甲基硅酸三环膦酸酯阻燃剂的合成与应用研究

Synthesis and application of methyl silicate tricyclic phosphate flame retardants

以甲基三甲氧基硅烷和笼状亚膦酸酯4-乙基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷为原料,合成有机硅膦阻燃剂甲基硅酸三环膦酸酯。考察了溶剂、反应时间、反应温度、物质的量比等对收率的影响,最佳的反应条件为:n(甲基三甲氧基硅烷)∶n(MSTRP)=1∶3,170℃反应18 h,收率为80.7%。采用FTIR、1H NMR和极限氧指数等技术表征了产物的结构和性能。应用性能测试结果表明,该产物阻燃效能高,与不饱和树脂相容性好,因此,有很好的开发应用前景。

An organic silicate phosphine flame retardant, methyl silicate tricyclic phosphonate was synthesized from methyltrimethoxysilane and cage phosphite ester 4-ethyl-2,6,7-trioxa-l-phosphorus-bicyclo [2.2.2] octane. The effects of solvent types ,reaction temperature and reactant ratio on the synthesis were investigated. The prod- uct yield reached 80.7% under the optimal conditions of n[CH3Si（CH3O）3]：n[MSTRP]=1：3 with the reaction at 170 ℃ for 18 hours. The structure and flame retardance of the product was characterized by means of FTIR, ^1H NMR, and limiting oxygen index technique. The results show that the product takes high flame-retarded effi- ciency and good unsaturated resin compatibility. Therefore, it has promising development prospects.