Kireev Vyacheslav V, Bilichenko Yulya V, Borisov Roman S, Mu Jianxin, Kuznetsov Dmitry A, Eroshenko Anastasiya V, Filatov Sergey N, Sirotin Igor S
Department of Plastics, Mendeleev University of Chemical Technology of Russia, Miusskaya sq. 9, 125047 Moscow, Russia.
Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, Leninskii pr. 29, 119991 Moscow, Russia.
Polymers (Basel). 2019 Nov 20;11(12):1914. doi: 10.3390/polym11121914.
Phosphazene-containing epoxy oligomers (PEO) were synthesized by the interaction of hexachlorocyclotriphosphazene (HCP), phenol, and bisphenol A in a medium of excess of epichlorohydrin using potassium carbonate and hydroxide as HCl acceptors with the aim of obtaining a product with lower viscosity and higher phosphazene content. PEOs are mixtures of epoxycyclophosphazene (ECP) and a conventional organic epoxy resin based on bisphenol A in an amount controlled by the ratio of the initial mono- and diphenol. According to P NMR spectroscopy, pentasubstituted aryloxycyclotrophosphazene compounds predominate in the ECP composition. The relative content in the ECP radicals of mono- and diphenol was determined by the MALDI-TOF mass spectrometry method. The organic epoxy fraction, according to gas chromatograpy-mass spectrometry (GC-MS), contains 50-70 wt % diglycidyl ether of bisphenol A. PEO resins obtained in the present work have reduced viscosity when compared to other known phosphazene-containging epoxy resins while phosphazene content is still about 50 wt %. Resins with an epoxy number within 12-17 wt %, are cured by conventional curing agents to form compositions with flame-retardant properties, while other characteristics of these compositions are at the level of conventional epoxy materials.
含磷腈环氧低聚物(PEO)是通过六氯环三磷腈(HCP)、苯酚和双酚A在过量环氧氯丙烷介质中相互作用合成的,使用碳酸钾和氢氧化钾作为氯化氢受体,目的是获得具有较低粘度和较高磷腈含量的产品。PEO是环氧环磷腈(ECP)和基于双酚A的传统有机环氧树脂的混合物,其含量由初始单酚和双酚的比例控制。根据磷核磁共振光谱,五取代芳氧基环磷腈化合物在ECP组成中占主导地位。通过基质辅助激光解吸电离飞行时间质谱法测定了ECP基团中单酚和双酚的相对含量。根据气相色谱 - 质谱联用(GC-MS)分析,有机环氧部分含有50 - 70 wt%的双酚A二缩水甘油醚。与其他已知的含磷腈环氧树脂相比,本工作中获得的PEO树脂粘度降低,而磷腈含量仍约为50 wt%。环氧值在12 - 17 wt%范围内的树脂可通过传统固化剂固化,形成具有阻燃性能的组合物,而这些组合物的其他特性与传统环氧材料相当。