非卤反应性阻燃剂N,N-二(2-羟乙基)氨甲基膦酸二乙酯的微波合成及结构表征  

The Microwave Synthesis and Structure Characterization of Halogen-Free Reactive Flame Retardant N,N-bis(2-Hydroxyethyl) Ammonium Dimethyl Ethyl Ester

作　　者：张猛[1,2] 周永红[1,2] 谢友利[1] 胡立红[1] 

机构地区：[1]中国林业科学研究院林产化学工业研究所,南京210042 [2]江苏强林生物能源材料有限公司,溧阳213364

出　　处：《聚氨酯工业》2011年第5期9-11,15,共4页Polyurethane Industry

基　　金：国家林业局"948"项目(2009-4-55);国家重大产业技术开发专项项目(发改高技[2008]2441号)

摘　　要：以甲醛、二乙醇胺、亚磷酸二乙酯为原料,采用常规和微波两种方法通过Mannich反应合成目标化合物N,N-二(2-羟乙基)氨甲基膦酸二乙酯(简称BHAPE),分别考察了反应时间、微波功率、微波反应温度对其产率的影响,结果表明,反应温度50℃、反应时间20 min、微波功率600 W时,微波反应产率达到98.9%;最后通过GC、FT-IR、MS、H-NMR对产物含量和结构进行了分析。N, N-bis （2-hydroxyethyl） ammonium dimethyl ethyl ester （BHAPE） was prepared from the formaldehyde, diethanolamine and diethyl phosphate by Mannich reaction. Two methods of conventional and microwave synthesis of the target compounds BHAPE were adopted. The influences of reaction time, microwave power, reaction temperature on BHAPE yield were investigated. The results showed that when the temperature was 50℃, reaction time was 20 min, microwave power was 600 W, the yield of microwave reaction was as high as 98.9%. Finally the content and structure of the product were analyzed by GC, FT-IR, MS, 1H-NMR.

关 键 词：微波 Mannich反应 N N-二(2-羟乙基)氨甲基膦酸二乙酯 表征 

分 类 号：TQ314.248[化学工程—高聚物工业]