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1、1-丁基-3-甲基咪唑六氟磷酸盐离子液体合成研究摘要离子液体是指完全由正负离子所组成,并且在室温或接近室温下呈现液态的盐,也称为低温熔融盐。与传统的有机溶剂相比,它具有很多优点:(1)几乎没有蒸汽压、不挥发、无臭;(2)有较大的稳定温度范围,较好的化学稳定性及较宽的电化学窗口;(3)通过阴阳离子的设计可调节其对水、有机物及聚合物的溶解性。本实验通过对加热方法、加热时间及药品的配比等方面的改变,最终确定一个产率较高的实验方案:将混合好的药品(l-甲基咪唑、溴代正丁烷、六氟磷酸钾摩尔比为:1:1.1:1.6)放入微波炉,功率调至最低,采用加热3s,暂停30s的间歇加热方法,反应时
2、间100min,再用去离子水和乙醚分别对其洗涤数次,最后对产物进行减压蒸馏,最终产物产率在60%左右。ISTUDYONSYNTHESISOF1-BUTYL-3-METHYLIMIDAZOLIUMHEXAFLUOROPHOSPHATEIONICLIQUIDABSTRACTIonicliquidsarecomposedentirelyofpositiveandnegativeions,andpresentatornearroomtemperatureliquidsalt,alsoknownaslow-temperaturemoltensalt.Comparedwithtradit
3、ionalorganicsolvents,ithasmanyadvantages:1.almostnovaporpressure,non-volatile,colorless,odorless;2.withagreaterrangeofstabletemperature,goodchemicalstabilityandwideelectrochemicalinterface;3.itcanbeadjustedthesolubilityforwater,organiccompoundsandpolymersthroughthedesignofions.Inthisstudy,1
4、-butyl-3-methylimidazoliumhexafluorophosphateionicliquidwaspreparedusingmicrowave.Thebasicprocessofpreparation:l-methylimidazole,n-butanebromideandpotassiumhexafluorophosphateweremixedinthecontaineratacertainpropotion,andthenheatedwiththemicrowave.Purifytheproduct,andtaketheinfraredanalysis
5、todeterminewhetherthetargetproduct.Theexperimentalprogramwithahigheryieldwasultimatelyestablishedbychangingheatingmethod,heatingtimeandtheratioofdrugsandsoon.Firstly,mixtureofdrugswereputtedinthemicrowaveovens,mostlow-endgearpreparedbyheating3s,suspended30sintermittentheatingmethod,reaction
6、timewas100min.Secondly,de-ionizedwaterandetherwereusedtowashthemseveraltimes,respectively.Finally,theproductswerecarriedonthereducedpressuredistillation,andthefinalproductyieldwasaround60%.KEYWORDS:Microwave,purification,infraredspectroscopy,ionicliquidIIhexafluorophosphate,1-butyl-3-methyl
7、imidazoliumIII目录第1章绪论....................................................................................1§1.1离子液体的定义................................................................1§1.2离子液体的发展史............................................................