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机构地区:[1]南京工业大学化学化工学院,江苏南京210009
出 处:《南京工业大学学报(自然科学版)》2007年第3期47-50,共4页Journal of Nanjing Tech University(Natural Science Edition)
基 金:江苏省自然科学基金资助项目(BK2005121)
摘 要:以溴代烷烃、N-甲基咪唑和六氟磷酸铵为原料,采用水浴微波法合成了3种疏水性咪唑类离子液体:[bmim]PF6、[hmim]PF6和[omim]PF6.结果表明,与传统方法相比,水浴微波法产率较高,且反应时间由传统的36 h缩短至50 min.通过正交试验对离子液体[bmim]PF6的水浴微波合成反应条件进行了优化,得到了适宜的合成条件:反应时间50 min,n(1-溴正丁烷)∶n(N-甲基咪唑)∶n(六氟磷酸铵)为1.1∶1.0∶1.0,微波功率385 W,产率可达到94.54%.结合反应机理对优化结果进行了分析,并通过红外光谱验证了3种疏水性离子液体的结构.Three hydrophobic imidazolium-based ionic liquids ( [ bmim ] PF6, [ hmim ] PF6 and [ omim ] PF6 ) were synthesized by reacting alkyl bromide, N-methylimidazolium with NH4PF6 using water-bath microwave method. The results showed that: compared to the conventional method, the yield of production was higher, and the reaction time was dramatically reduced to 50 minutes from 36 hours. Meanwhile, reaction conditions of water-bath microwave synthesis of [ bmim ] PF6 were optimized by orthogonal experiments. The obtained optimization results were: reaction time 50 minutes, molar ratio of butyl bromide, N-methylimidazolium and NH4PF61.1: 1.0: 1.0, microwave power 385 W. Under the above conditions, the yield of [ bmim ] PF6 could reach 94. 54%. The optimization results were also discussed with synthesis mechanism, and three ionic liquids' structures were verified by IR spectrum.
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