硅酸钠溶液分步碳分制备高纯沉淀氧化硅

614Vol161No1420104CIESCJournalApril2010,,,(,110004):;;:TQ12712:A:0438-1157(2010)04-1064-05PreparationofhighpuritySiO2bysplit2stepcarbonationprocessfromindustrialsodiumsilicatesolutionWANGJiadong,SHENXiaoyi,ZHAIYuchun,WUYan(SchoolofMaterialsandMetallurgy,NortheasternUniversity,Shenyang110004,Liaoning,China)Abstract:Byusingindustrialsodiumsilicatesolutionasrawmaterial,highpuritySiO2powderwassuccessfullysynthesizedbythesplit2stepcarbonationmethod1TherelationsbetweenpHvalueofendpointandtheremovalpercentageofimpurityatthefirstcarbonationandthepurityandyieldofproductSiO2powderatthesecondcarbonationwerestudied1TheSiO2powderwascharacterizedbyusingXRD,SEM,IRandcompositionanalysis1TheresultsshowedthatwhenthepHvalueofendpointatthefirstcarbonationwas1019,thepurityofSiO2preparedwasupto9919%1TheSiO2powdersynthesizedwasamorphouswithregularsphereshape,uniformsizeandnoreunion1Thereactionmechanismwasalsodiscussed.Keywords:sodiumsilicatesolution;SiO2;split2stepcarbonation2009-08-19,2010-01-20::(1979-),,:(2007CB613603)SiO2,,[123],,[427],SiO2SiO2,[8210],,CO2SiO2[11212],SiO2,SiO2,SiO2,,[13]SiO2Receiveddate:2009-08-19.Correspondingauthor:Prof.ZHAIYuchun,knightwjd@1261comFoundationitem:supportedbytheNationalBasicResearchProgramofChina(2007CB613603).1111:Na2SiO3(NaOH,1),CO2,NaOH(AR),:TFCE102012,1;KY2;SHZ2D();WB4PHG1000pH;XEPOSX;D/max22500PCX;SSX2550;Nicolet380FTIR1Table1Compositionanalysisofsodiumsilicatesolution/gL-1SiO2Na2OAl2O3Fe2O3ZnOMnOCaO721271600131014201030100201031121m3,2m3,400rmin-1,80,38%CO2,6Lmin-1,pHpH,pH=1019,,,pH=9915,,,,,113D/max22500PCX,SSX2550,Nicolet380FTIR,XEPOSX2211pHpH1,,pH,AlCa,100%,pH=1019,FeZn100%,Mn70%:AlCaFeZnMn,,pHNa2SiO3AlCaFeZn,Mn1pHFig11RelationshipbetweenpHvalueofendpointofthefirstcarbonationandratioofpurityremoval212pH2pH,,pH,,pH1019,SiO29919%2pHFig12RelationshipbetweenpHvalueofendpointofthefirstcarbonationandproductpurityofthesecondcarbonation213pH3pH,pH,,pH,11141019,115%,pH101956014:3pHFig13RelationshipbetweenpHvalueofendpointofthefirstcarbonationandyieldofthesecondcarbonation2,FeAlNaFeO2NaAlO2,CO2,,NaFeO2NaAlO2Fe(OH)3Al(OH)3,SiO2CO2-3,CO2-3Ca2+Mn2+,Fe(OH)3Al(OH)3,pH1019,,CO2,,pH9915,CO2,,,99152Table2SolubilityconstantsofmetallicimpuritiesionsFe(OH)3Al(OH)3CaCO3MnCO3ZnCO3310-39310-33310-9310-11310-11214SiO2pH=1019,pH=9SiO244(a)SiO2XRD,SiO22=23,SiO24(b)SiO2SEM,SiO2,SiO24(c)SiO210002h,1118175cm-1SiOSi478165cm-1SiOSi806145cm-1SiO4,3480cm-1968cm-1SiOH[14215],SiO2215SiO2SiO2,80SiO2660161SiO21000,XEPOSX,33SiO2Table3CompositionanalysisofSiO2product/%SiO2Al2O3Fe2O3ZnOMnOCaO99196010038010001401000200100042010014HG/T3065-1999,SiO2,HG/T30651999,4,SiO2HG/T306519994HG/T30651999Table4ComparisonbetweenHG/T30651999andtestingresultsofproductItemDataofHG/T30651999TestingresultcontentofSiO2/%909919pHvalue510810713masslossofheating/%410810611masslossofigniting/%710519absorptionvalueofDBP/cm3g-1210315217specificsurfacearea/m2g-170200165216SiO2Na2SiO3CO2SiO2nH2O,,,,:Na2OSiO2+nH2O+CO2Na2CO3+SiO2nH2OSiO2nH2OSiO2kH2O+(n-k)H2ONa2CO3+CO2+H2O2NaHCO3,SiO2,SiO2,SiO2,pH,pH=1019,,,Al3+,NaAlO2,Al(OH)3,SiO2,SiO2Al(OH)3,,pH9915,,SiO2,SiO2SiO255Fig15FlowchartofproducingSiO2bysplit2stepcarbonationmethod3SiO2,(1)pH=1019,AlCaFeZn100%,AlCaFeZnMn(2)pH1019,SiO29919%(3)SiO2References[1]LiFengsheng().Ultra2FinePowderTechnique().Beijing:NationalPress,2000[2]LiuJiping(),HaoXiangyang().NanotechnologyandScience().Beijing:SciencePress,2002:30231[3]HuBing(),JiangBinbo(),ChenJizhong().Manufacturetechnologiesandapplicationsofmono2dispersesilicondioxide1ChemicalIndustryandEngineeringProgress(),2005,24(7):603260776014:[4]XueJuanqin(),LanXinzhe(),DuShiyi(),LiWeida(),MengLingai().MechanismofSO2ultrasonicdesorptionfromcitratesolution1JournalofChemicalIndustryandEngineering(China)(),2007,58(4):9442950[5]ShenXiaoyi(),ZhaiYuchun(),LiuYan().Thepreparationofmono2dispersesphericalsilicondioxidebyultrasonichydrothermalandanalysisofinfluencingfactors1JournalofChemicalIndustryandEngineering(China)(),2008,59(4):9732977[6]ShenXiaoyi(),ZhaiYuchun(),SunYang().Preparationandcharacterizationofultrafinesilicapowderbymicrowavehydrothermal1JournalofSyntheticCrystals(),2008,37(4):9732976[7]WangHuichun,WuChengyuan,ChungChinchun,LaiMinghong,ChungTsairwang1Analysisofparametersandinteractionbetweenparametersinpreparationofuniformsilicondioxidenanoparticlesusingresponsesurfacemethodology1MaterialsandInterfaces,2006,45(24):804328048[8]YangXiuzao().Studyonsynthesesofparticleoftheamorphoussilicawithaverageparticlediameter(D)15nm1InorganicChemicalsIndustry(),2000,32(4):325[9]LiYong(),FengZongyu(),XueXiangxin(),QiaoGuibo().Comparisonofpreparationofprecipitatedsilicaoilshaleashandalkalidissociation1BulletinoftheChineseCeramicSociety(),2008,27(1):6211[10]WuYuan(),ChenYu().Preparationofultra2finewhitecarbonblackinsubmergedcirculativeimpingingstreamreactor1JournalofChemicalIndustryandEngineering(China)(),2003,54(10):138121386[11]HeKai(),ChenHonggang().Preparationofwhitecarbonblackwithlime2kilngasbycarbonization1TheChineseJournalofProcessEngineering(),2006,6(4):5542559[12]HuQingfu