含全氟壬烯基磷酸酯型表面活性剂的合成  

Synthesis of a Phosphate Ester Surfactant Containing Perfluorononenyl

作　　者：齐海[1] 史鸿鑫[1] 项菊萍[1] 武宏科[1] 陈立军[1] 

机构地区：[1]浙江工业大学绿色化学合成技术国家重点实验室培育基地,浙江杭州310032

出　　处：《合成化学》2010年第B09期157-163,共7页Chinese Journal of Synthetic Chemistry

摘　　要：以N-羟乙基-p-全氟壬烯氧基苯甲酰胺(I)为原料与三氯氧磷(POCl3)反应制备p-全氟壬烯氧基苯甲酰胺基乙基磷酰氯,反应结束后在常温下进行水解生成p-全氟壬烯氧基苯甲酰胺基乙基磷酸单酯(Ⅱ)。采用红外光谱(FTIR)、1HNMR、质谱(MS-ESI)对其结构进行了表征。考察了酯化反应时间、酯化反应温度、原料配比和缚酸剂对产物收率的影响。通过单因素实验和正交试验对反应进行优化,确定了最佳合成工艺条件为:n(I):n(POCl3)=1:1.6,反应温度70℃,反应时间7h,三乙胺做为缚酸剂,在此条件下Ⅱ的收率为84.3%。p-perfluorononenoxybenzamidoethyl phosphate monoester（Ⅱ） was synthesized by esterification from N-hydroxyethyl-p-perfluorononenoxy benzamide（Ⅰ） and phosphorus oxychloride（POCl3） and then by hydrolysis at room temperature.II was characterized by IR,1H NMR and MS-ESI.The effects of esterificaion time,esterification temperature,the ratio of I to POCl3 as well as proton trapper were investigated.The reaction conditions were optimized by means of single factor experiments and orthogonal experiments： n（Ⅰ）： n（POCl3）= 1 ： 1.6,at 70℃ reacts for 7 h in the presence of Et3N to give Ⅱin the yield of 84.3%.

关 键 词：磷酸单酯 三氯氧磷 表面活性剂 全氟壬烯 

分 类 号：TQ423[化学工程]