\r' iRII916s1 PLEASEDONOTREM.OVEFRCM.LIBRARY BureauofMinesReportofInvestigations/1988 Preparationof AmmoniumParatungstate FromaSodiumTungstate-Sodium ChloridePhase ByA.E.Raddatz,J.M.Gomes,andT.G.Carnahan g,. S. Department of theIntenor., Bureauof Mines SpokaneResearchCenter East315Montgomery Avenue Spokane,WA99207 UNITEDSTATESDEPARTMENTOFTHEINTERIOR Report of Investigations 9165 Preparationof AmmoniumParatungstate FromaSodiumTungstate-Sodium ChloridePhase ByA.E.Raddatz,J.M.Gomes,andT.G.Carnahan UNITEDSTA"rESDEPARTMENTOFTHEINTERIOR DonaldPaulHodel,Secretary BUREAUOFMINES DavidS.Brown,ActingDirector LibraryofCongressCataloginginPublicationData: Raddatz,A.E.(AndreaE.) Preparation of ammonium paratungstate fromasodium tungstate-sodiumchloridephase. (Reportof investigations;9165) Bibliography. Supt.of Docs.no.:I28.23: 9165. 1.Ammonium paratungstate. 2. Tungsten-Metallurgy. 3.Solvent extraction. I.Gomes, J.M.(John M.) II.Carnahan, T.G.(ThomasG.) III.Title.IV:' Series: Report of investiga tions(UnitedStates.Bureau of Mines); 9165. TN23.U43[QD181.W1]622s[669'.734]87-600413 CONTENTS Abstract... ... ... .... ........ ....... .. ...... ......... ..... . ......... ............. ..... . ..1 Introduction ............................................................ .,... .... .... ..2 Acknowledgment .............................................. , .................... .,3 Materialsandexperimentalprocedure...........................................3 Resultsanddiscussion...........................................................5 Conclusions...... .. .. ... .... .... ... .. ... ..... ... .. .. . .. ..... . . ..... ... .. .... .. . ..8 Appendix ............................. -.... --...................................9 ILLUSTRATIONS 1.Tungstenproductionfromscheeliteandwolframiteconcentrates...........2 2.ProposedflowsheetforsolventextractionprocesstorecoverAPTfrom wolframiteviahigh-temperaturemolten-saltextraction..................3 3.Tungstenextractionfromsyntheticsolutionasafunctionoftime........5 4.Tungstenextractionfromactualhalidesolutionasafunctionoftime....5 5.EqUilibriumdiagramforextractionoftungstenwithPrimeneJM-T.........6 6.Combinedcrossflow-countercurrentflowsolventextractioncircuit........7 1. 2. 3. 4. 5. A-I. A-2. A-3. A-4. TABLES Analysisofwolf rami teconcent rate Compositionofdilutedpregnantquench-leachingsolutionforsolvent extraction .................... ,.............. tI Tungs tenbala nee ........................... 1'1 ,. Tungstenextractiontotheorganicphaseincombinedcrossflow-counter-currentflowsolventextractionsystematphaseratioof0.5 , AnalysesofBureauofMinesandcommercialAPT Analysesofsilicatephasesofwolframiteconcentratestreatedbythe high-temperaturemolten-saltextractiontechnique Reagentsusedinleachingsilicatephaseandextraction Analysesofwolframiteprocessingresidues Summaryofreagentsusedandcompositeextractionresultsfromleaching 4 4 6 7 7 9 9 10 wolframiteresidues.....................................................10 UNITOFMEASUREABBREVIATIONSUSEDINTHISREPORT CdegreeCelsiusminminute ggrammLmilliliter giLgramperliterpctpercent hhourvolpctvolumepercent Lliter PREPARATIONOFAMMONIUMPARATUNGSTATE FROMASODIUMTUNGSTATE-SODIUMCHLORIDEPHASE EJyA.E.Raddatz,1J.M.Gomes,2andT.G.Carnahan3 ABSTRACT PreviousBureauofMinesresearchhasshownthattungstenorescon-t_ainingaslittle as40pctW032- canbeprocessedbyahigh-temperature molten-saltextractiontechniquetoproduceatungstate-bearingsodium chloridephasewith99pctW recoveryandlittleimpuritycontamination. Theobjectiveofthisworkwastodemonstratethatthetungstate-bearing sodiumchloridephasecanbeasuitablefeedmaterialforpreparingam-moniumparatungstate(APT)byamodificationtothepresentindustrial solventextractionprocess.Acombinedcrossflow-countercurrentflow solventextractiontechniquetoextracttungstenispresented.APTpro-ducedbythisnewtechniquecontained88.6pctW032- andthefollowing impurities,inpercent:Mn02_0.0007,Mo020.017,P205