PEINaAAl2O3复合支撑分子筛膜的微波水热合成

27520105FINECHEMICALSVol.27,No.5May2010:2010-01-25;:2010-02-04:(20976057,20876064):(1969-),,,,,E-mail:[e-mail]:,E-mail:[e-mail]2NaA/2Al2O31,1,2,13(1.,510640;2.,510640):(PEI)2NaA/2Al2O3NaA,X(XRD)(SEM)NaAXRD,NaA;SEM,NaANaA,,,95%,0105kg/(m2h),13000:2NaA/2Al2O3;NaA;;;:TQ426.61:A:1003-5214(2010)05-0421-05MicrowaveSynthesisofPolyetherimide2NaA/2Al2O3SupportedZeoliteMembraneYUANWen2hui1,CHENHua2rong1,LILi2,OUYANGXin2ping13(1.SchoolofChemistryandChemicalEngineering,SouthChinaUniversityofTechnology,Guangzhou510640,Guangdong,China;2.CollegeofEnvironmentalScienceandEngineering,SouthChinaUniversityofTechnology,Guangzhou510640,Guangdong,China)Abstract:Thehigh2performanceNaAzeolitemembranewassynthesizedonpolyetherimide(PEI)2NaAzeolite/2Al2O3compositesupportsbythemicrowaveheatingmethod.Theinfluenceofmicrowaveheatingtimeonmembranesynthesiswasmainlyinvestigated.Theas2synthesizedNaAzeolitemembraneswerecharacterizedbyXRDandSEM.XRDresultsshowthatonlyNaAzeoliteemergesonthecompositesupportsurface.TheSEMresultsshowthecompositesupportsurfaceisfullycoveredbyuniformandcompactNaAzeolitemembrane.Thepervaporationpropertiesoftheas2synthesizedmembranewereevaluatedbythedehydrationofalcohol/watermixture.Itwasfoundthatthefluxdecreasedwiththeincrementofthealcoholamountinthefeedandtheseparationfactorswerethecontrary.Thepervaporationresultspresentthattheseparationfactorswereashighas13000atm(CH3CH2OH)/m(H2O)=955.Ontheotherhand,thefluxeswereonly0105kg/(m2h).Keywords:PEI2NaAzeolite/2Al2O3;NaAzeolitemembrane;microwavesynthesis;pervaporationseparation;functionalmaterialsFoundationitem:SupportedbyNationalNaturalScienceFoundationofChina(20976057,20876064),[1],[2-3],,,,A(LTA),014nm,,[4],Xu[5]A2Al2O3NaA,9015min,4[6]n(Na2O)n(SiO2)n(Al2O3)n(H2O)=32121500,(dip2coating),NaA,1/41/5,012m,3m,H2/N25,H2O/EtOH690Ge[7](),10000PEINaA,NaA,,NaA(PEI),2Al2O3,NaA,XRDSEM/1111(AR,96%,),(Na2SiO39H2O,AR,),(PEI,GE),(AR,),(Al2O3Na2O,AlfaAesar)2Al2O3(211cm,2mm,30%40%)1121g50mL,20mL,015gNaA,2Al2O3,5s,10min,,606h,2NaA/2Al2O3113NaANaA:n(Na2O)n(SiO2)n(Al2O3)n(H2O)=504151950:5148gNa2SiO39H2O,20g,(50,350r/min)A;1718gNaOH017gNaAlO2,4615g,(50,350r/min)B;AB,BA,800r/min,5h,AB,,,,(60)6h,,1min90,1020min(150W,2450Hz),,12012h,NaA114X(XRD)NaA,XRDBrukerD8,:CuK(=1.5410-10m),30mA,40kV,550S-3700N(Hitachi)NaA,5min115NaA,NaA1NaA,,,,/,,,224FINECHEMICALS271;2;3;4;5;6;7;8;91Fig.1Schematicdiagramofpervaporation(Q),,:Q=WtA,W(kg);t(h);A(m2):=Ya/YbXa/Xb,XYab,a,b2211NaA21111290,NaAXRD2NaAXRDFig.2XRDprofilesofNaAzeolitemembranesynthesizedatdifferentmicrowaveirradiationtimes2,,,NaA10min,NaA,;15min,NaA,NaA;,20min,NaA,,2=1319NaA,,,;,,NaA,15min21112390,15min,2Al2O3/NaASEMa2Al2O3;b2Al2O3;c;d3NaASEMFig.3SEMimagesofNaAzeolitemembranes3245,:PEI2NaA/2Al2O33(a)(c),2Al2O3NaA,,2m,,;2NaA/2Al2O3,,,,12m,(b)(d),,,,8m,,2NaA/2Al2O3NaANaA,,,,,,212NaA4504NaAFig.4PermeationpropertiesofNaAzoelitemembraneswithdifferentEtOHconcentrations4,,,,-[8]:(1);(2);(3)NaA,,,,,,NaA,,95%,13000[9],NaA,/,1NaA/1NaATable1ComparisonofpervaporationpropertiesofNaAzeolitemembranesA/BB/%Q/kg/(m2h)A/B2Al2O3H2O/EtOH8595011930092Al2O3H2O/EtOH9501335690102Al2O3H2O/IPA95112710000112Al2O3H2O/EtOH900177246000122Al2O3H2O/EG85311810000132Al2O3H2O/EtOH80950105012130001,A,2NaA/2Al2O3NaA3n(Na2O)n(SiO2)n(Al2O3)n(H2O)=504151950,2NaA/2Al2O3,90150W15min,NaAXRDSEM,NaA,,,,,95%,0105kg/(m2h),13000NaA:[1],,,.[J].,2004,33(9):891-892.[2]PiereaE,CoronasJ,SalomonMA,etal.Synthesis,characterizationandseparationpropertiesofacompositemordenite/ZSM-5/chabazitehydrophilicmembrane[J].JournalofMembraneScience,1998,149(1):99.(432)424FINECHEMICALS2745w()=013%,11Table1Thefoamandinterfacialtensionpropertiesofsodiummono2fattyalcoholphthalate/(mN/m)/mm0s5min31310-218818611310-217517251610-316516021110-31591551,,,,,,,,10-3mN/m3(1):n()n()=1116,100,BN-1,,5h(2),,:[1].[D].:,2005.[2],,,.pas[J].,2005,12(2):88-90.[3],,,.pas-12[J].,2005,22(1):53-56.[4]Ishiguro,Hitoshi.Compositioncontainingphthalicacidmonoesterwithgoodstabilityandflowability[P].WO:2001007395,2001-02-01.[5]Tapnikar,SanjayMadhusudan.Selectivecatalyticesterificationofphthalicanhydridetomonoesters[P].IN:178729,1997-06-14.[6]JoshiRikesh,PatelHeemanshu.Synthesisofmonoestersanddiestersusingeco2friendlysolidacidcatalysts2M()tungstatesandphosphates[J].IndianJournalofChemicalTechnology,2008,15(3):238-243.[7]SkrzypekJerzy,LachowskaMaria.Synthesisofbis(22ethylhexyl)phthalateovermethanesulfonicacidcatalyst.Kineticinvestigations[J].ReactionKineticsandCatalysisLetters,2008,93(2):281-286.[8]JayakumarR,RajkumarM.Synthesis,characterizationandantibacterialactivityofdivalentmetalsaltsofmono(hydroxyethoxyethyl)phthalate[J].OrientalJournalofChemistry,2000,16(2):243-248.[9].[J].,1997(2):16-18.[10],,.[J].,1996(1):27-30.[11],.[J].,1995(3):24-26.[12],,.[J].,1998(5):24-26.[13],.[J].:,2006,32(1):93-95.[14],,,.(9)[J].,2005,6(9):38-41.[15],.[P].CN:101104139,2008-01-16.[16].[P].CN:10085456,2006-12-27.[17],.S2O82-/ZrO2[J].,2007,8(6):22-23,27.(424)[3]DudukovicMP.Trendsincatalyticrectionengineering[J].CatalysisToday,1999,48(1/2/3/4):