无卤阻燃剂1,2-亚乙基双膦酸四甲酯的合成

以亚磷酸三甲酯和1,2-二溴乙烷为原料,在催化剂(CH3)4NI的作用下合成了一种无卤环保型阻燃剂1,2-亚乙基双膦酸四甲酯。当反应温度为160℃,反应时间4.0 h,n(亚磷酸三甲酯)∶n(1,2-二溴乙烷)=3.0∶1.0,催化剂用量为原料质量的0.5%时,该产品产率可达90.9%。用高分辨质谱仪、红外光谱仪及核磁共振波谱仪对产品结构进行了表征,并对该反应条件进行了探讨。

Synthesis of Halogen-free Flame Retardant 1,2-Ethylene Bis(Dimethyl Phosphonate)

1,2-Ethylene bis(dimethyl phosphonate) was synthesized with trimethyl phosphite and 1,2-dibromoethane as base material and tetramethyl ammonium iodide as catalyst.It′s a kind of flame retardant which is environment-friendly and halogen-free.The optimal reaction conditions were obtained:the reaction temperature being 160 ℃,the reaction time being 4.0 h,the molar ratio of trimethyl phosphite to 1,2-dibromoethane being 3.0∶1.0,the mass of the catalyst being 0.5% of the reactant.The yield under these optimum reaction conditions was up to 90.9%.ESI-MS,IR and 1HNMR were used to characterize its chemical structure,and the reaction conditions were discussed in detail.