1,2,3-三(5,5-二溴甲基-1,3-二氧杂己内磷酰氧基)苯的合成  

Synthesis of 1,2,3-Tri(5,5-dibromomethyl-1,3-dioxaphosphorinanyl-2-oxy)benzene

作　　者：卢林刚[1] 周霞[2] 董希琳[1] 赵敏[3] 

机构地区：[1]中国人民武装警察部队学院科学技术研究所,廊坊065000 [2]中国人民武装警察部队学院研究生队,廊坊065000 [3]中国人民武装警察部队学院消防工程系,廊坊065000

出　　处：《化学通报》2009年第2期180-183,共4页Chemistry

基　　金："十一五"国家科技支撑计划项目(2006BAK06B06)资助

摘　　要：以二溴新戊二醇与三氯氧磷为原料,三乙胺为催化剂,合成得到5,5-二溴甲基-1,3-二氧杂己内磷酰氯,再与邻苯三酚反应得到新型磷系阻燃剂1,2,3-三(5,5-二溴甲基-1,3-二氧杂己内磷酰氧基)苯,两步反应总产率71.3%。目标产物结构经元素分析、IR、MS、及1HNMR证实。热失重分析表明,目标产物具有较高的热稳定性和良好的成炭性,起始分解温度为295.25℃,500℃时炭残余量达27.75%。Dibromoneopentyl glycol chlorophosphate was prepared by reaction of dibromoneopentyl glycol and phospous oxychloride in the presence of triethylamine. Then tided compound was synthesized by as-prepared phosphate and 1, 2, 3- trihydroxybenzene. The over yield was 71.3% . The structure of product was confirmed by elementary analysis, IR, MS and ~H NMR. The termogravimetry showed that it had high thermal stability and excellent char-forming ability. The beginning temperature of the product decomposition was above 295.25 ℃, and the char yield was about 27.75% at 500 ℃.

关 键 词：环状磷酸酯 合成 阻燃剂 炭残留物 

分 类 号：TQ314.248[化学工程—高聚物工业]