笼状有机硅季鏻盐阻燃抗静电剂的合成

Synthesis Study on Cage-shaped Organosilyl Quaternary Phosphonium as Antistatic Flame Retardant

以甲基三氯硅烷和四羟甲基硫酸鏻为原料合成了笼状有机硅季鏻盐阻燃抗静电剂1-甲基-4-羟甲基-1-硅杂-4-磷杂-2,6,7-三氧杂双环[2,2,2]-辛烷季鏻硫酸盐。考察了反应温度、反应时间、溶剂对产率的影响,最佳工艺条件为:甲基三氯硅烷与四羟甲基硫酸鏻的摩尔比为2∶1,以二乙二醇二甲醚作溶剂,反应温度为120℃,反应时间为8 h。采用FTIR、1HNMR对产物结构进行了表征,测试了产品的阻燃和抗静电性能。结果表明,该化合物在失重20%时的分解温度为478.5℃,有优良的阻燃抗静电性能。

1-Methyl-4-hydroxymethyl-l-silicone miscellaneous-4-phosphorus miscellaneous-2, 6, 7- trioxabicyclo [ 2, 2, 2 ]-octane quaternary phosphonium sulfate, a kind of cage-shaped organosilyl quaternary phosphonium as flame retardant antistatic agent, was synthesized by methyl trichlorosilane reacting with tetrakis hydroxymetyl phosphonium sulfuric. The impact of reaction temperature, reaction time and resolvent on the yield was discussed, and a new production route was designed, that is, the molar ratio of methyl triehlorosilane to tetrakis hydroxymetyl phosphonium sulfuric was 2：1 ,the reaction time was 8 h at 120 ℃, and diethylene glycol dimcthyl ether was used as solvent. The synthesized compound has been ascertained by FTIR,and 1HNMR,and its flame retardant and antistatic properties were tested. Further research of the product shows that the decomposition temperature of the compounds in weightlessness of 20% is 478.5 ℃, indicating its excellent flame retardant antistatic performance in the application tests.