用钙、镁和锑深度除铋

鬻觐链翱 Availableonlineatwww．sciencedirect．com ．一●● ··：，ScienceDirect Trans．NonfeITOUSMet．Soc．China21(2011)2311—2316 Transactionsof Nonfc!rrousMetals SocietyofChina WWW．tnmSC．cn Finedebismuthizingwithcalcium，magnesiumandantimony LUDian—kunl，JINZhe．nan’，JIANGKai．xi2 1．SchoolofMaterialsandMetallurgy,NortheasternUniversity,Shenyang110819，China； 2．BeijingGeneralResearchInstituteofMiningandMetallurgy,Beijing100044，China Received30October2010；accepted27May2011 Abstract：Inordertoachievefinedebismuthizingofleadbullion，theeffectsoftemperature．addingamountofcalciumand magnesiumandantimonyonthebismuthremoraJfrom】cadbullionwereinvestigated．Themechanismofdebismuth／zingwasalso discussed．Theresultsshowthatwhenaddingamountsofcalciumandmagnesiumreach0．1l2％and0．395％．respectively,bismuth levelof0．001％(massfraction)inthefinalleadisachievedat330oC，withouttheneedforantimonyaddition．Maintainingaddition amountofmagnesiumat0．155％，whencalciumadditionamountislessthan0．09％，theconcentrationofperitecticreactionpoint．the bismuthconcentrationcanbeeasilydecreasedto0．001％bvthefollowingantimonytreatment．Butthee行ectofantimonytreatment ondebismuthizinggetsbadifthecalciumadditionexceeds0．09％． Keywords：debismuthizing；／(roll—BeUeaonprocess；antimonytreatment；peritecticreaction 1Introduction Mostofthealkaliandalkalineearthmetalscan formintermetalliccompoundswithbismuth，andthe reactionsareoftenusedforthedebismuthizingoflead bullion[卜3】，buttheKroll—BeRerton(K-B)processwith calciumandmagnesiumreagentsistheonlypractical processin operationforpyrometallurgicaibismuth removal[4]．Historically,thiswasdonebyaddingpure magnesiumingotsandcalciumcrownorturnings．Lately, anewgenerationofdebismuthizingreagentcomprisedof magnesium-calciumalloywasdeveloped[5]．Butthe mechanismofdebismuthizingretainsunchanged．Onthe mechanismofbismuthremovalfromlead．BETTERToN andLEBEDEFF[6]suggestedthatitresultedfromthe formationofbothCa3Bi2andM93Bi2compounds accordingtothemicroscopicstudyandcalculation， whileEVERSf71believedthatit resultedfromthe formationofCaMg，Bi，．The1atteropinionhasbeen acceptedbyamajorityofresearchers[8—11]．DAVEY [12]summarizedthethermodynamicrelationshipsthat governtheremovalofbismuthfromleadbytheK—B process．TheremovaIofbismuthfromIeadbullionis governedbythereaction，asshowninthefollowing reaction： 2Mg+Ca+2Bi2M92CaBi2 (1) Thesolubilityrelationnearthefreezingpointofthe leadcanbeapproximatelyrepresentedby： lg([Mg]1ca][B∥)=一7．37 (2) ILEYandWARD[9】obtainedthesolubilityproduct ofthemagnesium，calciumandbismuthinleadbullion within322—350。C，asshowninEq．(3)．HANCOCK andHARRIS[10]gotanotherrelation，asshownin Eq．(4)． 19([Mg]1ca][B矿)=5．46～7560／T(3) lg([Mg]2[Ca】[Bi]2)=12．007—11437／T (4) Itcanbeseenapparentlythatthedifferentresultsof solubilityofCaM92Bi，inlcadareobtainedbydifferent researchers．Inaddition．BETTERTONandLEBEDEFF [6]claimedthatwhenusingantimonytreatment，itwas possibletoreducebismuthtolessthan0．001％f61．but DAVEY『81doubtedthisresult． Astothemechanismofbismuthremovalwith antimony,BETTERTONandLEBEDEFF[6】suggested theformationofaquaternaryCa．Mg．Bi．Sbcompound． DAVEY[8】suggestedthatcalciumandmagnesium antimonidesprecipitatedtohelpfloatingouttheresidual smallbismuthidecrystals．ILEYandWARD[9]thought Correspondingauthor：LUDian·kun；Tel：+86．24—83681319；E—mail：ludk@smm．neu．edu．cn DOI：10．1016／S1003·6326(11)61013-3 万方数据 2312 LUDian-kun，etal／Trans．NonferrousMet．Soc．China21(2011)231卜2316 thattheformationoftheinsolubleantimonidescauses thecoprecipitationand／orpost—precipitationof bismuthides． Asstatedabove．thereisstillgreatdifferenceinthe effectsofcalciumandmagnesiumadditionand temperatureonthelevelofbismuthremoval．andthereis stillargumentintheactionofantimonytreatment．In additiontotheseproblems．mostoftheleadalloysused forpreviousresearchworksareofrelativehighbismuth concentrations．i．e．bismuthcontentinprimary1cad above0．1％(massfraction)．whichisdisadvantageousto theresearchondebismuthizingmechanism． Thisstudyfocusesonunderstandingtheinfluence ofcalciumandmagnesiumadditionandtemperatureon debismuthizinglevelfromleadbullion．especiallyfrom theleadalloyswithlowbismuthconcentration．The mechanismofantimonytreatmentfollowingtheK．B processonthefinebismuthremovalisalsoinvestigated． 2Experimental Lead．bismuthalloywaspreparedbytheadditionof bismuthwith99．99％purityintoasteelpotcontaining about15kgmoltenleadwith99．99％purityat450。C， thenalead．bismuthalloy饵i0．023％inmassfraction) wasobtained．Calciumwasaddedaslcad．calciumalloy (Ca1．36％1andmagnesiumwasaddedasmagnesium piecewith99．99％purity． Allexperimentswereconductedinasealedvertical tubularcrucibleelectricfurnaceundertheprotectionof nitrogenatmosphere．Foreachtest．500gpreparedPb—Bi alloywasfirstlymeltedinaceramiccruciblewhile Pb—Caalloyandmagnesiumpieceswerehungbysteel wireinthefumace．Whenthetemperaturereached400 oC，Pb．Caalloyandmagnesiumwereaddedwithstirring intothemoltenalloy．Thetemperaturewasmaintainedat 400。Cfor10minandthencooledatarateof5。C／hto thedestinationtemperature，330oC，exceptfor temperaturedependenttests．AfterkeepingwaFITIatfinal temperaturefor4h，thedrosswasfishedoutwitha stainlesssteelnetandhungoverthecruciblefor15min toremoveextracontaminatedleadalloy．Theseparated alloyswereweighedandsampledtoICP．AESanalysis． Apartofthemwerealsotreatedwith0．07％fmass fraction)ofantimony 3Resultsanddiscussion 3．1Ef亿ctoftemperatureonbismuthremoval Alltestsinthisbatchhadthesameinitial concentrationsofbismuth，magnesiumandcalcium， whichwere0．0211％．0．155％and0．112％．respectively． Thefinalcoolingtemperaturewasarrangedbetween330 。Cto363oC．asshownin1'able1．Theexperiments resultsarealsosummarizedinT曲le1． ThedatainTablel showthatlittleCaM92Bi， formedabove352oCunderthepresentworkconditions． Themajorityofthedebismuthizingreactionoccurred between34l。Cand352oC．onlyalittleofextrabismuth wasremovedbelow34l。C．Thedrossratioisalsoin accordancewiththedebismuthizinglevel．Thereisalot ofdrossproducedat363oC．atwhichalmostnobismuth is removed．whilecalciuminfinalleadreduces significantly．Thedrossathightemperaturemaybe regardedasCa3M94Pbx，whichisamixtureofCaPb3and M92Pb，accordingtoPb-Ca-Mg-Biphasediagram[12]． Thecalculatedcompositionofthedrossat363。Cis Ca3M9362Pb4908，inwhichthePbcontentiSwellabove theratioofbothCaPblandMg，Pb．Itmeansthatthe drossisamixedsolidsolutionofCalM94Pbxandfinal lead．Thissituationcontinuestothelowertemperatures． TheapparentsolubilityproductofCaM92Bi2changes significantlywithtemperaturefrom34l。Cto352。C． butthesolubilityproductdifferenceat330。Cand341 oC．aswellas352。Cand363。C．isrelativelysmall．The aDparentvaluesofsolubilityproductbelow341 oCare abouttwicethatcalculatedbvDAVEYneartheliquidus 【11】．Itmeansthatthefinedebismuthizingresultcan onlybeachievedneartheliquidus，althoughthemajority ofbismuthhasbeenalreadyremovedatabout341。C． 3．2Effectofmagnesiumadditiononbismuthremoval Duringthisbatchofexperiments．theinitialcalcium concentrationwasmaintainedat0．112％andthefinal temperaturewas330oC．Othersexperimentalconditions andtheanalysisresultsoffinalleadalloyarelistedin Table2． Table1 Initialconditionsandanalysisoffinalleadalloyintemperaturedependenttests Finalmassfraction／％ No．Temperature／。CDrossratio／％—————————————————————————————— Ca Mg Bi [Ca】[Mg】2[Bi】2 A1 A2 A3 330 341 352 12．83 12．22 10．32 0．076 0．073 0．104 0．134 0．126 O．136 0．008 0．009 0．019 8．73x10—8 9．39x10—8 6．94×10—7 A4 363 6．41 0．093 0．146 0．021 8．74x10—7 万方数据 LUDian—kun．etal／Trans．NonferrousMet．Soc．China21(2011)231卜2316 2313 FromT，山le2itcanbeseenthatthefinalBicontent decreasedcontinuouslywiththeincreaseofmagnesium addition．Whentheinitialmagnesiumaddedcomeupto 0．395％．thebismuthcontentinleadalloydroppedto only0．001％．muchlowerthan0．0025％，whichis estimatedfromPb．Ca．Mg—BiphasediagrambyDAVEY f81。andtheconcentrationofmagnesiumleftinleadis alsowellbelow1％．Thefinalmagnesiumconcentration inleadalwaysincreasedwiththeadditionofmagnesium， butcalciumconcentrationinfinalalloytookaslow increasingtrendandfinallyheldatapproximately0．08％． ThecalculatedapparentsolubilityofCaM92Bi2is smallerthanthatfromEqs．(2)一(4)． 3．3Effectofcalciumadditiononbismuthremoval Alltestsinthisbatchheldaninitialmagnesium concentrationof0．155％．Theotherconditionsand analysisoffinalleadalloyarelistedinTable3．Thefinal bismuthconcen仃ationsill1‘able3showadownward trendwiththeincreaseofinitialcalciumaddition．But anomalousresultsoccurredforNo．C12andCl3．By carefullyrepeatingthetwotests，theresultremainstobe asametrend．Theseanomalousphenomenamayhave somethingtodowithPb—Caphasediagram．Figure1 showsthePb．Caphasediagramadoptedby BETTERTONandLEBEDEFF[6]．Incontrastwimthat providedbyotherreferences『13～14]，thereisaperitectic point刀situatedatapproximatebv0．09％ofcalciumin theenlargementofthePb．richcomerinFig．1． ThepointBissituatedatapproximate0．075％of calciumconcentration．CaPblwillgraduallyseparateout fromleadalongwiththedecreaseoftemperaturewhen calciumcontentexceeds0．075％．andthecalciumleftin leadapproachesto0．075％littlebylittlealongline彳曰． TheseparatedCaPblduringcoolingprocesswillreact withliquidleadtofcIITllsolidsolutionnearthefreezing Table2Initialconditionsandanalysisresultsoffinalleadalloyinmagnesiumdependenttests No．—坐堕竺堕坐堂竺一Drossratio慌——里些竺堕型型丝一[Ca][Mg]2[Bi】2一 ／％—— 【Ca儿M刮‘【BlJ‘Bi Mg Ca Mg Bl————————●—_●_-__—————————————————-————————————————————____——————-___————————————_______---_——————————————___-————————————————————————————————————————一。B5 O．0211 0．103 8．45 0．072 O．090 0．007 2．86x101B6 B7 B8 0．0211 O．021O O．0210 0．170 0．251 0．313 13．12 14．20 14．45 0．072 0．078 0．082 0．136 0．206 0．247 0．005 0．003 0．002 3．33x10—8 2．98x10—8 2．00x10—8 B9 0．0210 0．395 14．58 0．076 0．321 0．001 0．78×10—8 Table3Initialconditionsandanalysisresultsoffinalleadalloyincalciumdependenttests ．些!竺些型竺!墅一Drossratio／％No——旦坐竺鱼堂咝一[ca】[Mg】2[BtBi。12]．—— 一 [Ca儿T诅gJ。‘Bi Ca Ca Mg BiC10 0．0233 0．040 4．05 0．036 0．124 0．011 6．70x101C11C12 C13 0．0219 0．0215 0．0211 0．065 0．089 0．112 5．09 6．88 8．02 0．061 0．070 0．076 0．126 0．132 0．134 0．010 0．007 0．008 9．68x10—8 5．98x10—8 8．73x10—8 C14 0．0207 0．135 9．02 0．077 O．134 0．005 3．46x10—8 U ■ 2 皇 矗 。 厶 g o — Calciummassfraction／％ Fig．1Pb—Caphasediagram(a)andPb—richregion(b) 芝300 ： 砖 △ g 占200 100 (b) 爿 B／一，—一。 0 0．05 0．10 0．15 Calciummassfraction／％ 万方数据 2314 LUDian-kun，etal／Tmns．NonfermusMet．Soc．China21(2011)23ll一2316 point．Sowhentemperaturedecreasestoa_bOutfkezing point，partoftheseparatedCaPb3willre—dissolveinto lead． BecauseCaM92Bi2separatesouttogetherwim CaPb3duringthelastperiodofcoolingprocess，the activityofCaM92Bi2in drossis reducedand debismuthizingeffectgetsreinforced．Butwhenthe peritecticreactionoccurs，panoftheseparatedCaPblis consumedandthelastdrosstouchingwithmoltenlead willbelackofCaPb，．Thisresult，onareversetum，wiU increasetheCaM92Bi2activnyindross．Thusthe distributionbalanceofbismuthbetweendrossand moltenleadisbroken，andpartofthef撕nerbseparated CaM92Bi2re—dissolVesintolead，resultinginapoor debismuthingefrect．Thissituationoccum珂inallthe lastt11reeexperiments，Nos．C12，C13andC14． ForNo．C12．theinitialcalciumcontentisO．089％． iustalittleabovepointB．Underthiscalciumcontent conditions，CaM92Bi2isseparatedoutaloneduringthe mosttimeofcoolingprocess，onlyalittleofCaM92Bi2is separatedouttogetherwithCaPb3inaverynarrow temperaturemgeinthelastperiod．Sotheactivityof CaM92Bi2inthelatterpartofdrossgetssmallto reinforcedebismuthizinglevel．Whentheperitectic reactionoccurs，onlyalittleofdrosstakespartinthe reaction．Sothere-diss01vedCaM92Bi2isverylittleand thefinalbismuminleadremainsatalowlevel．Butfor No．C13。theinitialcalciumcontentis0．112％．whichis moreabovepointB．Sothealloytouchesliquiduslineat arelativehightemperature．CaPb3is separatedout togetherwithCaM92Bi2atarelatiVelyearlytimeduring coolingprocess．Therefore，arelativelylargeamountof CaM92Bi2andCaPb3coexistinthelatterdross．When meperitecticreactionoccurs，alargeramountofdross takespartinthereactioncomparedwithNo．C12，and moreCaM92Bi2isfornledbeforere．dissolvingtolead． Asaresult．mefinalbismumlevelinNo．C13isalittle higherthanmatinNo．C12．AstoNo．C14，theinitial caIciumconcentrationis0．135％．whichisalsoabove point日．LiketheNo．C13，themoltenalloVofNo．C14 touchesliquidusatahightemperature，andmostofme CaM92Bi2isseparatedouttogetherwithCaPb3during theearlytimeofcoolingprocess．Althoughthereisa la唱eamountofdrosstakingpartintheperitectic reactionduringtheendcoolingprocessandpanofthe CaM92Bi2indrossre—diss01vedintolead，thereis adequateCaPb3stillleRindrosstolowermeactivityof CaM92Bi2toarelativelylowlevel．Soasatisfactory debismuthizingresultcanalsobeachieved． 3．4Effectofantimonyt化atmentondebismuthizing Inthisbatchoftest，allfinalleadalloysobtained f}ompreViouscalciumandtemperaturedependenttests weren‘eatedwithO．07％ofantimony-Amongthese antimonytreatmenttests，finalleadalloysobtained行om calciumdependenttestsweretreatedat330oC；however’ those行omtempemturedependenttestsweretreatedat theiroriginaldebismuthizingtemperatures．Theinitial conditionsandfinalresultsofthetwogroupoftestsare summa打zedinto1'able4andT{lble5，respectively． 3．4．1Ef{．ectofinitialcalciumconcentmtiononantimonv treatment ThedatainTable4showthatalmostalltheadded antimonV20esintodross．Theinitialcalciumaddition hasadif诧renteffectonantimonytreatmentdepending onwhetheritisaboveorbelowthecalciumcontentof DointB．Whentheinitialcalciumadditiondoesnotreach pointB，thebismuthleRinleadislowerthan0．00l％ aRerantimonvtreatment．However_whentheinitial calciumadditionexceedspointB。debismuthizinge仃bct graduallygetsbadwiththeincreaseofinitialcalcium addition，andthebismuthcontent1eRinleadishighman 0．00l％．W11enmeinitialcalciumadditionreaches 0．135％． antimonv仃eatmenthasno effecton debismuthizinglevel．Theseresultsimplythatthe Deritecticreactionhasaremarkableinhibitioneff．ecton debismuthizinglevelbyantimony仃eatmem． Calciumandmagnesiumcanfo瑚bothbinaryand temaryintenTletalliccompoundswithantimonyf15—171． AccordingtothereportofILEYandWARD[9]，calcium andmagnesiumconcentrationswerereducedtotheir finallevelsshortlvaRert11eadditionofantimonv．Butthe bismuthconcentrationthencontinued白of．allwim additionalstirring．Thesef-actsmeanthattheinnuenceof antimonytreatmentondebismumizingappearsunlikely toactasthe凡nctionofphysicalc01lectionofresidual CaM92Bi2inleadbyM93Sb2andCaM92Sb2．Itcanbe hypothesizedthataUofthere．dissolvedbismuthduring peritecticreactionpresentsasthecompoundCaM92Bi2 infinallead：however．fbrthosetestsinwhichno peritecticreactionoccurs，mostofbismuthinfinallead arek印tinbismuthatom．Whenalargeamountof CaM92Sb2f．onnandarenoatedrapidlyuptothesurface ofleadbatch，theantimonyactivitvinleaddropstoa verylowvalue．SOtheresidualf．reebismuthatomcan substitutetheantimonVsiteandgoesintodrossd嘶ng continuedstirring．ThishypothesismaygiVea11 interDretationoftheresultsofantimonvtreatmenton bismuthremovalwithdiff．erentinitialcalciumcontent． 3．4．2Eff．ectoftempemtureonantimony仃eatment FromT曲le5 itcanbefoundthattheantimonv treatmentcanremovebismuthtoalowleveleveIlata relativehi曲temperature．However’mebismuth concentrationleRinleadislackofregularity．Almostan theaddedantimonygoesintodmss，resultingiIlalarge amountofdross．Thetemperatureofantimony treatmenthasnoperceptibleinnuenceonthedross 万方数据 LUDian—kun，etal／Trans．NonferrousMet．Soc．China21(2011)2311—2316 2315 "Irable4Testconditionsandresultsofinitialcalciumconcentrationonantimonytreatment Initialmassfraction／％ Finalmassfraction／％ No Drossratio／％ Ca Bi Ca Mg Bi Sb !垒垒!!苎!!坠!旦呈垒!!!竺翌!竺璺!!!竺!坐竺!!!竺2111坐12翌呈坐!翌竺里兰坚!!翌!坐 Initialmassfraction／％ Finalmassfraction／％No．Temperature／。C——Drossratio／％————————————————————————————————————一 Ca Bi Ca Mg Bi Sb orelductionbetween330oCand363。C． Becausetheinitialcalciumadditionwasfixedat 0．112％inpreliminarydebismuthizingtests(Table1．No． A1toA41。whichisabovethepointB，allthealloysused inthisbatchtestshadthechancetoexperiencethe peritecticreaction．Buttheextentsofperitecticreaction differedatdifferentendcoolingtemperatures．Thealloy usedinNo．E20．whichwascooledat330。C。would haveexperiencedmoreperitecticreactions，resultingin moreCaM92Bi2tore．dissolveintothefinallead．This willleadtoapoorbismuthremovalresultduringthe followingantimonytreatment．ThebismuthlevelofNo． 20onlydroppedfrom0．008％to0．004％afterantimony treatmentat330oC．Asforthetestat341。C．alarge amountofbismuthhavebeenremovedduring debismuthizingbycalciumandmagnesium，andno peritecticreactionoccurredbefore．So，mostofthe residualbismuthinlcadmaypresentasbismuthatom whichisreadilycarriedoutbyM93Sb2andCaM92Sb2． TheresultsoftheNo．E21 agreewellwithhypothesis． thebismuthconcentrationfallsfrom0．009％to0．001％ afterantimonytreatment．Comparedwiththealloyused intestat341。C．onlylittlebismuthinalloyusedat352 。Chasbeenremovedbycalciumandmagnesium，and thesolubilityofCaM92Bi2ishigherthanthatat341 oC． Therefore．thebismuthlevelonlydecreasedfrom 0．019％to0．007％fortheNo．E22．Totestat363。C．the originaldebismuthizingreactionwithcalciumand magnesiumhasbeenverylimited．mostofthebismuthin lcadpresentedasbismuthatomandlessCaM92Bi2 formed．Therefore，theantimonytreatmentexhibited betterresultthanthatat352。C．andthebismuthlevel fellfrom0．021％to0．006％ 4Conclusions 1、Theinfluenceofcalciumadditionon debismuthizingis complicatedduetotheperitectic reaction．Whenthecalciumadditionisnearthecalcium concentrationofperitecticreactionpoint．alittle disturbancetothedebismuthizinglevelcanbeexpected． 2、Debismuthizingwithcalciumandmagnesium alonecallreachthelevelof0．001％Biinfinalleadat 330。C，andthecorrespondingcalciumandmagnesium concentrationsleftinthefinallcadare0．076％and 0．32l％．respectively． 3、Whentheinitialbismuthconcentrationinlcadis 0．021％．majorityofthedebismuthizingreactionwith calciumandmagnesiumoccurbelow352oC：nobismuth canberemovedabove363。C． 4、Whenthecalciumadditionislessthanthe calciumconcentrationofperitecticreactionpoint，the bismuthconcentrationcanbedecreasedto0．001％easily bythefollowingantimonytreatment．Ahighamountof calciumaddedinthelcadmayhasanegativeeffecton theantimonytreatmentforfurtherdebismuthizing． 5)Antimonytreatmentappearsunlikelytoactasa physicalcollectionforCaM92Bi2．Theprobably mechanismisthattheaddedantimonyformsCaM92Sb2 compoundandthebismuthinthelcadisfurtherremoved bypartialsubstitutionofSbwithBi．Sotheantimony treatmentcanonlyremovefreebismuthatomsbuthas littleeffectontheremovalofCaM92Bi，． 万方数据 2316 References 【2】 【3】 【4】 【5】 【6】 【7】 [8】 【9】 LUDian-kun，etal／Trans．NonferrousMet．Soc．China21(2011)231卜2316 【10】HANCOCKP’HARRISR．Solubilityofcalcium·magnesium- bismuthintermetallicinmoltenlead【J】．CanadianMetallurgy Quarterly，1991，30：275—291． JOLLIVETLEquilibriainsystemsrichinleadandcontainingalkali andalkalineearthmetals[J]ComptesRendus，1949，228：1495． CHENGuo—fa．Leadmetallurgy【M】．Beijing：MetallurgicalIndustry Press．2000：126-127．(inChinese) XINHX，QINXY，ZHUXGZHANGJ，KONGMGFabtication ofnanocrystallineM93X2(X=Bi，Sb)withsupersaturatedsolid solubilitybymechanicalalloying【J】．MaterialsScienceand 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