双氧水氧化环戊酮合成δ-环戊内酯的工艺分析-process analysis of synthesis of δ - cyclopentanone by oxidation of cyclopentanone with hydrogen peroxide.docx

ABSTRACTδ-valerolactoneisanimportantfinechemicalintermediateandiswidelyused.Inrecentyears,polyvalerolactone,thering-openingpolymerizationproductofδ-valerolactone,haswideapplicationsinthefieldofmedicalmaterialsandenvironmentalprotectioninrecentyears,whichcausesthemarketdemandofδ-valerolactonehasbeenincreasingyearbyyearaccordingly.Therefore,thedevelopmentofacleaningsynthesisroutewhichhasthemildreactionconditionsandiseasyforindustrializedproductionisveryimportant.Therearemanywaystosynthesizeδ-valerolactone,ofwhichtheBaeyer-Villigeroxidationofcyclopentanoneattractsmoreinterest.Withthecyclopentanoneastherawmaterial,thesynthesistechnologyandkineticsforthesynthesisoftheδ-valerolactonewasstudied,whichhasimportantengineeringapplicationprospectandacademicsignificance.Avarietyofcatalysts,suchasLewisacids,metaloxides,werefirstlyscreenedinthesynthesisofδ-valerolactonewithaqueoushydrogenperoxideasanoxidant.TheresultsshowedthatSnO2andWO3hadhighercatalyticactivitythantheothercatalystsforthereaction.ThenusingSnCl4·5H2OandNa2WO4·2H2Oasprecursors,aseriesofSn-WcompositemetaloxideswerepreparedbychemicalprecipitationandcharacterizedbyXRD,FTIR,BETandSEMtechniques.Theresultsshowedthatamongallthemetaloxideswithdifferentmetalratioandcalcinationtemperature,theSnO2/WO3catalystafterbeingcalcinedat600℃withtheSn/Wmolarratioof2:1presentedanexcellentperformance,sothecompositemetaloxideSn/W-2-600waschosenasthecatalystinlaterexperiments.Thepreparationofthecatalystwassimple,andcouldberecoveredthroughsimplefiltractionanddrying,theresultsshoweditcouldbereusedthreetimes.Anewsynthesistechnologyofcyclopentanonetoδ-valerolactonewasexplored,whichusedtheaqueoushydrogenperoxidecontaining30%H2O2asoxidant,propionicacidassolventandthecompositemetaloxideSn/W-2-600ascatalyst.IIBesides,thecyclohexanewasusedaswatercarryingagentandthewholedevicewasundernegativepressureconditions.TheproductwaspurifiedbyvacuumdistillationandthencharacterizedandanalysedbyFTIRand1HNMR.Throughthesingle-factorandorthogonaldesigns,thesynthes