新型磷系阻燃剂1，2，3-三(5，5-二甲基-1，3-二氧杂环己内磷酸基)苯的合成研究  

Synthesis of novel flame retardant from 1,2,3-tri(5,5-dimethyl-1,3-dioxacyclophosphorinane phosphonate) benzene

作　　者：卢林刚[1] 王大为[2] 王会娅[3] 于宝刚[1] 王学宝[4] 杨守生[4] 唐凯[1] 王永明[3] 

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研究生队,河北廊坊065000 [3]中国人民武装警察部队学院基础部,河北廊坊065000 [4]中国人民武装警察部队学院消防工程系,河北廊坊065000

出　　处：《化学试剂》2008年第3期171-174,共4页Chemical Reagents

基　　金：“十一五”国家科技支撑计划项目(2006BAK06B06)

摘　　要：以1,2,3-三羟基苯、新戊二醇、三氯氧磷等为主要原料,三乙胺为缚酸剂,采用简洁、高效的合成路线制备出标题化合物。制取目标化合物的最佳反应条件:n(1,2,3-三羟基苯)∶n(新戊二醇磷酰氯)∶n(三乙胺)=1∶4·5∶5·0,反应温度50℃,反应时间6h,产率75%。通过红外光谱、核磁共振氢谱、质谱及元素分析等表征了目标化合物结构。热失重分析表明,该阻燃剂具有较高的热稳定性和良好的成炭性,起始分解温度为287·47℃,500℃时炭残余量高达44·21%。The novel flame retardant was synthesized via the reaction of 1,2,3-tri （hydroxy） benzene, neopentyl glycol, and phosphorus oxychloride in the presence of triethylamine as acid-binding agent. This method was facile, highly efficient and useful. At the same time, the effects of feedstock mole ratio, reaction temperature and reaction time were studied. The optimum ratios of reactants studied by experiments were n （ tri （ hydroxy ） benzene） ： n （ neopentyl glycol phosphoryl chloride ） ： n （ triethylamine ） = l：4.5：5.0.The optimized reaction was conducted at 50 ℃for 6 h at the final phase of reaction. The structure of the novel flame retardant was identified and studied by Fr-IR, 1HNMR, ESI-MS and elementary analysis, respectively. The termogravimetry showed that the novel flame retardant had high thermal stability and excellent char-forming ability. The starting temperature for decomposition of the said compound was above 287.47 ℃, and the char yield was about 44.21% at 500℃.

关 键 词：阻燃剂 1 3-二氧杂环己内磷酸酯 合成 炭残留物 

分 类 号：TQ314.248[化学工程—高聚物工业]