不同pH下鸟粪石MAP法目标产物的分析与表征王崇臣

29　42010　　7　　　ENVIRONMENTALCHEMISTRYVol.29,No.4July　　2010　200951.　＊(863)(2006AA06Z320);(50978013);(PHR20100508PHR201008372);(KM200910016009);2009().　＊＊.pH(MAP)＊王崇臣　郝晓地＊＊　王　鹏　兰　荔(,,,100044)　　XRD,IR,TGApHMAP.XRDIR,.,(90.0%)pH7.0—9.0,,(90.0%)pH7.0—7.5.　XRD,IR,TGA,,.　　(MgNH4PO4·6H2O,MAP),(MAP),[1—7].　　X(XRD)、(IR)、(TGA)pHMAP,,pHCa2+.1　1.1　　　A:Ⅰ0.5L5.0mmolNaH2PO4·2H2O;Ⅱ0.5L6.0mmolMgSO4·7H2O15.0mmolNH4Cl.Ⅱ1.5L,Ⅰ,.Mg∶N∶P1.2∶3∶1..pH=7.0,NaOH(NaOH,1mol·l-1NaOH)0.5pH,pH,7.0—11.0.(25℃),.、1h,.,,,().,(25℃).　　B:,A.:C(Ca2+)=2.17mmol·l-1,C(Mg2+)=1.34mmol·l-1.1.2　　　(99.0%,Alfa-Aesar).　　RigakuD/maxⅢAX(CuKα,λ=1.5406A゜,,10°,80°,3°·min-1).Spectrum100FT-IR4000—400cm-1(KBr).ZRY-1P,10℃·min-1600℃,,α-Al2O3.IRISAdvantageICP-AES,DX-120Mg2+、Ca2+NH+4-N.760　　　　　　　　292　2.1　XRD　　,XRD,1.1,pH7.5—9.0,pH7.0—8.5,(001)、(002)2θ20.85°、33.27°,MgNH4PO4·6H2O(PDF#15-0762),MgNH4PO4·6H2O.　　,,pH9.5,,Mg3(PO4)2·4H2O,Mg(OH)2(001)(002),MgNH4PO4·6H2O,Mg3(PO4)2·4H2O、Mg(OH)2,LeCorre[8]XRD.,,pH=9.0,Mg3(PO4)2、Mg(OH)2、Ca3(PO4)2(Ksp=2.1×10-33)CaHPO4(Ksp=1.8×10-7)(001)(002).1　(A)(B)pHXRD1.,2.pH=7.5,3.pH=8.0,4.pH=8.5,5.pH=9.0,6.pH=9.5,7.pH=10.0,8.pH=10.5,9.pH=11.0,10.pH=11.5Fig.1　XRDpatternofprecipitatesobtainedunderdifferentpHinpurewater(A)andtapwatersystem(B)　　1,,pH10.5,(001)(002),,.2.2　　　2pH.2　(A)(B)pHIR1.pH=7.5,2.pH=11.5Fig.2　IRspectrumofprecipitatesobtainedunderdifferentpHinpurewatersystem(A)andtapwatersystem(B)　　2,pH=7.5—11.0pH=7.5—10.0　4:pH(MAP)761　　455cm-1、568cm-1、1000cm-11430cm-1NH+4[9],pH,,,.,NH+4(1500—1385cm-1),,,,,.2.3　　　pHTGDTA,3,50℃,[10].100℃,600℃,45%.Frost[11],42%,(7.34%),(34.65%),1mol,4.7mol,.,,,MAP.3　TGDTAFig.3　TGandDTAplotofsomeselectedprecipitates2.4　　　,,MAP[5].N、P、Mg1∶1∶1,XRD,pH,PMg,Mg(OH)2(Ksp=5.1×10-12)Mg3(PO4)2(Ksp=1.0×10-24).NH+4(MgNH4PO4,CaNH4PO4).,N.(1):　　=n×Mm×100%(1),m;n;M.　　(1),98.9%,(99.0%).,4.4　(%)pHFig.4　EffectofpHonthestruvitecontentsintheprecipitatie762　　　　　　　　29　　4,pH7.510.5,,,90%pH7.5—9.0,pH10.5,.pH,Ca2+.pH7.07.5,96.8%95.7%.pH7.5,,pH=10.0,15.5%.pH10.5,.2.5　　　,pH,,50.12%96.27%(5),MAP.pH,,,AltinbasM[12].pHNH+4-NNH3、[13],,pH.pH.pH,,pH.5　pHFig.5　TheP-removalrateandstruvitecontentintheprecipitatesunderdifferentpHinpurewatersystem3　　　pH,pH,pH,.90%pH7.5—9.0,Ca2+90%pH7.0—7.5.　　Ca2+Mg2+,pH,Ca,.　　　[1]　PastorL,ManginD,BaratRetal.,APilot-scaleStudyofStruvitePrecipitationinaStirredTankReactor:ConditionsInfluencingtheProcess[J].Bioresour.Technol.,2008,99(14)∶6285—6291[2]　RonteltapM,MaurerM,GujerW,StruvitePrecipitationThermodynamicsinSource-SeparatedUrine[J].WaterRes.,2007,41∶977—984[3]　WilsenachJ,SchuurbiersC,VanLoosdrechtM,PhosphateandPotassiumRecoveryfromSourceSeparatedUrinethroughStruvitePrecipi-tation[J].WaterRes.,2007,41∶458—466[4]　HaoXD,vanLoosdrechtMCM,Model-BasedEvaluationofStruviteRecoveryfromP-releasedSupernatantinaBNRProcess[J].WaterSci.Technol.,2006,53(3)∶191—198[5]　HaoXD,WangCC,LanLetal.,StruviteFormation,AnalyticalMethodsandEffectsofpHandCa2+[J].WaterSci.Tech.,2008,58(8)∶1687—1692[6]　AbbonaF,BoistelleR,LundagerH,CrystallizationofTwoMagnesiumPhosphates,StruviteandNewberyite:EffectofpHandConcentra-tion[J].J.Cryst.Growth,1982,57∶6—14[7]　,,,MAP[J].,2009,30(4)∶185—190[8]　LeCorreK,Valsami-JonesE,HobbsPetal.,ImpactofCalciumonStruviteCrystalSize,ShapeandPurity[J].J.Cryst.Growth,　4:pH(MAP)763　　2005,283(3—4)∶514—522[9]　BanksE,ChianelliR,KorensteinR,CrystalChemistryofStruviteAnalogsoftheTypeMgMPO4.6H2O(M=Potassium(1+),Rubidium(1+),Cesium(1+),Thallium(1+),Ammonium(1+)[J].Inorg.Chem.,1975,14∶1634—1639[10]　RensburgPV,MusvotoEV,WentzelMCetal.,ModellingMultipleMineralPrecipitationinAnaerobicDigesterLiquor[J].WaterResearch,2003,37(13)∶3087—3097[11]　FrostRL,WeierML,KristyLErickson,ThermalDecompositionofStruviteImplicationsfortheDecompositionofKidneyStones[J].JournalofThermalAnalysisandCalorimetry,2004,76∶1025—1033[12]　AltinbasM,YanginCOzturkIStruvitePrecipitationfromAnaerobicallyTreatedMunicipalandLandfillWastewaters[J].WaterScienceandTechnology,2002,46(9)∶271—278[13]　AndradeA,SchuilingR,TheChemistryofStruviteCrystallization[J].MineralJournal,2001,23(5—6)∶37—46THEANALYSISANDCHARACTERIZATIONOFPRECIPITATESOBTAINEDFROMSTRUVITE(MAP)PRECIPITATIONWANGChong-chen　　HAOXiao-di　　WANGPeng　　LANLi(KeyLaboratoryofUrbanStormwaterSystemandWaterEnvironment,BeijingUniversityofCivilEngineeringandArchitecture,Beijing,100044,China)ABSTRACT　　TheprecipitatesharvestedfromMAPmethodunderdifferentpHconditionswerecharacterizedandanalyzedbyXRD,IR,TGAandelementalanalysis.TheresultsrevealthatXRDandIRcanqualitativelydeterminethepresenceofstruviteintheprecipitates,whiletheelementalanalysismethodcanquantitativelydefinetheexactcontentofstruvite.AndtheelementalanalysisresultsshowthattheoptimalpHrangeforhavinghighstruvitecontent(90.0%)wasrespectivelybetween7.5—9.0underpurewatersystemand7.0—7.5undertapwatersystem.　　Keywords:XRD,IR,TGA,elementanalysis,struvite.