Method to upgrade titania slag and resulting productUGS.docx
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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
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