结晶母液中锆钇的分离回收分析-separation and recovery analysis of zirconium and yttrium in crystallization mother liquor.docxVIP

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结晶母液中锆钇的分离回收分析-separation and recovery analysis of zirconium and yttrium in crystallization mother liquor.docx

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结晶母液中锆钇的分离回收分析-separation and recovery analysis of zirconium and yttrium in crystallization mother liquor

ABSTRACTWiththewidelyapplicationofzirconiumandyttriuminyttria-stabilizedzirconia(YSZ)ceramic,ceramicwastecontainedzirconiumandyttriumisincreasing.BecauseChinesereservesofzirconiumispoor,andthereservesofyttriumisrelativerichbuttheamountislimited,therefore,studyinrecoveryofzirconiumandyttriumisimminent.HydrochloricacidsolutioncontainingzirconiumandyttriumwasobtainedfromYSZceramicwastebymechanicalcrushing,alkalidissolutionandaciddissolution.Andcrystallizationmotherliquor(CML)wasobtainedaftercoarsecrystallization.Inthisprocess,CMLunavoidablycontainedotherimpuritiesfromYSZceramicwasteandtheexternal.TheresultsofXRFtestshowedthattheseexsitsironandtraceofcopperexceptzirconiumandyttriumintheCML.Tofastlyandaccuratelydeterminethecontentofzirconium,ironandyttriuminintheCML,amethodaboutcontinuousdeterminationoftheZr-Fe-YcontentbyEDTAhasbeendiscussedbasedonaseriesofmethodsaboutseparatedeterminationofzirconiumoryttriumiron,.Amixedsolutionconsistsofzirconiumchloride,ferricchlorideandyttriumchloridewithdifferentratiohadbeenprepared.Then,theinfluenceofpHvalue,someironionmaskingagentsandindicatorswasstudied.Finally,reasonableexperimentalschemeforcontinuousdeterminationoftheZr-Fe-Ycontentwasdesigned.Theschemewasasfollow:xylenolorangeastheindicator,transformedFe3+intoFe2+byaddingareductantatpH≈0.2,andthentitratingZrO2+,afterthat,transformedFe2+intoFe3+byanoxidantatpH≈1.5andtitratingFe3+withtheexistenceofaceticacid,andfinally,titratingY3+aspH=5～6.TheRSDofthismethodwaslessthan2%.TheanalysisresultsoftheCMLwereCZrO2+=0.825mol/L,CFe3+=0.107mol/L,CY3+=0.085mol/L.BecauseironionhadgreatinfluenceontheseparationofZrandYbyextracting,experimentschemeofremovingironbeforetheseparationofzirconiumandyttriumwasdesigned.Itwasfoundthat81%oftheironioncouldbeextractedexceptZrO2+andY3+through3stagesofcounter-currentextractionwhentheacidityofthematerialliquidwas5mol/L,andtheextractingagentwas2-octanol:kerosene=7:3,andO:A=1:1.ItwasfoundthattheextractioneffectofP204wasbetterthanthatofP507,soP204wasadoptedforthe