干燥方法对钛柱撑蒙脱石结构的影响王丽娟

　332Vol.33,No.2　20052JOURNALOFTHECHINESECERAMICSOCIETYFebruary,2005王丽娟,廖立兵(,　100083)　:TiCl4,(Ti-pillaredmontmorillonite,TiPILM)。TiPILM(airdrying,AD)、40℃(commondrying,CD)、(ethanolextractiondrying,EAD)、(vacuumdrying,VD),。XRD,IR,DTATG,N2TiPILM。:TiPILM。ADEAD2.7nmTiPILM,AD500℃,285.7m2/g,。CDVD,,TiPILM,。:;;:P578.964;TB383　　:A　　:04545648(2005)02021505EFFECTOFDIFFERENTDRYINGMETHODSONSTRUCTUREOFTITANIUMPILLAREDMONTMORILLONITEWANGLijuan,LIAOLibing(SchoolofMaterialsScienceandEngineering,ChinaUniversityofGeosciences,Beijing　100083,China)Abstract:Titaniumpillaredmontmorillonite(TiPILM)wassynthesizedbycationexchangeofsodiummontmorillonitewithTi-polymericcationspreparedbypartialhydrolysisofTiCl4inHCl.Differentdryingmethods,suchascommondryingat40℃inair(CD),airdryingatroomtemperature(AD),airdryingatroomtemperatureafterethanolextraction(EAD),vacuumdr-yingatroomtemperature(VD),wereusedtoobtainTiPILM,followedbyheattreatmentatdifferenttemperatures.ThestructureofTiPILMwascharacterizedbymeansofXRD,BET,IRandDTATGandresultsshowthatthedryingmethodshavemuchinfluenceonthethermalstabilityofTiPILM.TiPILMwithlargecrystalinterplanarspacingofaround2.7nmcanbeobtainedbyusingthedryingmethodsofTiPILM(AD)andTiPILM(EAD).ThesampledriedbyTiPILM(AD)hasbetterthermalstabilityat500℃anditsspecificsurfaceareareachesto285.7m2/g.Howeverthetitaniapillarsinmontmo-rillonitearecollapsedwhenTiPILMaredriedbyCDandVDmethods,resultedinthedestroyoflayerstructureofTiPILM,whichaffectsthethermalstabilityofthematerial.Keywords:titaniumpillaredmontmorillonite;dryingmethod;thermalstability　　TiO2,,、、、:20040510。:20040721。:(2022017)。:(1979～),,。:(1963～),,,,。、[1]。,,(Ti-pillaredReceiveddate:20040510.Approveddate:20040721.Firstauthor:WANGLijuan(1979—),female,graduatestudentformasterdegree.Email:[e-mail]:LIAOLibing(1963—),male,doctor,professor.Email:[e-mail]:牨牥牨牬牥牰牪牤jissn牥牬牭牬牭牰牬牳牪牥牥牭牥牪牥牨牱montmorillonite,TiPILM),TiO2。,、、。TiPILM、[2,3],。,,TiCl4TiPILM[4,5]。,TiPILM,,TiPILM。TiCl4TiPILM,(airdrying,AD)、40℃(commondrying,CD)、(ethanolextractiondrying,EAD)、(vacuumdrying,VD),,。1　实　　验1.1　、(d001=1.25nm)。TiCl46mol/L,[Ti]=0.82mol/L,[HCl]=0.74mol/L。4d,20mmol/g0.2%,16hCl-。、40℃、、25℃,TiPILM,AD,CD,EAD,VD。,,500℃3hAD5003。1.2　　　D/maxrAX。CuKα(λ=0.154nm),40kV,100mA,2°/min。PE983G,180～4000cm-1,KBr,20℃,38%。WCT2A()DTA,TG。10℃/min,。N2MicromeriticsASAP2400,,1.3Pa200℃4h。BET,BJH(BarrettJoynerHalenda)。2　结果和讨论1　TiPILMXRDFig.1　XRDpatternsofTimontmorillonite(TiPILM)ADsamples(inairdryed)andcal-cinedunderdifferentconditionsThemeaningsofsymbolADinsamplenamearethatthreedigitalnumberdenotesthecalcinedtem-perature,℃;onedigitalnumberdenotesthetimeforcalcinedinhours2.1　TiPILM1XRD。1aTiPILM216　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　2005　,X;1bTiPILM,,,X。1a,2θ3.4°6.5°(d0012.64nm1.34nm)2,TiCl42。300,400,500℃1～3h,6.5°,3.4°,。、,,。,、,,,TiPILM()。700℃3h,3.4°,。,500℃TiPILM。1b1a,1a,500℃3h6.5°。X,1b,,TiPILM。25.3°,,。2TiPILMXRD。2,40℃(CD)25℃(VD)TiPILM(3.4°)。[6,7]TiCl4、CDTiPILM。(EAD)TiPILM3.4°,,500℃1h,。TiPILM,,,[8]。,。,Ti2　TiPILMXRDFig.2　XRDpatternsofTiPILMbydifferentmethodsAD———Airdrying;CD———Commondrying;EAD———Ethanolextractiondrying;VD———Vacuumdrying;EAD5001———ThemeaningofnumberinthenameissameasinFig.1PILM,,,40℃(CD)25℃(VD)TiPILM,。,TiPILM。,TiPILM。2.2　DTATGTiPILM(AD)DTATGNaTiPILM(CD)(3)。Na,96℃,,5.21%。649℃,2,,6.23%。813℃。Na,AD1,,AD。,[Ti20O32(OH)12(H2O)18]4+[9]。244℃,,。2,600℃,ADNa。AD5001217　332　　　　　　　　　　:3　NaTiPILMDTATGFig.3　DTATGcurvesofNamontmorilloniteandTiPILMpreparedbydifferentmethods、,500℃,AD,。CD1、2AD,244℃。CD,TiO2,TiO2,。X。ADCD2、,,Si—O。、TiO2,525℃。ADDTA,244℃,。2.3　、TiPILM(AD)500℃1hIR4。Na,3618cm-1Al—OH,3432,1635cm-1,1040,468cm-1Si—O—SiSi—O,918cm-1Al—O(OH)—Al,796cm-1MgAl—OH[10]。500℃4　TiNaFig.4　IRspectraofairdryingTiPILM(AD)andstartingNamontmorillonite1h,Na3617cm-1,3432,1635cm-1,,Na(),。ADIR,,,Al—OH,3618cm-1。3401cm-1,,,3249cm-1,DTATG。600～900cm-1TiO2。500℃,、,3249cm-1,—OH。796cm-1Mg(Al)OH,Ti。Ti—O—Si,Si—O,Si—O1053,478cm-1。2.4　N2N2。Na、AD,CD,AD5001CD5001,5。5a。,BrunaureⅣ[11],。N2,218　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　2005　。。DeBoreB[12],,。5　TiPILMN2BJHFig.5　N2adsorptiondesorptionisothermsandporesizedistributioncurvesofTiPILM、1。1,AD,CD,AD5001CD5001Na,,。XRD,CD3.4°,1,CDAD(,),CD,。。,AD5001CD5001d001、1　TiPILMN2Table1　InterplanarspacingsandresultsofN2adsorptiondesorptionisothermsofTiPILMSampled001/nmBETsurfacearea/(m2g-1)Porevolume/(cm3g-1)Averageporesize/nmNamont1.2547.80.1099.35CD1.51290.10.2373.87CD50011.24259.10.2284.05AD2.75310.40.2373.75AD50012.26285.70.2283.90,。XRD,。BJH5b,TiPILM,,2～4nm。Ti-PILM,ADCD,,XRD(TiPILM)。3　结　　论TiCl4TiPILM,。,、、,500℃。40℃、、25℃、,,,TiO2。500℃,TiO2,,,,。700℃。:[1]　LINSEBIGLERAL,LUG,YATESJT.PhotocatalysisonTiO2surface:principles,mechanisms,andselectedresults[J].ChemRev,1995,95:735—758.[2]　STERTEJ.Synthesisandpropertiesoftitaniumoxidecross-linkedmontmorillonite[J].ClaysClayMiner,1986,34(6):658—664.[3]　MOGYORÓSIK,DÉKNYI,FENDLERJH.Preparationandcharacterizationofclaymineralintercalatedtitaniumdioxide(continuedonp.224)219　332　　　　　　　　　　:。,。:[1]　MAESN,HEYLENI,COOLP,etal.Therelationbetweenthesynthesisofpillaredclaysan