含全氟基团的丙烯酸酯单体的制备

全氟辛酸与亚硫酰氯 (SOCl2 )在 85℃进行酰基化反应 1h得全氟辛酰氯 (Ⅰ ) ,Ⅰ与乙醇胺在 30℃下反应 3h得到N 羟乙基全氟辛酰胺 (Ⅱ ) ,然后以二月桂酸二丁基锡为催化剂 ,N2 保护 ,Ⅱ先与 2 ,4 甲苯二异氰酸酯 (TDI)于 6 5～ 70℃反应 3h ,然后再与甲基丙烯酸 β 羟乙酯于75～ 80℃反应 4h ,得目标产品含全氟基团的丙烯酸酯单体 (Ⅲ )。三步总收率可达 6 0 %。探讨了影响反应的主要因素和最佳工艺条件 ,产品结构经红外光谱进行了分析确证

Preparation of Perfluoro Acrylate Monomer

Perfluorooctanoyl chloride(I) was prepared by reaction of perfluorooctanoic acid and SOCl 2 at 85 ℃ for 1 h,then Ⅰ was treated with ethanolamine at 30 ℃ for 3 h to give N hydroxyethyl perfluorooctanamide(Ⅱ).Under the catalysis of dibutyltin dilaurate and the protection of N 2,Ⅱ was firstly treated with 2,4 tolylene diisocyanate at 65-70 ℃ for 3 h,then the reation mixture was further treated with β hydroxyethyl methylacrylate at 75-80 ℃ for 4 h to give the title compound (Ⅲ).The total productivity reached 60%.The main influencing factors in each reaction above mentioned were studied and the structures of the products in each step were confirmed by IR spectrum.