固载化离子液体的制备及其应用

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1、摘要定性差和键和型纤维素类CSP手性拆分性能差的缺点。关键词：离子液体B一环糊精纤维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