羟甲基膦杂环状甲基膦酸酯的合成与应用

Synthesis and application of hydroxymethyl phosphine heterocyclic methylphosphonate

以三羟甲基膦和甲基膦酸二甲酯为原料,合成有机膦阻燃剂1-氧-1-甲基-4-羟甲基-2,6-二氧杂-1,4-二磷杂环己烷。考察了物质的量比、反应时间和反应温度对产率的影响,确定适宜的反应条件为n(三羟甲基膦)∶n(甲基膦酸二甲酯)=1.04∶1,150℃反应4 h,产率为91.6%。通过FTIR,1H-NMR及极限氧指数等技术表征了产物的结构及性能。应用实验表明,产物在不饱和树脂和环氧树脂中都具有很好的阻燃效果。

An organic phosphine flame retardant,1-methyl-4-hydroxymethyl-2,6-dioxa-1,4-diphosphinane,was synthesized by tris（hydroxymethyl） phosphine and dimethyl methylphosphonate. The effects of molar ratio,reaction temperature and reaction time on the yield were investigated. The optimal conditions were as follows ：n（THMP）∶n（DMMP） is 1.04∶1. The reaction kept going at 150 ℃ for 4 h,the yield can reach 91.6%. The structure and flame retardance of the product were characterized by means of FTIR,1 H-NMR, and LOI. The application in unsaturated resin and epoxy resin shows that the product has a good flame retardant effect.