固載化離子液體的制備及其應(yīng)用

固載化離子液體的制備及其應(yīng)用

ID:32503388

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頁數(shù):60頁

時間:2019-02-09

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1、摘要定性差和鍵和型纖維素類CSP手性拆分性能差的缺點。關(guān)鍵詞:離子液體B一環(huán)糊精纖維素手性固定相手性拆分ⅡAbstractIonicliquidbecauseofitsuniquenaturehasawiderangeofapplicationsontheseparationandpurification.Cyclodextrinandcelluloseisopticallyactivenaturalpolymer,andischeapandeasytoget.Ashighpressureliquidchromatography(HPLC)

2、chiralstationaryphase(CSP),theyhavehighselectivityandawiderangeofapplications.Thepurposeofthisstudyistoexplorethesynergiesgeneratedbycombiningtheionicliquidandchiralactivemoleculesbothimmobilizedonthesurfaceofsilicagelandresearchapplicationperformanceonchiralseparationandp

3、urificationoffinechemicalsfield.Themaincontentsandresultsarcasfollows:1.Adoptingbatchfeeding,6-deoxy—tosyl-p—Cyclodextrin(6-OTs—p-CD)ispreparedbythereactionof13-Cyclodextrin(13一CD)andp-toluenesulfonylchloride(p—TsCl)insodiumhydroxideaqueoussolution.Bysingle-factormethodexa

4、miningeffectofreactionconditionontheyield,theoptimumtechnologicalconditionsarefoundasfollows:totalreactiontime5h,reactiontemperature0℃,alkalisolubility0.45mol/L,theamountofalkalisolution240mL(whentheamountof13-CDis8g),咒(p—TsCl):n(13-CD)=4.Undertheseconditions,theyieldof6-O

5、Ts—p—CDisupto46.2%.Thenbymulti—stepreaction.the13-cyclodextrinchiralionicliquidwithcertainchairalseparationperformanceandthermalstabilityisprepared.TheproductsofeachstepofthereactionarecharacterizedbyinfraredspectroscopyandNMRtodeterminethestructure.2.Bythepolymericgraftin

6、gmethod,the[3-cyclodextrinchiralionicliquidisimmobilizedtothesurfaceofthesilicagel,obtainingchiralstationaryphaseCSPI.Testingchiralseparationperformance,theresultsshowthat:1)CSPIdoesnotfitinthenormalphasemode,becauseitispronetoswelling,resultingincolumnpressureincreasing.2

7、)Undertheinvertingmode,CSPIseparatesavarietyofacidicchiralcompoundenantiomers,andhasgoodstability,buthaspoorseparationperformanceforalkalineandneutralchiralcompounds.TakingDL—alpha—Methoxyphenylaceticacidforexample,theeffectofthemobilephaseconditionsonseparationIIIAbstract

8、performanceshowsthat:whenthemethanol/water=30/70(V/功,theseparationdegreeislarger;flowrate

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