepared by Ring-Opening Polymerization and Dehydration Condendation
- Polymer Bulletin Vol. 26, Issue 12, Pages: 88-93(2013)
- 作者机构：
  
  1.四川省非金属复合与功能材料重点实验室-省部共建国家重点实验室培育基地，绵阳　621010
  2.中国工程物理研究院总体工程研究所，绵阳　621900
- 作者简介：
- 基金信息：
- DOI：
  CLC：
- Published：2013-12，
  
  Received：03 June 2013，
  
  Revised：21 August 2013，
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Qiang HUANG, Ming KANG, Zheng GU, Qing-xia HAN, Yu-hong HUANG. Synthesis and Characterization of Polysiloxane Containing p-Silphenylene Prepared by Ring-Opening Polymerization and Dehydration Condendation. [J]. Polymer Bulletin 26(12):88-93(2013)
DOI：

Qiang HUANG, Ming KANG, Zheng GU, Qing-xia HAN, Yu-hong HUANG. Synthesis and Characterization of Polysiloxane Containing p-Silphenylene Prepared by Ring-Opening Polymerization and Dehydration Condendation. [J]. Polymer Bulletin 26(12):88-93(2013) DOI：

摘要

通过阴离子开环与脱水缩合制备了亚苯基聚硅氧烷

研究了原料比例、催化剂用量、反应温度对反应产率的影响。采用傅里叶变换红外光谱(FT-IR)、核磁氢谱(

H-NMR)、凝胶色谱(GPC)和热重分析(TGA)分别对亚苯基聚硅氧烷的结构、分子量及其分布、热氧化稳定性进行了研究。研究结果表明:该方法成功制备亚苯基聚硅氧烷

产物的实际分子量大于理论值

分子量可控

分子量分布指数(M

)为1.33~1.45;随着原料中对-双(二甲基羟基硅基)苯(BHB)比例的提高

反应产率降低

而增加催化剂用量和提高反应温度有利于产率的提高;聚硅氧烷热稳定性随亚苯基含量的增加而逐渐提高

亚苯基含量为15.09%时

该聚合物10%的失重温度提高到477℃。

Abstract

The polysilcoxane containing p-silphenylene was synthesized through ring-opening polymerization and dehydration condensation. The Effect of proportion of raw materials

amount of catalyst and temperature on the yield of reaction and the content of phenylene on the thermal performance of siloxane were systematically studied in this article. And the structure of the polymer was characterized by fourier transform infrared spectroscopy(FT-IR) and hydrogen nuclear magnetic resonance(

H NMR). Molecular weight characteristics and thermal stability of the silicone were characterized by gel permeation chromatography(GPC) and thermal gravimetric analysis(TGA)

respectively. The results show that polysilicone containing p-silphenylene unit has been successfully prepared with this method and its molecular weight is controllable and greater than theoetical value and polydispersity index is 1.33 to 1.45. The yield is reduced with the increase of BHB in precursors

whereas it is improved with the increase of catalyst and reaction temperature. The 10% weight loss temperature was increased from 352℃ to 477℃ in air when p-silphenylene unit content is 15.09% and p-silphenylene unit significantly improved polysilicone thermal stability at high temperature.

关键词

聚硅氧烷亚苯基开环聚合脱水缩合热氧化稳定性

Keywords

Polysiloxanep-SiphenyleneRing-opening polymerizationDehydration condensationThermal oxidation stability

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