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以四氯化硅(STC)与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,合成了氯化硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(SDSPEC),而后经水解得到二羟基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(SDSPE)。探讨了反应温度、反应时间及物料比对产率的影响,得到的最优工艺条件为:二氧六环作溶剂,n(STC)∶n(SPEPA)=1.0∶2.1,在30℃下反应6 h,水解反应条件为:n(SDSPEC)∶n(H_2O)=1.0∶2.0,60℃下反应4 h,得到SDSPE,产率为93.9%。通过FTIR、~1HNMR、热重分析及极限氧指数测试对产物的结构及性能进行了表征。结果表明,产物有很好的热稳定性,分解温度达270℃;当SDSPE加入量达到191不饱和树脂质量的20%时,191不饱和树脂的LOI值为28%,且残炭量高达38.6%,表明应用于191不饱和树脂时,表现出了较好的阻燃成炭效果。
Silicon tetrachloride (STC) and 1-thiophenyl-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane (SPEPA) Thiadiazaphosphoric-2,6,7-trioxabicyclo [2.2.2] octyl-4-methyl ester (SDSPEC), which is then hydrolyzed to give bis-1-thio Phospha-2,6,7-trioxabicyclo [2.2.2] octyl-4-methyl ester (SDSPE). The effects of reaction temperature, reaction time and material ratio on the yield were investigated. The optimum conditions were: dioxane as solvent, n (STC): n (SPEPA) = 1.0: 2.1, reaction at 30 ℃ The reaction conditions were as follows: n (SDSPEC): n (H_2O) = 1.0: 2.0 and reacted at 60 ℃ for 4 h. The yield of SDSPE was 93.9%. The structure and properties of the product were characterized by FTIR, ~ 1HNMR, TG and LOI. The results showed that the product had good thermal stability and the decomposition temperature was 270 ℃. When the amount of SDSPE reached 20% of 191 unsaturated resin, the LOU of 191 unsaturated resin was 28% and the residual carbon content was as high as 38.6 %, Indicating that when applied to 191 unsaturated resin, showed a good flame retardant charcoal effect.