硫酸酯型氟表面活性剂的合成与表面活性

以4-全氟壬烯氧基苯磺酰氯和2-甲氨基乙醇为主要原料，经酰胺化、酯化和中和反应制备了硫酸2-（N-甲基-4-全氟壬烯氧基苯磺酰胺基）乙酯钠（I），用红外光谱和19F NMR，1H NMR对中间体和产物分子结构进行了表征，借助正交试验法优化了反应条件。酰胺化反应较佳工艺条件：n（4-全氟壬烯氧基苯磺酰氯）: n（2-甲氨基乙醇）＝1.0 : 2.0，以三乙胺为缚酸剂，在THF溶剂中，室温下搅拌反应3.0 h，收率93.4 ％；酯化反应较佳工艺条件：n（ N-羟乙基-N-甲基-4-全氟壬烯氧基苯磺酰胺）: n（氯磺酸）＝1.0 : 2.0，在THF溶剂中，室温下反应0.5 h，收率97.1 ％。硫酸2-（N-甲基-4-全氟壬烯氧基苯磺酰胺基）乙酯钠表面活性剂的临界胶束浓度 8.0×10-4mol/L，γcmc 23.1 mN/m (25℃)。

Synthesis and Surface Activity of Fluorocarbon Surfactant Containing Sulfuric ester

Sodium 2- (N-methyl- 4-perfluorous nonenyloxyphenylsulfonamido) ethyl sulfate （I）was synthesized from 4-perfluorononenyloxy benzenesulfonyl chloride, 2-(methylamino)ethanol and chlorsulfonic acid via amidation and esterification, the intermedium and product were characterized by IR, 19F NMR and 1H NMR respectively. The reaction conditions were optimized by means of orthogonal experiments. For the amidation, the optimal reaction conditions were that: n(4-perfluorononenyloxy benzenesulfonyl chloride) : n(2-methylamino ethanol) = 1.0 : 2.0, triethylamide as acid acceptor, in THF at 30℃ for 3.0 h giving N-hydroxyethyl- N-methyl-4- perfluorous nonenyloxybenzenesulfonated amide(II) in the yield of 93.4%; The optimal reaction conditions of esterification were that: n(II) : n(chlorsulfonic acid) = 1.0 : 2.0 in THF at room temperature for 0.5 h giving I in the yield of 97.1%. The critical micelle concentration(CMC) of I was 8.0×10－4mol/L, and its surface tension(γcmc) is 23.1mN/m (25℃).