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Si-O-Ph交联增强硅树脂的合成与热稳定性研究

Study on the synthesis and thermal stability of silicone resins reinforced by Si-O-Ph cross-linking.

作者信息

Zhang Huadong, Yan Zhongyi, Yang Zhizhou, Yao Jinshui, Mu Qiuhong, Peng Dan, Zhao Hui

机构信息

School of Materials Science and Engineering, Qilu University of Technology (Shandong Academy of Sciences) Jinan 250353 China

Shandong Provincial Key Laboratory of Special Silicone-Containing Materials, Advanced Materials Institute, Qilu University of Technology (Shandong Academy of Sciences) Jinan 250014 China.

出版信息

RSC Adv. 2021 Sep 20;11(49):30971-30979. doi: 10.1039/d1ra05524k. eCollection 2021 Sep 14.

Abstract

A novel silicone resin (SR-OH) containing phenolic hydroxyl (Ph-OH) groups was designed and synthesized co-hydrolysis/condensation and catalytic hydrogenation. During the curing process, the cross-linking degree of the resin was further increased by the Si-O-Ph bonds formed by the reaction of the Ph-OH and terminal Si-OH groups. Thermogravimetric analysis (TGA) showed that the cured resin product exhibited excellent thermal and thermo-oxidative stability, which was much higher than that of a typical methyl phenyl silicone resin (SR-Ph). The temperature at which 5% weight loss occurs ( ) was up to 606 °C (nitrogen) and 542 °C (air), and its char yield at 800 °C was 91.1% and 85.3% in nitrogen and air, respectively. The significant improvement in thermal stability was mainly attributed to the formation of Si-O-Ph bonds which not only increases the cross-linking degree of the resin but also significantly prevents degradation by the 'back-biting' and oxidative cleavage.

摘要

通过共水解/缩合和催化氢化设计并合成了一种新型的含酚羟基(Ph-OH)的硅树脂(SR-OH)。在固化过程中,Ph-OH与末端Si-OH基团反应形成的Si-O-Ph键进一步提高了树脂的交联度。热重分析(TGA)表明,固化后的树脂产品具有优异的热稳定性和热氧化稳定性,远高于典型的甲基苯基硅树脂(SR-Ph)。5%重量损失发生时的温度( )在氮气中高达606℃,在空气中为542℃,其在800℃时在氮气和空气中的残炭率分别为91.1%和85.3%。热稳定性的显著提高主要归因于Si-O-Ph键的形成,该键不仅增加了树脂的交联度,还显著防止了“回咬”和氧化裂解导致的降解。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77cd/9041364/37961034d912/d1ra05524k-s1.jpg

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