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以苯基三甲氧基硅烷(PhTMO)和1-硫基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(SPEPA)为原料,合成了Si、P、S三元素协同硫代磷酸酯阻燃剂苯基甲氧基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(PSMDSPE)。探讨了溶剂、反应温度、反应时间及物质的量比等对产率的影响。其最佳反应条件:PhTMO和SPEPA物质的量比为1∶2.2,升温至150℃,分馏反应8h,产率为92.7%。通过FT-IR、1 H-NMR、热重分析及极限氧指数测试等对产物的结构及性能进行了表征。测试结果表明:该化合物热稳定性好,应用于聚对苯二甲酸丁二醇酯(PBT)中有良好的阻燃及成炭防滴落效果,并且其与三聚氰胺聚磷酸盐(MPP)复配用于PBT阻燃时表现有协同增效性。
Using phenyltrimethoxysilane (PhTMO) and 1-thiophenyl-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane (SPEPA) as raw materials, Si , P, S Three-element synergistic phosphorothioate flame retardant Phenylmethoxysilicic acid bis-1-thiophosphoric-2,6,7-trioxabicyclo [2.2.2] octyl-4- Methyl ester (PSMDSPE). The effects of solvent, reaction temperature, reaction time and mass ratio on the yield were discussed. The optimal reaction conditions were as follows: the molar ratio of PhTMO to SPEPA was 1: 2.2, the temperature was raised to 150 ℃, and the fractional distillation was carried out for 8h, the yield was 92.7%. The structure and properties of the product were characterized by FT-IR, 1 H-NMR, TG-IR and Oxygen Index. The results show that the compound has good thermal stability, good flame retardancy and charcoal anti-drip effect when used in polybutylene terephthalate (PBT), and has good compatibility with melamine polyphosphate (MPP) complex Equipped with PBT flame retardant synergistic performance.