笼状含硅季鏻阻燃抗静电剂的合成研究

以甲基三甲氧基硅烷和四羟甲基硫酸鏻为原料合成了笼状含硅季鏻阻燃抗静电剂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。讨论了温度、时间、溶剂等对产率的影响。其最佳工艺条件为:甲基三甲氧基硅烷与四羟甲基硫酸鏻的摩尔比为2∶1,以二甲苯作溶剂,反应温度为140℃,反应时间为8h。并用红外图谱、核磁图谱及差热图谱表征了产品的结构及性能,还对产品作了应用研究。实验表明该化合物分解温度为478.5℃,有优良的阻燃抗静电性能。

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

1-Methyl-4-hydroxymethyl-1-silicone miscellaneous-4-phosphorus miscellaneous-2,6,7-trioxabicyclo-octane quaternary phosphonium sulfate,a kind of cage-shaped silicic quaternary phosphonium as flame retardant antistatic agent,was synthesised by reacting methyltrimethoxy silane with tetrakis hydroxymethyl phosphonium sulfate.Effects of the process conditions of reaction were investigated and the optimum parameters were obtained.When the molar ratio of methyltrimethoxy silane and tetrakis hydroxymetyl phosphonium sulfuric was 2∶1,the reaction time was 8 h at temperature of 140℃,and xylene was used as solvent.FT IR、1H NMR and DTA were used to characterize the structure and performance of the final product.Further research of the product showed that the decomposition temperature was 478.5 ℃,and the flame retardant antistatic performance in the application tests was excellent.