含硫有机磷阻燃剂DMSSPE的合成与应用

Synthesis and Application of Organic Phosphorus Flame Retardant DMSSPE Containing Sulfur

用1-硫基磷杂-2,6,7-三氧杂-4-羟甲基-双环[2.2.2]辛烷（SPEPA）和二甲基二甲氧基硅烷（DMCS）合成了二甲基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯（DMSSPE）。探讨了溶剂、反应温度、反应时间及DMCS与SPEPA摩尔比等对产物产率的影响,并通过FTIR、-1H-NMR、TG/DTA分析与极限氧指数测试对产品结构及阻燃性能等进行了表征。结果表明：以二氧六环作溶剂,DMCS与SPEPA摩尔比为1：2.2,升温至95℃,分馏反应7 h,产物产率可达90.1%;DMSSPE的热稳定性较好,分解温度达270℃,用于聚对苯二甲酸丁二醇酯（PBT）中具有良好的阻燃性能及成炭防滴落效果;DMSSPE与三聚氰胺聚磷酸盐（MPP）复配用于PBT阻燃时具有协同增效作用。

Dimethyl silicate double-1-sulfonium phosphorus mixed-2,6,7-three oxygen mixed double loop[2.2.2] octyl-4-methyl ester（DMSSPE） was synthesized with SPEPA and dimethyl dimethoxy silane（DMCS）. The effects of solvents, reaction temperature, reaction time and molar ratio of DMCS to SPEPA on the yield of the product were discussed. The product structure and flame retardancy were characterized by FTIR, -1 H-NMR, TG/DTA analysis and limiting oxygen index test. The results show that： using dioxane as solvent, the mole ratio of DMCS to SPEPA is 1：2.2, the temperature rises to 95℃, the fractionation reaction is 7 h, and the product yield reaches 90.1%. DMSSPE has good thermal stability and decomposition temperature up to 270℃. DMSSPE and melamine polyphosphate（MPP） was used for flame retardant PBT has a synergistic effect.