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含磷硅元素的功能化氧化石墨烯改性环氧树脂的热稳定性和阻燃性能

Thermal Stability and Flame Retardancy Properties of Epoxy Resin Modified with Functionalized Graphene Oxide Containing Phosphorus and Silicon Elements.

作者信息

Zhi Maoyong, Liu Quanyi, Chen Hao, Chen Xiantao, Feng Sihai, He Yuanhua

机构信息

College of Civil Aviation Safety Engineering, Civil Aviation Flight University of China, Deyang 618307, People's Republic of China.

出版信息

ACS Omega. 2019 Jun 24;4(6):10975-10984. doi: 10.1021/acsomega.9b00852. eCollection 2019 Jun 30.

DOI:10.1021/acsomega.9b00852
PMID:31460195
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6648042/
Abstract

Phosphorus- and silicon-modified graphene oxide was prepared to improve the thermal stability and flame retardancy properties of epoxy resin. 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and vinyltriethoxysilane (VTES) were successfully grafted onto the surface of graphene oxide (GO) through solvothermal synthesis and hydrolysis-condensation reaction, respectively. Subsequently, the functionalized graphene oxide grafted by DOPO and VTES (DOPO-VTES-GO) was incorporated into the epoxy resin by the solution blending method. The effect of DOPO-VTES-GO on the thermal stability and flame-retardant properties of epoxy resin was systematically studied. Thermogravimetric analysis showed that the thermal stability and char residue yield of DOPO-VTES-GO/epoxy were increased obviously compared with those of pure epoxy resin and DOPO-GO/epoxy. Cone calorimeter test results showed that DOPO-VTES-GO/epoxy had better flame retardancy than pure epoxy resin and DOPO-GO/epoxy on reducing the peak of heat release rate, total heat release, and total smoke production. Furthermore, the char residue after the cone calorimeter tests was investigated by scanning electron microscopy-energy-dispersive X-ray spectrometry, Raman spectroscopy, and Fourier transform infrared measurements. These results demonstrated that the DOPO-VTES-GO can enhance the graphitization degree of char residues and promote the formation of the thermally stable char. In addition, the mechanism of flame retardancy was proposed, and DOPO-VTES-GO exerts the synergistic effect mainly by means of catalytic charring in the condensed phase and capturing hydroxyl or hydrogen radicals from thermal decomposition of epoxy resin in the gas phase. This work provides novel insights into the preparation of phosphorus-silicon-graphene oxide ternary synergistic flame retardants for thermosetting polymer materials.

摘要

制备了磷和硅改性的氧化石墨烯，以提高环氧树脂的热稳定性和阻燃性能。分别通过溶剂热合成和水解缩合反应，将9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO）和乙烯基三乙氧基硅烷（VTES）成功接枝到氧化石墨烯（GO）表面。随后，采用溶液共混法将DOPO和VTES接枝的功能化氧化石墨烯（DOPO-VTES-GO）引入环氧树脂中。系统研究了DOPO-VTES-GO对环氧树脂热稳定性和阻燃性能的影响。热重分析表明，与纯环氧树脂和DOPO-GO/环氧树脂相比，DOPO-VTES-GO/环氧树脂的热稳定性和残炭率明显提高。锥形量热仪测试结果表明，在降低热释放速率峰值、总热释放量和总产烟量方面，DOPO-VTES-GO/环氧树脂比纯环氧树脂和DOPO-GO/环氧树脂具有更好的阻燃性。此外，通过扫描电子显微镜-能量色散X射线光谱、拉曼光谱和傅里叶变换红外测量对锥形量热仪测试后的残炭进行了研究。这些结果表明，DOPO-VTES-GO可以提高残炭的石墨化程度，促进热稳定炭的形成。此外，还提出了阻燃机理，DOPO-VTES-GO主要通过凝聚相催化成炭和气相中捕获环氧树脂热分解产生的羟基或氢自由基发挥协同作用。这项工作为热固性聚合物材料的磷-硅-氧化石墨烯三元协同阻燃剂的制备提供了新的见解。

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