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含三氟乙烯基醚基团有机硅树脂的合成与热稳定性研究

Study on the Synthesis and Thermal Stability of Silicone Resin Containing Trifluorovinyl Ether Groups.

作者信息

Huang Rui, Yao Jinshui, Mu Qiuhong, Peng Dan, Zhao Hui, Yang Zhizhou

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

Polymers (Basel). 2020 Oct 5;12(10):2284. doi: 10.3390/polym12102284.

Abstract

Silicone resin is a high-temperature resistant material with excellent performance. The improvement of its thermal stability has always been the pursuit of researchers. In this paper, a sequence of silicone resins containing trifluorovinyl ether groups were prepared by the co-hydrolysis-polycondensation of methyl alkoxysilane monomers and {4-[trifluorovinyl(oxygen)]phenyl}methyldiethoxysilane. The structures of the silicone resins were characterized by FT-IR and H NMR. The curing process of them was studied by DSC and FT-IR spectra, and results showed that the curing of the resins included the condensation of the Si-OH groups and the [2 + 2] cyclodimerization reaction of the TFVE groups, which converted to perfluorocyclobutane structure after curing. The thermal stability and thermal degradation behavior of them was studied by TGA and FT-IR spectra. Compared with the pure methyl silicone resin, silicone resins containing TFVE groups showed better thermal stability under both N and air atmosphere. Their hydrophobic properties were characterized by contact angle test. Results showed that PFCB structure also improved the hydrophobicity of the silicone resin.

摘要

有机硅树脂是一种性能优异的耐高温材料。提高其热稳定性一直是研究人员追求的目标。本文通过甲基烷氧基硅烷单体与{4-[三氟乙烯基(氧)]苯基}甲基二乙氧基硅烷的共水解缩聚反应制备了一系列含三氟乙烯基醚基团的有机硅树脂。通过傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(H NMR)对有机硅树脂的结构进行了表征。利用差示扫描量热法(DSC)和傅里叶变换红外光谱对其固化过程进行了研究,结果表明树脂的固化包括硅羟基(Si-OH)的缩合以及三氟乙烯基醚(TFVE)基团的[2 + 2]环二聚反应,固化后转化为全氟环丁烷结构。通过热重分析(TGA)和傅里叶变换红外光谱对其热稳定性和热降解行为进行了研究。与纯甲基有机硅树脂相比,含TFVE基团的有机硅树脂在氮气和空气气氛下均表现出更好的热稳定性。通过接触角测试对其疏水性能进行了表征。结果表明,全氟环丁烷(PFCB)结构也提高了有机硅树脂的疏水性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a078/7601899/8acf047dfaf7/polymers-12-02284-sch001.jpg

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