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以三羟乙基异氰尿酸酯、二甲基二氯硅烷和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,合成了阻燃剂异氰尿酸三[2-(二甲基硫代PEPA氧基硅氧基)乙基]酯,即异氰尿酸三{2-[二甲基(1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛烷基-<4>-甲氧基)硅氧基]乙基}酯(TPSEC)。探讨反应时间、温度及摩尔比等对产率的影响。最佳条件为n(三羟乙基异氰尿酸酯)∶n(二甲基二氯硅烷)∶n(SPEPA)=1∶3∶3.4,第一步在70℃下反应7 h,第二步在95℃下反应6 h,收率为92.4%。通过FTIR、~1H-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:该化合物具有很好的热稳定性,应用于聚丙烯中有良好的阻燃及成炭防滴落效果。
Trihydroxyethylisocyanurate, dimethyldichlorosilane and 1-thiophospho-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane (SPEPA ) As a raw material, a flame retardant isocyanurate tris [2- (dimethylthio PEPA oxysiloxy) ethyl] isocyanurate, namely tris {2- [dimethyl 2,6-trioxabicyclo [2.2.2] octanyl- <4> -methoxy) siloxy] ethyl} ester (TPSEC). Effects of reaction time, temperature and molar ratio on yield were discussed. The best condition is n (trihydroxyethylisocyanurate): n (dimethyldichlorosilane): n (SPEPA) = 1: 3: 3.4, the first step is reaction at 70 ℃ for 7 h, the Two steps at 95 ℃ for 6 h, the yield was 92.4%. The structure and properties of the product were characterized by FTIR, ~ 1H-NMR, TG-IR and Oxygen Index. The test results show that: the compound has good thermal stability, used in polypropylene flame retardant and charcoal anti-drip effect.