含硫笼状磷酸酯阻燃剂的合成与应用

Synthesis and application of synergistic phosphorus and sulfur flame retardant

以三羟甲基硫化膦与三氯硫磷作为原料,合成一种阻燃剂含硫笼状磷酸酯,即1,4-二硫代-2,6,7-三氧杂-1,4-二磷杂双环[2. 2. 2]辛烷(DSDPCP)。研究得出最佳制备工艺条件为:三羟甲基氧化膦与三氯硫磷的摩尔比1:1,氮气氛围下,控制在65℃、105℃、140℃三个阶梯温度下分别反应3h、3h、8h,排去氯化氢后调节PH,除去溶剂和缚酸剂,氯仿洗涤后下层粘性液体用0℃冰水快速洗涤、过滤既得产物,最终产物收率为94. 2%。利用FTIR、1H-NMR、热重分析及极限氧指数等技术手段对该产物的结构以及性能进行表征。产物的阻燃性能测试结果表明,产物单独应用于PBT中还是与MPP复配后应用于PBT中都有很好的阻燃效用。

A type of flame retardant sulphur containing cage like phosphate was synthesized with three hydroxymethyl phosphine sulphide and three chlorosulphite,that is,1,4-two thiosulphic-2,6,7-three-1,4-two phospho heterocyclic[2. 2. 2]octane( DSDPCP). The optimum preparation conditions are as follows: the mole ratio of three hydroxymethyl phosphine oxide and three chloroform 1:1,under nitrogen atmosphere,control 3 h,3 H and 8 h at 65℃,105℃,140℃,respectively,after removing hydrogen chloride to adjust PH,remove the solvent and bind acid agent,and the lower viscosity liquid of the lower layer after chloroform washing is fast at 0 ℃ice water.The product was obtained by washing and filtering quickly,and the yield of the final product was 94. 2%. The structure and properties of the product were characterized by FTIR,1 H-NMR,thermogravimetric analysis and limiting oxygen index.The test results of the flame retardancy of the products showed that the products can be applied to PBT alone or combined with MPP,which has good flame retardancy in the application of PBT.