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1、1-丁基-3-甲基咪唑六氟磷酸鹽離子液體合成研究摘要離子液體是指完全由正負(fù)離子所組成,并且在室溫或接近室溫下呈現(xiàn)液態(tài)的鹽,也稱為低溫熔融鹽。與傳統(tǒng)的有機(jī)溶劑相比,它具有很多優(yōu)點(diǎn):(1)幾乎沒有蒸汽壓、不揮發(fā)、無臭;(2)有較大的穩(wěn)定溫度范圍,較好的化學(xué)穩(wěn)定性及較寬的電化學(xué)窗口;(3)通過陰陽離子的設(shè)計(jì)可調(diào)節(jié)其對(duì)水、有機(jī)物及聚合物的溶解性。本實(shí)驗(yàn)通過微波輔助加熱法制備1-丁基-3-甲基咪唑六氟磷酸鹽離子液體。制備的基本過程:將藥品l-甲基咪唑、溴代正丁烷、六氟磷酸鉀按一定比例混合于反應(yīng)容器內(nèi),然后置于微波爐中加熱。將制得的產(chǎn)物進(jìn)行提純,并進(jìn)行紅外分析,確定其是否
2、為目標(biāo)產(chǎn)品。本實(shí)驗(yàn)通過對(duì)加熱方法、加熱時(shí)間及藥品的配比等方面的改變,最終確定一個(gè)產(chǎn)率較高的實(shí)驗(yàn)方案:將混合好的藥品(l-甲基咪唑、溴代正丁烷、六氟磷酸鉀摩爾比為:1:1.1:1.6)放入微波爐,功率調(diào)至最低,采用加熱3s,暫停30s的間歇加熱方法,反應(yīng)時(shí)間100min,再用去離子水和乙醚分別對(duì)其洗滌數(shù)次,最后對(duì)產(chǎn)物進(jìn)行減壓蒸餾,最終產(chǎn)物產(chǎn)率在60%左右。關(guān)鍵詞:微波,提純,離子液體,紅外光譜,1-丁基-3-甲基咪唑六氟磷酸鹽STUDYONSYNTHESISOF1-BUTYL-3-METHYLIMIDAZOLIUMHEXAFLUOROPHOSPHATEIONIC
3、LIQUIDABSTRACT?Ionicliquidsarecomposedentirelyofpositiveandnegativeions,andpresentatornearroomtemperatureliquidsalt,alsoknownaslow-temperaturemoltensalt.Comparedwithtraditionalorganicsolvents,ithasmanyadvantages:1.almostnovaporpressure,non-volatile,colorless,odorless;2.withagreaterr
4、angeofstabletemperature,goodchemicalstabilityandwide?electrochemicalinterface;3.itcanbeadjustedthesolubilityforwater,organiccompoundsandpolymersthroughthedesignofions.Inthisstudy,1-butyl-3-methylimidazoliumhexafluorophosphateionicliquidwaspreparedusingmicrowave.?Thebasicprocessofpre
5、paration:l-methylimidazole,n-butanebromideandpotassiumhexafluorophosphateweremixedinthecontaineratacertainpropotion,andthenheatedwiththemicrowave.Purifytheproduct,andtaketheinfraredanalysistodeterminewhetherthetargetproduct.?Theexperimentalprogramwithahigheryieldwasultimatelyestabli
6、shedbychangingheatingmethod,heatingtimeandtheratioofdrugsandsoon.Firstly,mixtureofdrugswereputtedinthemicrowaveovens,mostlow-endgearpreparedbyheating3s,suspended?30sintermittentheatingmethod,reactiontimewas100min.Secondly,de-ionizedwaterandetherwereusedtowashthemseveraltimes,respect
7、ively.Finally,theproductswerecarriedonthereducedpressuredistillation,andthefinalproductyieldwasaround60%.KEYWORDS:Microwave,purification,infraredspectroscopy,ionicliquidhexafluorophosphate,1-butyl-3-methylimidazolium目錄第1章緒論1§1.1離子液體的定義1§1.2離子液體的發(fā)展史1§1.3離子液體的分類2§1.4離子液體的性質(zhì)及應(yīng)用3§1.4.1離
8、子液體的性質(zhì)3§1.4.2離子液體的應(yīng)