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以全氟己基磺酰氟和N,N-二甲基-1,3-丙二胺为原料,经酰胺化和季铵化反应,制备了N,N,N-三甲基-N-(N’-全氟己基磺酰胺基)丙基碘化铵。用IR、1HNMR、MS(ESI)等方法对其结构进行了表征,并测试了其表面张力等性能。结果表明,N,N-二甲基-N’-全氟己基磺酰基丙二胺合成的较佳工艺条件为:以乙酸乙酯为溶剂,三乙胺为缚酸剂,n(C6F13SO2F)∶n〔H2NC3H6N(CH3)2〕=1∶1.2,室温反应3 h,收率为90.9%。季铵化反应的较优合成条件为:以四氯化碳为溶剂,n〔C6F13SO2NHC3H6N(CH3)2〕∶n(CH3I)=1∶1.7,室温反应2 h,收率为97.6%。所得季铵盐临界胶束浓度(CMC)为3.50 mmol/L,在CMC时表面张力为17.8 mN/m,具有良好的表面活性。
N, N, N-trimethyl-N- (N, N-dimethylformamide) was prepared by the amidation and quaternization of perfluorohexylsulfonyl fluoride and N, N’-perfluorohexylsulfonamido) propyl ammonium iodide. Its structure was characterized by IR, 1HNMR and MS (ESI), and its surface tension and other properties were tested. The results showed that the optimum conditions for the synthesis of N, N-dimethyl-N’-perfluorohexylsulfonylpropanediamine were as follows: ethyl acetate as solvent and triethylamine as acid-binding agent, n (C6F13SO2F) n [H2NC3H6N (CH3) 2] = 1: 1.2, at room temperature for 3 h, the yield was 90.9%. The optimal conditions for the quaternization reaction were as follows: carbon tetrachloride was used as the solvent, n [C6F13SO2NHC3H6N (CH3) 2]: n (CH3I) = 1: 1.7 and the reaction was carried out at room temperature for 2 h. The yield was 97.6%. The CMC of the obtained quaternary ammonium salt was 3.50 mmol / L, and the surface tension was 17.8 mN / m at CMC with good surface activity.