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疏水性咪唑类离子液体的水浴微波合成
Water-bath microwave synthesis of hydrophobic imidazolium-based ionic liquids
【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.
【Abstract】 Three hydrophobic imidazolium-based ionic liquids(PF6,[hmim]PF6 and 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 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 PF6 could reach 94.54%.The optimization results were also discussed with synthesis mechanism,and three ionic liquids′ structures were verified by IR spectrum.
【Key words】 hydrophobic; ionic liquid; microwave synthesis; optimization;
- 【文献出处】 南京工业大学学报(自然科学版) ,Journal of Nanjing University of Technology(Natural Science Edition) , 编辑部邮箱 ,2007年03期
- 【分类号】TQ252.3
- 【被引频次】10
- 【下载频次】578