螺环季戊四醇磷酸酯阻燃剂的合成与表征  

Synthesis and Characterization of Spiropentaerythritol Phosphate Flame Retardant

作　　者：付渊[1] 陈家兴 刘呼努斯吐 吴天赐 FU Yuan;CHEN Jia-xing;LIU Hunusitu;WU Tian-ci(Inner Mongolia Vocational College of Chemical Engineering,Inner Mongolia Hohhot 010070,China)

机构地区：[1]内蒙古化工职业学院,内蒙古呼和浩特010070

出　　处：《广州化工》2021年第9期46-47,87,共3页GuangZhou Chemical Industry

基　　金：2019年内蒙古自治区科学研究“十三五”规划课题(项目编号:NZJGH2019203)。

摘　　要：螺环季戊四醇磷酸酯磷含量高、热稳定性好,且由于其分子中含有羟基,可作为反应型阻燃剂来使用。本文采用三氯化磷和季戊四醇反应制得螺环季戊四醇磷酸酯。通过实验得到适宜的合成条件:以氯苯为溶剂,制得中间体二磷杂螺环十一烷。中间体制备时三氯化磷和季戊四醇的摩尔比为3:1,反应先进行至60℃时,保温1 h,反应平稳后继续升温至80℃。中间体与适当过量的苯乙酮反应后,在62~67℃下滴加甲酸到反应体系中,产率达80%。Spropentarythritolphosphate has high phosphorus content,good thermal stability and can be used as a reactive flame retardant because of its hydroxyl group.Spiropentaerythritol phosphate was prepared by the reaction of Phosphorus trichloride and Pentaerythritol.The suitable synthetic conditions were obtained by experiments.The intermediate diphosphono-spirodecane was prepared by using chlorobenzene as the solvent.The molar ratio of phosphorus trichloride to Pentaerythritol was 3:1.The reaction was kept at 60℃for 1 hand then kept at 80℃after the reaction was stable.After the intermediate reacted with Acetophenone,formic acid was added into the reaction system at 62~67℃,the yieldreached 80%.

关 键 词：螺环季戊四醇磷酸酯 合成 红外光谱 

分 类 号：O657.33[理学—分析化学]