摘要
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′-perfluorohexylsulfonamido）propyl]-N,N,N-trimethyl ammonium iodide（Ⅰ） was prepared first by amidation from perfluorohexylsulphonyl fluoride（Ⅱ） and N,N-dimethyl-1,3-propane diamine（Ⅲ）,then by quaternization with methyl iodide（Ⅳ）,and the final product was characterized by means of IR,1HNMR,and MS.The surface tension（γ） and critical micelle concentration（CMC） of the aqueous solutions of Ⅰ were investigated.The optimal process conditions of amidation were：n（Ⅱ）∶n（Ⅲ）=1∶1.2,the reactants being agitated at room temperature for 3 h in EtOAc in the presence of N（Et）3 to give C6F13SO2NHC3H6N（CH3）2（Ⅴ） in the yield of 90.9%.The optimal process conditions of quaternization were：n（Ⅴ）∶n（Ⅳ）=1∶1.7,Ⅴ and Ⅳ reacting at room temperature for 2 h in CCl4 to give Ⅰ in the yield of 97.6 %.The CMC of the aqueous solution of Ⅰ is 3.50 mmol/L and its γCMC is 17.8 mN/m,showing excellent performance of surface activity of Ⅰ.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2012年第5期438-442,共5页
Fine Chemicals
基金
浙江省科技厅创新团队资助项目(2011R09002-10)~~
关键词
氟碳表面活性剂
全氟己基磺酰氟
表面张力
临界胶束浓度
fluorocarbon surfactant
perfluorohexylsulphonyl fluoride
surface tension
critical micelle concentration
