Method to upgrade titania slag and resulting productUGS.docx

Method to upgrade titania slag and resulting productUGS.docx

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MethodtoupgradetitaniaslagandresultingproductUGS

Methodtoupgradetitaniaslagandresultingproduct

UnitedStatesPatent

5,830,420

Borowiec, etal.

November3,1998

Abstract

Amethodisdisclosedincluding:

（a）sizingatitaniaslagtoaparticlesizerangeoffrom75micronsto850microns;（b）oxidizingthesizedtitaniaslagbycontactingthesizedtitaniaslagwithanoxygencontaininggasatatemperatureofatleastabout950.degree.C.foraperiodofatleastabout20minutessuchthatasubstantialportionoftheironoxideisconvertedtoaferricstate,suchthatthereducedtitaniumoxidesareconvertedtoatetravalentstate,andsuchthatatleastamajorportionoftheglassysilicatephaseisdecomposed;（c）reducingtheoxidizedtitaniaslaginareducingatmosphereatatemperatureofatleastabout700.degree.C.foraperiodofatleastabout30minutessuchthattheferricstateironoxideisconvertedtoaferrousstate;（d）leachingthereducedtitaniaslagwithmineralacidatatemperatureofatleast125.degree.C.andunderapressureinexcessofatmosphericpressuretoyieldanupgradedleachedslagproductandaleachate;and（e）washingandcalciningtheupgradedleachedslagproductbyheatingatatemperatureintherangeoffrom600.degree.C.to800.degree.C.ThemethodprovidesadvantagesinthatitcanbeusedtoproduceaproductwithhighTiO.sub.2contentthatissuitableforthechlorideprocessofTiO.sub.2pigmentproduction.

Inventors:

Borowiec;Krzysztof（Tracy,CA）;Grau;AlfonsoE.（St-Bruno,CA）;Gueguin;Michel（Tracy,CA）;Turgeon;Jean-Fran.cedilla.ois（Tracy,CA）

Assignee:

QIT-FeretTitaneInc.（Quebec,CA）

Appl.No.:

561602

Filed:

November21,1995

CurrentU.S.Class:

423/69;423/74;423/82;423/86

Intern'lClass:

C01G 023/00;C22B 034/10

FieldofSearch:

423/86,82,74,69

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PrimaryExaminer:

Bos;Steven

Attorney,AgentorFirm:

Nilles&Nilles

Claims

Whatisclaimedis:

1.AmethodtoupgradeatitaniaslagtoobtainahighTiO.sub.2-containingproducthavingresidualimpuritycontentandgrainsizedistributionsuitableforuseasafeedstockinachlorideprocessoftitaniumdioxidepigmentproduction,saidtitaniaslagcontainingreducedtitaniumoxidesandimpuritiesincludingatleastonememberselectedfromthegroupconsistingofironoxide,manganeseoxide,chromiumoxide,vanadiumoxide,aluminumoxide,siliconoxideandalkaline-earthoxides,saidatleastonememberbeingdistributedinapseudo-brookitephaseandaglassysilicatephase,themethodcomprising:

（a）sizingthetitaniaslagtoaparticlesizerangeoffrom75micronsto850microns;

（b）oxidizingthesizedtitaniaslagbycontactingthesizedtitaniaslagwithanoxygencontaininggasatatemperatureofatleastabout950.degree.C.foraperiodofatleastabout20minutessuchthataportionoftheironoxideisconvertedtoaferricstate,suchthatreducedtitaniumoxidesareconvertedtoatetravalentstate,andsuchthatatleastamajorportionofaglassysilicatephaseisdecomposed;

（c）reducingtheoxidizedtitaniaslaginareducingatmosphereatatemperatureofatleastabout700.degree.C.foraperiodofatleastabout30minutessuchthattheferricstateironoxideisconvertedtoaferrousstate;

（d）leachingthereducedtitaniaslagwithmineralacidatatemperatureofatleast125.degree.C.andunderapressureinexcessofatmosphericpressuretoyieldanupgradedleachedslagproductandaleachate;and

（e）washingandcalciningtheupgradedleachedslagproductbyheatingatatemperatureintherangeoffrom600.degree.C.to800.degree.C.

2.Themethodofclaim1whereintheresultingupgradedslagproductcontainsatleast90%byweightoftitaniumdioxideandlessthan1%byweightofmagnesiumoxideandlessthan0.2%byweightofcalciumoxide.

3.Themethodofclaim1whereinthealkaline-earthoxideimpuritiescontainedinthetitaniaslagcomprisemagnesiumoxideandcalciumoxide.

4.Themethodofclaim2or3whereinthetitaniaslagcontainsatleast3%byweightofironoxides.

5.Themethodofclaim4whereinsaidtitaniaslagcontainsatleast1%byweightofmagnesiumoxideandatleast0.2%byweightofcalciumoxide.

6.Themethodofclaim1whereinpriortostep（b）,thetitaniaslagispreheatedtoimproveperformanceofstep（b）andstep（b）isconductedinafluidizedbedreactor.

7.Themethodofclaim1whereinstep（b）isconductedinafluidizedbed.

8.Themethodofclaim7whereinstep（b）isconductedatatemperaturerangeoffromabout1000.degree.C.to1100.degree.C.

9.Themethodofclaim7whereinstep（b）isconductedforaperiodofbetween1and2hours.

10.Themethodofclaim7whereinafluidizinggascontainsinexcessof2%oxygen.

11.Themethodofclaim1whereinstep（c）isconductedusingareducingagentthatincludesatleastonememberselectedfromthegroupconsistingofcarbonmonoxide,hydrogengas,smeltergas,reformednaturalgasandcoal.

12.Themethodofclaim11whereinstep（c）isconductedinafluidizedbedreactoratatemperaturerangeoffromabout700.degree.to900.degree.C.

13.Themethodofclaim12whereinstep（c）isconductedatatemperaturerangeofabout800.degree.to850.degree.C.

14.Themethodofclaim13whereinstep（c）isconductedforaperiodofabout11/2to2hours.

15.Themethodofclaim1whereinstep（d）isconductedatatemperaturerangeof140.degree.to160.degree.C.,underagitationandatapressureofatleastabout50psi.

16.Themethodofclaim15whereinstep（d）isamultiplestageleachingoperation.

17.Themethodofclaim1whereinsaidmineralacidincludesatleastoneacidselectedfromthegroupconsistingofsulfuricacidandhydrochloricacid.

18.Themethodofclaim17whereinstep（d）isasinglestageleachingoperation.

19.Themethodofclaim17whereinstep（d）isatwostageleachingoperation.

20.Themethodofclaim17whereinthemineralacidispresentinatleasta10%stoichiometricexcessofwhatisneededtoconvertleachableoxidesandalkaline-earthimpuritiestosolublechlorides.

21.Themethodofclaim20whereintheconcentrationofmineralacidisatleastabout15%byweightandstep（d）isconductedatapressureofatleast40psig.

22.Themethodofclaim21whereintheconcentrationofmineralacidisabout20%byweightandstep（d）isconductedatapressureoffrom50psigto70psig.

23.Themethodofclaim1whereinstep（e）comprisesthesequentialstepsofseparatingtheupgradedleachedslagproductfromtheleachate,washingtheupgradedleachedslagproductwithwater,dryingtheupgradedleachedslagproductandthencalciningsaidupgradedleachedslagproduct.

24.Themethodofclaim15whereintheleachingisconductedatatemperatureofabout150.degree.C.

25.Themethodofclaim24whereinthereducedtitaniaslagiscontactedwiththemineralacidforatimeof3to7hours.

26.Themethodofclaim1conductedincontinuousmodeasacontinuousprocess.

27.Themethodofclaim1conductedinbatchmode.

28.Themethodofclaim1whereinstep（e）includesacausticleachingoftheupgradedleachedslagproductthatisconductedaftersaidwashingandpriortosaidcalcining.

29.Themethodofclaim28whereinsaidcausticleachingisconductedunderagitationandinbatchmode.

30.Themethodofclaim28whereinsaidcausticleachingisconductedunderagitationincontinuousmode.

31.Themethodofclaim29whereinsaidcausticleachingisperformedwithasodiumhydroxidesolutionatatemperatureofatleastabout50.degree.C.

32.Themethodofclaim30whereinsaidcausticleachingisperformedwithasodiumhydroxidesolutionatatemperatureofatleastabout50.degree.C.

33.Amethodoftreatingatitaniaslagtoobtainanintermediateproductincludingrutile,pseudo-brookiteandilmenite,saidtitaniaslagcontainingreducedtitaniumoxidesandimpuritiesincludingatleastonememberselectedfromthegroupconsistingofironoxide,manganeseoxide,chromiumoxide,vanadiumoxide,aluminumoxide,siliconoxideandalkaline-earthoxides,saidatleastonememberbeingdistributedinapseudo-brookitephaseandaclassysilicatephase,themethodcomprising:

（a）sizingthetitaniaslagtoaparticlesizerangeoffrom75micronsto850microns;

（b）oxidizingthesizedtitaniaslagbycontactingthesizedtitaniaslagwithanoxygencontaininggas