新型树状磷-溴协效阻燃剂1,3,5-三(5,5-二溴甲基-1,3-二氧杂己内磷酰氧基)苯的合成及其应用研究  

Synthesis and application of novel P-Br synergistic arborescent flame retardant 1,3,5-tri(5,5-dibromomethyl-1,3-dioxaphosphorinanyl2-oxy)benzene

作　　者：卢林刚[1] 周霞[2] 赵敏[3] 于宝刚[1] 王会娅[4] 

机构地区：[1]中国人民武装警察部队学院科学技术研究所,河北廊坊065000 [2]中国人民武装警察部队学院研究生队,河北廊坊065000 [3]中国人民武装警察部队学院工程系,河北廊坊065000 [4]中国人民武装警察部队学院基础部,河北廊坊065000

出　　处：《化学试剂》2008年第10期721-724,共4页Chemical Reagents

基　　金："十一五"国家科技支撑计划项目(2006BAK06B06)

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,再与间苯三酚反应得到新型树状阻燃剂标题化合物,两步反应总产率74.1%。目标产物结构经元素分析I、R、MS及1HNMR证实。热失重分析表明目标产物具有较高热稳定性和良好成炭性,起始分解温度为324.0℃,600℃时炭残余量达38.88%。目标产物对环氧树脂有较好的阻燃效果,最佳添加量为20%。Dibromoneopentyl glycol chlorophosphate was prepared by reaction of dibromoneopentyl glycol and phosphorus oxychloride in the presence of triethylamine.Then 1,3,5-tri（5,5-dibromomethyl-1,3-dioxaphosphorinanyl-2-oxy）benzene was synthesized by reaction of the above-mentioned compound with 1,3,5-tri（hydroxy）benzene.The overall yield was 74.1%.The structure of the novel flame retardant was confirmed by elementary analysis,IR,MS and ^1HNMR spectroscopy.Thermogravimetric analysis showed that the novel flame retardant had high thermal stability and excellent char-forming ability.The initial temperature leading to decomposition of the compound was above 324.0 ℃,and the char yield was about 38.88% at 600 ℃.The results demonstrated that this compound was effective on the flame retardancy of epoxy resin,and the optimum addition dosage was 20%.

关 键 词：环状磷酸酯 合成 阻燃剂 炭残余物 

分 类 号：TQ314.24[化学工程—高聚物工业]