季戊四醇二磷酸酯蜜胺盐的合成新方法

采用非溶剂法经过二步反应合成了膨胀型阻燃剂季戊四醇二磷酸酯蜜胺盐 ( PDM) ,首先三氯氧磷和季戊四醇反应得到季戊四醇二磷酸酯二磷酰氯 ( PDD) ,然后 PDD再与水、蜜胺反应 ,制备得到 PDM。在第一步反应中 ,当 n(三氯氧磷 )∶n(季戊四醇 ) =6∶ 1 ,在 60°C反应 1 h,再回流 1 0h,PDD的收率为 82 .3%。在第二步反应中 ,当 n( PDD)∶n(蜜胺 ) =1 .1∶ 2 ,回流时间为 2 h时 ,PDM的收率为 79

A new Method of Preparing of Pentaerythritol Diphosphonate of Melamine

Pentaerythritol diphosphonate of melamine (PDM), a novel intumescent flame retardant, was synthesized from water, melamine and pentaerythritol diphosphonate dichloride (PDD) which was prepared from pentaerythritol and phosphorous oxychloride in the absence of organic solvent. In the first step, when n (phosphorous oxychloride)∶ n (pentaerythritol)=6∶1, reacting at 60 °C for 1 h and refluxing for 10 h the yield of PDD is 82.3%. In the second step, when n (PDD)∶ n (melamine)=1∶1.2 and refluxing for 2 h, the yield of PDM is 79%.