WO2018227237A1 - Procédé de production de cobalt et d'oxydes associés à partir de divers matériaux de charge - Google Patents

Procédé de production de cobalt et d'oxydes associés à partir de divers matériaux de charge Download PDF

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Publication number
WO2018227237A1
WO2018227237A1 PCT/AU2018/050569 AU2018050569W WO2018227237A1 WO 2018227237 A1 WO2018227237 A1 WO 2018227237A1 AU 2018050569 W AU2018050569 W AU 2018050569W WO 2018227237 A1 WO2018227237 A1 WO 2018227237A1
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WO
WIPO (PCT)
Prior art keywords
cobalt
aqueous solution
containing aqueous
solution
nickel
Prior art date
Application number
PCT/AU2018/050569
Other languages
English (en)
Inventor
Bryn Harris
Carl White
Original Assignee
Urban Mining Pty Ltd
Nmr 360 Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Urban Mining Pty Ltd, Nmr 360 Inc filed Critical Urban Mining Pty Ltd
Priority to KR1020197038887A priority Critical patent/KR20200059191A/ko
Priority to CN201880048086.1A priority patent/CN111278997A/zh
Priority to AU2018286479A priority patent/AU2018286479A1/en
Priority to JP2019569259A priority patent/JP2020523482A/ja
Priority to US16/621,282 priority patent/US20200109462A1/en
Priority to CA3066938A priority patent/CA3066938A1/fr
Priority to EP18816937.9A priority patent/EP3638819A4/fr
Publication of WO2018227237A1 publication Critical patent/WO2018227237A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0476—Separation of nickel from cobalt
    • C22B23/0484—Separation of nickel from cobalt in acidic type solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00—Obtaining manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates generally to methods for the production of cobalt and associated oxides from various primarily cobalt-bearing feed materials.
  • This process is also fundamentally pyrometallurgical, requiring a "low- temperature" (relative to smelting) roasting step combined with physical separation. Additional lithium hydroxide is then added to return the lithium content of the recovered cathode material to its original composition. It is not really a recovery process as such, but rather one of refurbishing the original component.
  • a method for the recovery of cobalt from a Co- and Ni-containing aqueous solution including: providing a Co- and Ni-containing aqueous solution having a pH of from about 4.5 to about 6.5 and an oxidation-reduction potential of from about 750 to about 900 mV as measured against a Pt-Ag/AgCI electrode; treating the Co- and Ni-containing aqueous solution with an amount of hypochlorite to oxidise and precipitate a portion of the cobalt to form a precipitate of CoOOH and to form a Co-lean Ni-aqueous solution; and separating the CoOOH from the Co-lean Ni-containing aqueous solution.
  • This process advantageously recovers cobalt in a trivalent state oxidation state as opposed to prior art processes which typically recover cobalt salts in the divalent state.
  • a cobalt product in the trivalent state is of particular economic value as it eliminates further processing steps, such as the oxidation of divalent cobalt, for applications that require cobalt in the trivalent state - particularly in electrochemical processes such as those in battery operation.
  • the Co- and Ni-containing aqueous solution is a chloride and/or sulphate solution.
  • the Co is in the form of a Co 2+ cation
  • the Ni is in the form of a Ni 2+ cation.
  • the amount of hypochlorite is a sub-stoichiometric amount.
  • the sub-stoichiometric amount of hypochlorite is sufficient to precipitate up to 90% of the cobalt as CoOOH.
  • the inventors have found that using a sub-stoichiometric amount of hypochlorite provides for a precipitate that is substantially pure CoOOH and substantially free of other metals. This high degree of purity is of particular importance as a number of applications, such as in electrochemical processes, demand high levels of purity if they are to be efficient.
  • substantially free of other metals it is meant that on a comparative basis, other metals (for example Ni) are present in the precipitate in an amount of 0.5 wt% or less in comparison with Co (based on elemental Co).
  • a preferred hypochlorite is NaOCI.
  • the method further includes: treating the Co-lean Ni-containing aqueous solution with an amount of hypochlorite to substantially oxidise and precipitate the remaining cobalt in the Co-lean Ni-containing aqueous solution as CoOOH and form a Co-barren Ni-containing aqueous solution; and separating the CoOOH from the Co-barren Ni-containing aqueous solution.
  • the pH of the Co- and Ni-containing aqueous solution is from about 5.0 to about 5.5.
  • the oxidation-reduction potential of the Co- and Ni-containing aqueous solution is from about 800-850 mV.
  • the step of treating the Co- and Ni-containing aqueous solution is conducted for a time of less than 2 hours.
  • the step of treating the Co- and Ni-containing aqueous solution is conducted for a time of at least 30 minutes.
  • the Co- and Ni-containing solution has a Co:Ni ratio of from about 100: 1 to about 1 : 10.
  • the Co:Ni ratio is less than or equal to about 5.
  • the method further includes a Ni-precipitating step including adding a precipitant to the Co-barren Ni-containing aqueous solution to precipitate nickel; and separating the nickel from the solution.
  • the precipitant is a carbonate.
  • the pH of the Co- barren Ni-containing aqueous solution is adjusted to a value of from about 7.5 to 8.5.
  • the Ni-precipitating step is conducted at a temperature of from 45-80°C.
  • the Co- and Ni-containing solution is substantially free of Cu,
  • the method includes: treating a precursor solution containing at least Mn, Co, and Ni with a precipitant to selectively form a Mn-precipitate; and separating the Mn-precipitate to form the Co- and Ni-containing aqueous solution.
  • the pH of the precursor solution is adjusted to a value of from about 3.5 to about 5.0.
  • the precipitant is a permanganate, and the permanganate oxidises the Mn to form a precipitate of Mn0 2 .
  • sufficient permanganate is added to adjust the oxidation-reduction potential of the precursor solution to a value of from about 700 to about 800 mV as measured against a Pt- Ag/AgCI electrode.
  • the precursor solution prior to treating the precursor solution with the precipitant, the precursor solution is treated to remove iron and copper.
  • Figure 1 Process flow diagram of an embodiment of the invention.
  • Figure 2 XRD spectrum of solids produced according to an embodiment of the invention.
  • Figure 1 provides a schematic representation of an embodiment of the invention for a method for the recovery of cobalt, manganese and nickel from a Co-, Ni- and Mn- containing aqueous feed solution.
  • the Co, Ni and Mn are present in the solution in ionic form.
  • the Co-, Ni-, and Mn-containing feed solution may be a sulphate and/or chloride based aqueous solution, in which case the Co, Ni, and Mn are present as sulphate and/or chloride salts and are in the form of Co(ll) Ni(ll), or Mn(ll) respectively.
  • the feed solution has been pre-treated to remove metal ions which may interfere with the recovery of cobalt from the Co-,Ni-, and Mn- containing aqueous feed solution to form a pre-purified feed solution 10.
  • metal ions include at least Fe and Cu.
  • Fe and Cu may be removed by methods known to those skilled in the art. Such methods may include precipitation with a base such as lime, electrowinning, solvent extraction or ion exchange.
  • the Co-,Ni-, and Mn- containing aqueous feed solution may be subjected to additional treatment steps to remove other metal ion contaminants if necessary.
  • the pre-purified feed solution 10 (being substantially free of Fe and Cu) additionally includes Mn ions (generally in the form of Mn(ll)).
  • Mn ions generally in the form of Mn(ll)
  • the inventors have found that Mn(ll) can be effectively removed in an oxidation/precipitation process that involves treating the pre-purified feed solution 10 with permanganate.
  • the pre-purified feed solution 10 is first adjusted 1 1 with caustic soda 12 to raise the pH to a value in the range of from about 3.5 to about 5.0, preferably from about 4.0 to about 4.5, and most preferably to a pH value of about 4.2.
  • Sodium permanganate 14 is then added in order to preferentially and selectively oxidise the divalent manganese in solution 10 and form a precipitate slurry 15 that includes a manganese dioxide precipitate 17.
  • oxidation-reduction potential (ORP) of the pre-purified feed solution 10 is added to adjust the oxidation-reduction potential (ORP) of the pre-purified feed solution 10 to a value of from about 700 to about 800 mV (versus the Pt-Ag/AgCI electrode), and preferably to about 750 mV.
  • ORP oxidation-reduction potential
  • manganese can be selectively and quantitatively recovered while avoiding precipitation of cobalt or nickel according to Equation (1 ) below in a sulphate medium:
  • Sodium permanganate 14 is the preferred oxidant, because it is sufficiently powerful to affect the oxidation of divalent manganese in solution. Hydrogen peroxide, for instance, a commonly-employed oxidant, does not work in this system. Potassium permanganate, a more common chemical than sodium permanganate, can also be used. However, this is more expensive to prepare than sodium permanganate.
  • the precipitation slurry 15 then undergoes solid-liquid separation 16. This may be effected by any convenient means, such as, but not limited to, flocculation and thickening, filter press or vacuum belt filter.
  • the solids 17 are a pure form of manganese dioxide, part of which 19 are recycled to make sodium permanganate 14. To regenerate sodium permanganate, the solids portion 19 is first fused 20 with solid caustic soda 21 , and the liquid melt 22 is quenched in water 23, where it dissolves 13 to form sodium permanganate solution 14. Sodium permanganate solution can be unstable if stored, but in this case it is used immediately, so no such issues arise. The remaining manganese dioxide solids 18 form a product for sale.
  • the treated feed solution 24 from solid-liquid separation 16 then proceeds to a first stage of cobalt precipitation 25 which is effected by the addition of sodium hypochlorite 27.
  • the pH of the treated feed solution 24 is first adjusted by the addition of an alkali, such as caustic soda 26, to a value of from about 4.5 to about 6.5, preferably from about 5.0 to about 5.5.
  • the ORP is then adjusted by the addition of sodium hypochlorite 27 to a value of from about 750 to about 900 mV, preferably from about 800 to about 850 mV (relative to the Pt-Ag/AgCI electrode).
  • the inventors have found that these pH and ORP values allow for the preferential and selective oxidation of the cobalt (e.g. from Co(ll) to Co(lll)) and the precipitation of the cobalt in the form of a heterogenite, a hydrated cobaltic oxide, CoOOH. Equation (2) shows the reaction from a chloride medium:
  • Nickel can also react under these conditions which is undesirable.
  • the reaction with nickel is very slow, given this, one option for preventing the reaction of nickel is by limiting the residence time.
  • the inventors have found that by limiting the residence time, such as to a time of limited to less than two hours (and preferably of from about 30 to about 60 minutes) the co-precipitation of nickel can be avoided allowing an essentially pure cobalt product to be obtained (i.e. a cobalt precipitate that does not include additional metal co-precipitate).
  • using a sub-stoichimetric amount of sodium hypochlorite relative to cobalt can also avoid co-precipitation of nickel.
  • a multi-stage cobalt oxidation and precipitation process can be used.
  • the solution 31 then undergoes a second stage of cobalt precipitation 32 by the addition of excess sodium hypochlorite 33. This ensures that all of the cobalt is recovered. This may also result in the co-precipitation of a small amount of nickel.
  • the second cobalt precipitation slurry 34 undergoes solid-liquid separation 35, which may be effected by any convenient means, such as, but not limited to, flocculation and thickening, filter press or vacuum belt filter.
  • the solids 36 are returned to the leaching stage (not shown) of the flowsheet.
  • the solution 37 now substantially free of cobalt, then undergoes nickel precipitation 38.
  • the precipitation slurry 40 undergoes solid-liquid separation 41 , which may be effected by any convenient means, such as, but not limited to, flocculation and thickening, filter press or vacuum belt filter.
  • the solids 42 are pure nickel carbonate.
  • the solution 43 containing a mixture of sodium sulphate and sodium chloride if the original solution was sulphate, or just sodium chloride if the original solution was chloride, may be treated for their recovery if warranted, or simply disposed of.
  • Example 1 A solution containing 80 g/L Co and 20 g/L Ni was adjusted to pH 5.5 with caustic soda, and then sodium hypochlorite was added to raise the ORP to 850 mV (versus Pt- Ag/AgCI). Black solids were formed immediately, which after filtering, washing and air drying were found to contain 59% Co and just 0.2% nickel, with the balance being primarily oxygen.
  • Figure 2 shows an XRD scan of the solids which indicates that the solids are primarily heterogenite (CoOOH), together with a small amount of a mixed cobaltic-nickelic oxide.
  • CoOOH heterogenite
  • This example demonstrates the ability of the process to recover a high-purity form of trivalent cobalt oxide from a solution containing high levels of nickel.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé pour la récupération de cobalt, de nickel et de manganèse à partir de minerais, de concentrés, de résidus, d'alliages de ferraille et de batteries usagées sous une forme oxydée, qui est approprié pour une utilisation directe dans la fabrication de batteries au lithium-ion, en particulier. Le procédé est unique dans sa capacité à récupérer du cobalt, en particulier, à partir de solutions concentrées où le rapport nickel/cobalt est proche de l'unité, plutôt que des 10:1 ou 1:100 plus courants. Le procédé comprend la précipitation oxydative sélective de chaque métal dans différentes conditions de pH et d'ORP (potentiel d'oxydo-réduction). L'hypochlorite de sodium est le précipitant préféré, étant donné qu'il ne génère pas d'acide, et est par conséquent auto-tampon au pH sélectionné. Un aspect unique du procédé est l'utilisation du Mn(VII) pour effectuer la précipitation du Mn(ll).
PCT/AU2018/050569 2017-06-14 2018-06-08 Procédé de production de cobalt et d'oxydes associés à partir de divers matériaux de charge WO2018227237A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
KR1020197038887A KR20200059191A (ko) 2017-06-14 2018-06-08 다양한 공급 물질로부터 코발트 및 관련 산화물의 생성 방법
CN201880048086.1A CN111278997A (zh) 2017-06-14 2018-06-08 由各种供给材料生产钴及相关氧化物的方法
AU2018286479A AU2018286479A1 (en) 2017-06-14 2018-06-08 Method for the production of cobalt and associated oxides from various feed materials
JP2019569259A JP2020523482A (ja) 2017-06-14 2018-06-08 さまざまな原料からコバルト及び関連酸化物を製造する方法
US16/621,282 US20200109462A1 (en) 2017-06-14 2018-06-08 Method for the production of cobalt and associated oxides from various feed materials
CA3066938A CA3066938A1 (fr) 2017-06-14 2018-06-08 Procede de production de cobalt et d'oxydes associes a partir de divers materiaux de charge
EP18816937.9A EP3638819A4 (fr) 2017-06-14 2018-06-08 Procédé de production de cobalt et d'oxydes associés à partir de divers matériaux de charge

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201762519457P 2017-06-14 2017-06-14
US62/519,457 2017-06-14

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WO2018227237A1 true WO2018227237A1 (fr) 2018-12-20

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US (1) US20200109462A1 (fr)
EP (1) EP3638819A4 (fr)
JP (1) JP2020523482A (fr)
KR (1) KR20200059191A (fr)
CN (1) CN111278997A (fr)
AU (1) AU2018286479A1 (fr)
CA (1) CA3066938A1 (fr)
WO (1) WO2018227237A1 (fr)

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US11078583B2 (en) 2013-03-15 2021-08-03 Nemaska Lithium Inc. Processes for preparing lithium hydroxide
US11083978B2 (en) 2016-08-26 2021-08-10 Nemaska Lithium Inc. Processes for treating aqueous compositions comprising lithium sulfate and sulfuric acid
US11085121B2 (en) 2014-02-24 2021-08-10 Nemaska Lithium Inc. Methods for treating lithium-containing materials
US11142466B2 (en) 2017-11-22 2021-10-12 Nemaska Lithium Inc. Processes for preparing hydroxides and oxides of various metals and derivatives thereof
US11254582B2 (en) 2012-05-30 2022-02-22 Nemaska Lithium Inc. Processes for preparing lithium carbonate
CN114585756A (zh) * 2019-10-10 2022-06-03 法国原子能源和替代能源委员会 用于回收锂电池的方法
US11697861B2 (en) 2013-10-23 2023-07-11 Nemaska Lithium Inc. Processes for preparing lithium carbonate

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11254582B2 (en) 2012-05-30 2022-02-22 Nemaska Lithium Inc. Processes for preparing lithium carbonate
US11634336B2 (en) 2012-05-30 2023-04-25 Nemaska Lithium Inc. Processes for preparing lithium carbonate
US11078583B2 (en) 2013-03-15 2021-08-03 Nemaska Lithium Inc. Processes for preparing lithium hydroxide
US11697861B2 (en) 2013-10-23 2023-07-11 Nemaska Lithium Inc. Processes for preparing lithium carbonate
US11085121B2 (en) 2014-02-24 2021-08-10 Nemaska Lithium Inc. Methods for treating lithium-containing materials
US11519081B2 (en) 2014-02-24 2022-12-06 Nemaska Lithium Inc. Methods for treating lithium-containing materials
US11083978B2 (en) 2016-08-26 2021-08-10 Nemaska Lithium Inc. Processes for treating aqueous compositions comprising lithium sulfate and sulfuric acid
US11142466B2 (en) 2017-11-22 2021-10-12 Nemaska Lithium Inc. Processes for preparing hydroxides and oxides of various metals and derivatives thereof
US11542175B2 (en) 2017-11-22 2023-01-03 Nemaska Lithium Inc. Processes for preparing hydroxides and oxides of various metals and derivatives thereof
US12006231B2 (en) 2017-11-22 2024-06-11 Nemaska Lithium Inc. Processes for preparing hydroxides and oxides of various metals and derivatives thereof
CN109921126A (zh) * 2019-04-16 2019-06-21 常熟理工学院 一种从废旧含钴锂离子电池正极材料回收活性材料的方法
CN114585756A (zh) * 2019-10-10 2022-06-03 法国原子能源和替代能源委员会 用于回收锂电池的方法

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Publication number Publication date
JP2020523482A (ja) 2020-08-06
KR20200059191A (ko) 2020-05-28
CA3066938A1 (fr) 2018-12-20
EP3638819A4 (fr) 2021-01-27
AU2018286479A1 (en) 2020-01-02
US20200109462A1 (en) 2020-04-09
CN111278997A (zh) 2020-06-12
EP3638819A1 (fr) 2020-04-22

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