N,N-二(2-羟乙基)氨甲基膦酸二乙酯的合成

改进了非卤反应型阻燃剂N,N-二(2-羟基乙基)氨甲基膦酸二乙酯(BHAPE)的合成方法.在35℃左右将二乙醇胺滴入37%~40%的甲醛水溶液中,加毕,于40~45℃继续保温反应2 h,然后于80~82℃,小于0.094 MPa,减压蒸馏直到没有馏分为止,得到中间体3-(2-羟基乙基)-1,3-氧氮杂环戊烷(HENH).向HENH中加入阳离子交换树脂催化剂,于55~62℃滴入亚磷酸二乙酯,加毕,于60~62℃保温反应2 h,降到室温,过滤回收催化剂,得黄色透明液体产品,收率98.5%.用元素分析、红外光谱和核磁共振谱表征了中间体和标题化合物.

Synthesis of N, N-Bis(2-hydroxyethyl) aminomethyl Phosphonic Acid Diethyl Ester

The synthetic method for N,N-bis(2-hydroxyethyl)aminomethyl phosphonic acid diethyl ester(BHAPE),a halogen-free reactive flame retardant,was improved.Diethanolamine was added to formalin at 35 ℃,and the mixture was warmed to 40~45 ℃ for 2 h.Whereafter,the water in the mixture was evaporated with vacuum distillation at 80~82 ℃ under 0.094MPa to obtain intermediate,3-(2-hydroxyethyl)-1,3-oxazole(HENH).Both of cation exchange resin catalyst and diethyl phosphite were added to HENH at 55~62 ℃ successively,then the reaction continued at 60～62 ℃ for 2 h.Finally,the mixture was cooled to room temperature,the catalyst was recovered by filtration and BHAPE was obtained as yellow white liquid in yield of 98.5 %.The structures of HENH and BHAPE were identified by elemental analysis,FTIR and ~(1)H NMR.