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%.
出处
《化学试剂》
CAS
CSCD
北大核心
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)
关键词
环状磷酸酯
合成
阻燃剂
炭残余物
cyclic phosphoric ester
synthesis
flame retardant
char residue