新型单组分磷溴协效阻燃剂1,3-二(5,5-二溴甲基-1,3-二氧杂己内磷酰氧基)苯的合成

Synthesis of novel mono-component P-Br synergistic flame retardant 1,3-bis(5,5-dibromomethyl-1,3-dioxaphosphorinanyl-2-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,再与间苯二酚反应得到标题化合物,两步反应总产率76.9%。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301.0℃,500℃时炭残余量达32.52%。

5,5-Dibromomethyl-1,3-dioxaphosphoryl chloride was prepared by using dibromoneopentyl glycol and phospous oxychloride as raw materials and triethylamine as catalyst.Then 1,3-bis（5,5-dibromomethyl-1,3-dioxaphosphorinanyl-2-oxy）benzene was synthesized.The overall yield of two steps was 76.9%,and the structure of the above novel flame retardant was confirmed by means of elementary analysis,IR,MS and 1HNMR spectra.The thermogravimeter analysis results showed that the novel flame retardant has high thermal stability and excellent char-forming property.The beginning decomposition temperature of title compound was above 301.0 ℃,and the char yield was about 32.52% at 500 ℃.