31PNMR在阻燃剂DOPO合成中的应用  

Application of ^(31)P NMR in the Synthesis of Flame Retardant DOPO

作　　者：赖华[1] 李想[1] 刘兴[1] 朱小明[1] 谭雄文[1] 熊平生[2] 

机构地区：[1]衡阳师范学院化学与材料科学学院,功能金属有机材料湖南省普通高等学校重点实验室,湖南衡阳421008 [2]衡阳师范学院城市与旅游学院,湖南衡阳421008

出　　处：《波谱学杂志》2017年第1期61-68,共8页Chinese Journal of Magnetic Resonance

基　　金：国家自然科学基金资助项目(41471153);衡阳师范学院科学基金资助项目(13B30);衡阳市科学技术发展计划资助项目(2014KJ19)

摘　　要：9,10-二氢-9氧杂-10-膦杂菲-10-氧化物(DOPO)的合成涉及酯化、酰基化、水解和脱水环化反应.通过核磁共振磷谱(^(31)P NMR)对各步反应得到的产物进行表征,分析各反应产物的组成,由此得出各步反应规律,并找出了影响DOPO的产率和纯度的一些关键因素.The synthesis of flame retardant 9,10-dihydro-9-oxa-10-phosphaphen-anthrene-10-oxide (DOPO) involves many steps of chemical reactions, including esterification, Friedel-Crafts acylation, hydrolysis and dehydration. We analyzed the composition of the products from each of the steps with 31P NMR. The results were used to deduce the reaction routes and to optimize the reaction conditions. Based on the results, some key factors that may influence the yield and purity of DOPO were determined.

关 键 词：核磁共振磷谱(31PNMR) 阻燃剂 9 10-二氢-9-氧杂-10-膦杂菲-10-氧化物(DOPO) 

分 类 号：O482.53[理学—固体物理]