均匀设计法在三邻苯二胺基环三磷腈合成中的应用  

Application of Uniform Design in Synthesis of Tri (o-phenylenediamine)-cyclotriphosphazene

作　　者：许肖丽[1] 郝冬梅[1] 陈涛[1] 林倬仕[1] 尹亮[1] 陈崇伟[1] 吴向阳[1] 徐静安[1] 

机构地区：[1]上海化工研究院,上海200062

出　　处：《化学世界》2013年第7期415-418,434,共5页Chemical World

基　　金：上海市科委基金项目(11nm0501800)

摘　　要：以六氯环三磷腈和邻苯二胺为原料,甲苯为溶剂,滴加缚酸剂三乙胺的方法,发生亲核取代,合成出三邻苯二胺基环三磷腈(HACTP),利用HPLC、FT IR、MS、31P NMR和1 H NMR表征产物并确定其结构。采用均匀设计法考察了合成中反应时间、原料配比和缚酸剂用量三个因素对产物收率的影响,利用DPS数据回归处理方法建立数学模型,确定出实验范围内的最佳合成条件:反应时间14.5h,原料配比n(邻苯二胺)∶n(六氯环三磷腈)=4.5∶1,缚酸剂用量n(三乙胺)∶n(六氯环三磷腈)=6.5∶1时,产物收率达92.547%。The tri（ophenylenediamine） cyclotriphosphazene （HACTP） was synthesized by onestep nucle ophilic substitution with hexachlorocyclotriphosphazene and ophenylenediamine as raw material, triethyl amine solution as catalyst and methylbenzene as solvent. The structure of the product was characterized by HPLC.FT IR.MS.31P NMR and 1H NMR. The influences of reaction time, ratio of reactant and amount of catalyst on yield of the synthetic reaction were studied by the uniform design method. Regression analy sis was used to establish a mathematics model by DPS and the optimum conditions were. reaction time of 14.5 h at reflux temperature, molar ratio of ophenyienediamine to hexachlorocyclotriphosphazene 4.5 ： 1, and the molar ratio of triethylamine to hexachlorocyclotriphosphazene 6.5 ＂ 1. The yield of synthetic reac tion may go beyond 92. 547% under the optimum conditions.

关 键 词：六氯环三磷腈 邻苯二胺 均匀设计法 DPS 

分 类 号：O627.51[理学—有机化学]