新型阻燃剂1 ,3 ,5-三(5 ,5-二甲基-1 ,3-二氧杂己内磷酸酯基)苯的合成及表征  

Synthesis and Characterization of Novel Flame Retardant 1,3,5-Tri(5,5-dimethyl-1,3-dioxacyclophosphorinane phosphonate)benzene

作　　者：卢林刚[1] 王会娅[2] 王大为[3] 于宝刚[1] 王永明[2] 唐凯[1] 

机构地区：[1]中国人民武装警察部队学院科学技术研究所,河北廊坊065000 [2]中国人民武装警察部队学院基础部,河北廊坊065000 [3]中国人民武装警察部队学院研究生队,河北廊坊065000

出　　处：《化学研究》2007年第4期16-19,共4页Chemical Research

基　　金："十一五"国家科技支撑计划项目(2006BAK06B06)

摘　　要：以1，3，5-三羟基苯、新戊二醇、三氯氧磷等为原料，采用简洁、高效的合成路线，通过两步反应合成了新型阻燃剂1，3，5-三（5，5-二甲基-1，3-二氧杂已内磷酸酯基）苯．通过红外光谱、核磁共振氢谱、质谱、元素分析以及热失重分析等对产物结构和热性能进行了表征和研究．热失重分析表明：该阻燃剂起始分解温度为295．26℃，在295．26℃～343．38℃和350．40℃～578．04℃温区迅速炭化；当阻燃剂被加热到681．03℃时，炭残余量高达43．33％．The novel flame retardant was synthesized using neopentylglycol, phoshorus oxychloride and 1, 3, 5-trihydroxy benzene by facile and high efficient method consisting of two reactions. The structure and thermal behaviors of the novel flame retardant were identified and studied by FT-IR, ^1H NMR, ESI-MS, elementary analysis and TGA respectively. The characters of TGA for the product were discussed. The thermogravimetry shows that the beginning temperature of decomposition of the compound is above 295.26 ℃ , and rapidly carbonized between 295.26℃ to 343.38 ℃ and 350.40℃ to 578.04℃ . The char yield is about 43.33 % at 681.03 ℃ .

关 键 词：阻燃剂 1 3-二氧磷杂环内磷酸酯 合成 炭残留物 

分 类 号：TQ314.24[化学工程—高聚物工业]