新型无卤阻燃剂双酚S-二(5,5-二甲基-1,3-二氧杂己内磷酸酯)的合成

Synthesis of Novel Halogen-free Flame Retardant Bisphenol S-bis(5,5-dimethyl-1,3-dioxaphosphorinanyl-2-oxy)

以新戊二醇、三氯氧磷为原料,三乙胺为催化剂,合成了5,5-二甲基-1,3-二氧杂己内磷酰氯,再与双酚S反应得到高产率的新型无卤阻燃剂双酚S-二(5,5-二甲基-1,3-二氧杂己内磷酸酯),目标产物结构经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288.0℃,600℃时炭残余量达37.7%.

The neopentyl glycol chlorophosphate（2） was prepared by reaction of neopentyl glycol and phospous oxychloride in the presence of triethylamine.Then bisphenol S-bis（5,5-dimethyl-1,3-dioxaphosphorinanyl-2-oxy）（3） was synthesized by compound 2 and bisphenol S in high yields.The structure of the novel flame retardant was confirmed by IR,MS and 1 HNMR spectroscopy.The termogravimetry showed that the novel flame retardant had high thermal stability and excellent char-forming ability.The beginning temperature of the compound 3 decomposition was above 288.0 ℃,and the char yield was about 37.7 % at 600 ℃.