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%.
作者
付渊
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)
出处
《广州化工》
CAS
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)。
