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

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%。

Synthesis of novel mono-component P-Br synergistic flame retardant 1,3-bis(5,5-dibromomethyl-1,3-dioxaphosphorinanyl-2-oxy)benzene

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 ℃.