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

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%.