含氯溴硅酸酯阻燃剂的合成及表征

Synthesis and Characterization of Chlorine-Bromine Silicate Ester Flame Retardants

以三溴苯酚、四氯化硅及环氧乙烷为主要原料,通过三溴苯基环氧丙基醚与四氯化硅反应生成中间产物三溴苯氧基氯丙氧基三氯化硅,再与环氧乙烷反应,合成硅、氯、溴三元素协同高效阻燃剂三溴苯氧基氯丙氧基硅酸三(氯乙基)酯。探讨了反应温度、时间、原料摩尔比对产率的影响,得到反应的最佳合成工艺条件:n(三溴苯基环氧丙基醚)∶n(四氯化硅)∶n(环氧乙烷)=1∶1∶3.2,50℃反应4 h,产率达98.6%。采用FTIR、1HNMR表征了产物的分子结构。应用研究表明,在聚氯乙烯中加入质量分数10%该阻燃剂时,其极限氧指数为28%。

With tribromophenol, silicon tetrachloride and ethylene oxide as the main raw materials, the efficient flame retardants tribromophenoxy chloropropoxy silicate tris （chloroethyl） ester with the three elements of silicon, chlorine and bromine was synthesized. The effect of reaction temperature, time and amount ratio of substance on the reaction yield was discussed. The optimal conditions for the preparation were determined as follows ： n （ tribromophenyl epoxy propyl ether） ： n （ silicon tetrachloride ） ：n （ ethylene oxide） was 1 ： 1：3.2, and the reaction time was 4 h at 50℃. The percentage of the reaction yield could reach 98.6%. The molecular structures of the product and its flame retardant properties were characterized by means of FTIR, 1HNMR and LOI technique. Applied research shows that the limiting oxygen index of the flame retardants was up to 28% when 10% tribromophenoxy chloropropoxy silicate tris（chloroethyl） ester was added into PVC.