一种新型膨胀型阻燃剂的合成

Synthesis of a New Intumescent Flame Retardant

以季戊四醇、三氯氧磷、三聚氰胺为原料经3步合成了膨胀型阻燃剂双(1-氧代-4-亚甲基-1-磷杂-2,6,7-三氧杂双环[2,2,2]辛烷)磷酸酯三聚氰胺盐(Melabis).重点对第一步反应的条件进行了探索.通过对比实验确定了第一步反应的溶剂为1,4-二氧六环,缚酸剂为三乙胺,三氯氧磷与季戊四醇物质的量之比为1.04:1,反应时间为5h,反应温度为95℃.在此条件下产率可达84.0%.同时采用元素分析、IR等分析方法证实了产品的结构.

Bis （ 2,6,7-trioxa-1 -phoshabicyclo [ 2,2,2 ] -octane-4-methanol ） phosphate （ Melabis ） was synthesized from pentaerythritol, phosphorous oxychloride and melamine after the three-step. We mainly focus on the reaction conditions of step 1. It is determined by contrastive experiment that triethylamine and 1,4-Dioxane are used as HC1 acceptot and the solvent of the first step. With an experiment method, the suitable synthesis condition are defined as follows： the molar ratio of phosphorous oxychloride and the entaerythritol is 1.04： 1, reaction time 5h,reaction temperature 95℃. Under the above conditions,synthetic productivity can reach 84. 0%. The structure of the product was defined by elemental analysis and IR.