Advances in Crystallization Elution Fractionation.pdf

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1、14Macromol.Symp.2009,282,14–24DOI:10.1002/masy.200950802AdvancesinCrystallizationElutionFractionationB.Monrabal,*L.Romero,N.Mayo,J.Sancho-TelloSummary:CrystallizationElutionFractionationhasbeenoptimizedtoimproveresolutionpowerandreduceco-crystallization.Mostimport

2、antsteptobeoptimizedisthefirstseparationcycleofDynamicCrystallizationwhichcanbeinvestigatedwiththehelpofCrystallizationAnalysisFractionationexperiments.Anewapproachtoreduceco-crystallizationandimproveresolutionispresentedbyapplyingsuccessivecoolingandheatingcyclesi

3、nalongcolumn.ThenewprocessknownasMultipleCrystallizationElutionFractionationaddsextendedseparationateachcoolingandheatingcycles.Keywords:CCD;CEF;CRYSTAF;crystallization;polyethylene;TREFIntroductionInthispaper,theoptimizationoftheDynamicCrystallizationprocessisinv

4、esti-CrystallizationElutionFractionation(CEF)gated.PreliminaryCRYSTAFresultshaveisanewseparationtechniquefortheprovedtobeveryhelpfultoestablishtheanalysisoftheChemicalCompositionmostappropriatecrystallizationtempera-Distribution(CCD)insemicrystallinepoly-turerange

5、andcrystallizationßowtobemers.CEFwasintroducedin2006attheusedinfollowingDCandCEFruns.TheFirstInternationalConferenceonPolyole-optimizationobtainedinDCwillapply[1]ÞnCharacterizationinHouston.TheautomaticallytoimprovetheCEFanalysis.CEFtechniqueisbasedonanewsepara-An

6、ewprocessofrunningCEFwithtionprinciplereferredtoasDynamicmultiplecrystallization-dissolutioncycles[2]Crystallization(patentpending)thatinalongcolumnisbeingpresented.Theseparatesfractionsinsideacolumnbynewapproach,whichwewillrefertoascrystallizabilitymeanwhileasmal

7、lßowofMultipleCrystallizationElutionFractiona-solventispassingthroughthecolumn;thetion,m-CEF,resemblestheZoneMeltingseparationinDynamicCrystallization(DC)processforpuriÞcationofcrystallinesolids.occursduringthecoolingstepandthereforeresultsarecomparabletoCrystalli

8、zation[3]AnalysisFractionation(CRYSTAF).TechniquesDescriptionCEFcombinestheseparationpowerofDCinthecrystallizationstepwiththeTemperatureRisingElutionFra