阻燃剂甲基苯基甲氧基硅酸单环膦酸酯的合成与应用

Synthesis and Application of Methylphenyl Silicic Acid Monocyclic Phosphonates Flame Retardant

以甲基苯基二甲氧基硅烷和4-乙基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷(简称:笼状亚磷酸酯)为原料,合成了一种有机硅膦阻燃剂——甲基苯基硅酸单环状膦酸酯(MSAMP),讨论了反应温度、反应时间和物质的量比对所得产率的影响,得到最佳反应条件:加入催化剂硫酸二甲酯后,在170℃的条件下保温反应18h,4-乙基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷和甲基苯基二甲氧基硅烷的物质的量比为1∶1.2,目标产物得率89.3%。通过FT IR、1 H NMR、热重-差热分析(TG-DTA)对产物MSAMP的结构进行了表征分析,利用极限氧指数法将产物应用于191不饱和树脂和尼龙6(PA6)中测试阻燃性能。结果表明,产物MSAMP具有良好的阻燃功效。

A flame retardant of methylphenyl silicic acid monocyclic phosphonates was synthesized through the reaction between dime thoxymethylphenylsilane and 4-ethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane(cage phosphite).The effects of reaction temperature,reaction time and amount of substance on the yield were discussed.The optimal conditions were selected as follows:after adding dimethyl sulfate as catalyst,the reaction was carried out at 170℃for 18 h,the molar ratio of cage phosphate and methylphenyldimethoxysilane was 1∶1.2,the yield was 89.3%.The product was characterized by FT IR,1 H NMR and Thermogravimetry-differential thermal analysis(TG-DTA).Extreme oxygen exponential method was employed to test the flame retardant properties in 191unsaturated resins and Nylon 6(PA6).The results show that the product exhibits good flame retardant ability.