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
  • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
  • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
  • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
  • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
• • 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
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G45/00—Compounds of manganese
  • C01G45/02—Oxides; Hydroxides
• • 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
  • C22B21/00—Obtaining aluminium
  • C22B21/0015—Obtaining aluminium by wet processes
  • C22B21/0023—Obtaining aluminium by wet processes from waste materials
• • 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
  • C22B23/043—Sulfurated acids or salts thereof
• • 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
  • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
  • C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
• • 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
  • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
  • C22B26/10—Obtaining alkali metals
  • C22B26/12—Obtaining lithium
• • 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
  • 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
  • C22B7/007—Wet processes by acid leaching
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/54—Reclaiming serviceable parts of waste accumulators
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/40—Electric properties
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M4/00—Electrodes
  • H01M4/02—Electrodes composed of, or comprising, active material
  • H01M4/36—Selection of substances as active materials, active masses, active liquids
  • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
  • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
  • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
• • 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
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
  • Y02E60/10—Energy storage using batteries
• • 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
  • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
  • Y02W30/00—Technologies for solid waste management
  • Y02W30/50—Reuse, recycling or recovery technologies
  • Y02W30/84—Recycling of batteries or fuel cells

Definitions

• the present invention relates to the general field of the recycling of lithium batteries and more particularly to the recycling of batteries of the Li-ion type.
• the invention relates to a process for dissolving a positive electrode material, with a view to its recycling and the recovery of the metallic elements which compose it.
• the invention is particularly interesting since the extraction efficiency of these elements is very high and the method is quick and simple to implement.
• Lithium-ion accumulators comprise a negative electrode, a positive electrode, a separator, an electrolyte and a box (“casing”) which can be a polymer pocket, or a metal packaging.
• the negative electrode is generally made of graphite mixed with a binder of the PVDF type deposited on a copper sheet.
• the positive electrode is a lithium ion insertion material (for example, UC0O 2 , LiMn0 2 , LÎ 3 NiMnCo0 6 , LiFeP04) mixed with a binder of the polyvinylidene fluoride type deposited on an aluminum sheet.
• the electrolyte consists of lithium salts (UPF 6 , L1BF 4 , L1CIO 4 ) dissolved in an organic base formed from mixtures of binary or ternary solvents based on carbonates.
• the operation is as follows: during charging, the lithium is deintercalated from the active material of the positive electrode and is inserted into the active material of the negative electrode. When discharging, the process is reversed.
• the physical methods consist, for example, in dismantling the batteries, crushing them and then sifting the crushed material thus obtained.
• the thermal methods are based on pyrometallurgical processes consisting in heating the residues at high temperature to separate the metals in the form of slag or alloys.
• these thermal methods are energy-intensive because they require temperatures that can reach 1400°C.
• very effective in separating cobalt, nickel and copper they do not allow manganese and lithium to be recovered.
• Chemical methods are used to recover valuable elements in a pure form. These are hydrometallurgical processes using reagents in the liquid phase to dissolve and/or precipitate the metals. Traditional leaching uses highly concentrated acids. This step makes it possible to fully dissolve the electrode materials to be upgraded, in ionic form. The leachate thus obtained contains mixed metal ions such as lithium, cobalt, nickel, manganese ions, etc. Chemical processes are then necessary to recover the valuable elements in a pure form.
• document WO 2005/101564 Al describes the recycling of cells and batteries with a hydrometallurgical treatment process.
• the process comprises the following steps: dry grinding, at ambient temperature and under an inert atmosphere, then treatment by magnetic separation and densimetric table, and aqueous hydrolysis, with a view to recovering the lithium, for example in the form of carbonate.
• the fine fraction freed from soluble lithium and comprising the valuable elements is dissolved in a 2N sulfuric medium at a temperature of 80° C. in the presence of steel shot.
• the cobalt is recovered by precipitation by adding sodium hypochlorite, with regulation of the pH to a value between 2.3 and 2.8. This method is used for a solution rich in cobalt (>98%) and very low in manganese ( ⁇ 2%). For a solution both rich in cobalt and in manganese, electrolysis is carried out at a temperature of 55° C. under a current density of between 400 and 600 A/m 2 .
• hypochlorite is detrimental for the installations, the safety and therefore increases the cost of the process.
• the process for recovering metals from ground lithium batteries or battery cells comprises the following steps:
• the elution of the nickel and cobalt ions is, for example, carried out with a solution complexing the nickel and/or cobalt ions, for example with the aminopolycarboxylic acid.
• the elution of the manganese ions is, for example, carried out with a mineral acid at a concentration of 2N to 4N.
• ion exchange resins are relatively expensive, and need to be regenerated. Their use generates a lot of effluents, long treatment times and high acid consumption.
• manganese has a low economic interest and must imperatively be removed upstream to avoid impacting the purity of the cobalt, nickel and lithium recovered (purity of 99.99%).
• An object of the present invention is to propose a process for dissolving a positive electrode material, remedying the drawbacks of the prior art, the process having to be simple to implement, with a low environmental impact.
• the present invention proposes a process for dissolving a positive electrode material of a battery comprising a step during which the positive electrode material, comprising lithium and optionally cobalt and/or nickel, in an acid solution at a pH of between 0 and 4, the acid solution additionally containing either manganese ions or hydrogen peroxide, whereby the lithium and optionally the cobalt and/or the nickel are dissolved and , if necessary, the manganese ions are selectively precipitated in the form of manganese oxyhydroxide.
• the invention differs fundamentally from the prior art by the implementation of a hydrometallurgical process during which an electrode to be recycled is immersed in a so-called leaching or dissolving solution containing manganese ions or hydrogen peroxide.
• the metals of interest such as lithium, nickel and/or cobalt are in the ionic form, and the manganese is in the form of a solid oxyhydroxide MnO(OH) .
• the leaching/dissolution process makes it possible to recycle the positive electrode materials of batteries, of all electrochemical systems, which may contain manganese, of the accumulator or battery type treated separately or as a mixture.
• the process can be used for various battery chemistries (NCA, NMC with different proportions, for example, 1/1/1, 5/3/2, 6/2/2, 8/1/1 or 9/0 , 5/0, 5).
• NCA battery chemistries
• This recycling and recovery process is robust and has good manganese separation yields for different types of battery waste.
• the positive electrode material further comprises manganese.
• the manganese of the positive electrode is dissolved in solution, as additional manganese ions, the additional manganese ions then precipitating out selectively as manganese oxyhydroxide .
• This method makes it possible to selectively, quickly and efficiently recover manganese from an electrode containing lithium and possibly other elements, such as cobalt and/or nickel, even if the chemistry of manganese and that of these elements are very similar.
• waste batteries preferably ground battery
• the dissolving of waste batteries leads in a single step to the leaching of the metals contained in this waste and to the selective separation of the manganese.
• the manganese of the positive electrode material is entirely recovered in the form of manganese oxo hydroxide.
• the leaching solution contains manganese ions.
• it is Mn(ll).
• the manganese ions are obtained by dissolving a manganese salt.
• the manganese salt is a manganese sulphate salt.
• the manganese salt is introduced in stoichiometric proportion or in excess relative to the metals of the positive electrode material. It is, for example, between 1g/L and 10g/L.
• the leaching solution contains hydrogen peroxide (H2O2).
• H2O2 hydrogen peroxide
• the reaction with hydrogen peroxide is advantageously exothermic, which avoids heating the solution.
• the concentration by volume of hydrogen peroxide is between 0.1% and 16%, preferably between 1% and 12% (for example between 1% and 10%), and even more preferably between 1% and 6% (for example between 1% and 4%).
• 1% and 4% it is meant that the terminals are included. The same applies to the ranges described here and subsequently.
• the solid/liquid (S/L) ratio is between 5% and 40%, and advantageously between 5% and 30% (for example between 15% and 30%), preferably between 5% and 20% (by example 10%).
• the solid corresponds to the mass (g) of the positive electrode material (typically lithium mixed oxide) and the liquid to the volume (mL) of the solution.
• the pH is between 0.5 and 2.5 and preferably between 1 and 2.5. It is for example 2.
• the concentration by volume of hydrogen peroxide is chosen as a function of the S/L ratio.
• the ratio between the concentration by volume of hydrogen peroxide and the solid/liquid ratio is between 0.1 and 0.4 and preferably between 0.2 and 0.3.
• concentrations are sufficient to, on the one hand, dissolve at least 90% or even completely the lithium and possibly the cobalt and/or the nickel in solution and, on the other hand, to completely dissolve the manganese and cause it to precipitate in the form of a solid manganese oxyhydroxide. These conditions avoid bringing the manganese into solution and thus facilitate its separation from the other elements of the solution.
• the solid/liquid ratio is between 5% and 40% and the concentration by volume of hydrogen peroxide is between 1% and 12%.
• the solid/liquid ratio is between 5% and 20% and the concentration by volume of hydrogen peroxide is between 1% and 6%.
• the solid/liquid ratio is between 5% and 10%
• the pH is between 1 and 2.5
• the concentration by volume of hydrogen peroxide is between 1% and 3%.
• a concentration by volume of hydrogen peroxide of between 2% and 3% will be chosen.
• the positive electrode is an NMC, NCA or
• the temperature of the solution is between 70°C and 100°C, preferentially between 80°C and 95°C, and even more preferentially between 80°C and 85°C.
• the solution is stirred.
• the positive electrode material is in particulate form.
• the invention particularly finds applications in the field of recycling and/or recovery of batteries/accumulators/cells of the Li-ion type, and in particular of their electrodes.
• a battery but it could be a cell or an accumulator.
• battery waste the battery or part of the battery which has been recovered after securing and dismantling the battery.
• the battery waste comprises lithium and optionally cobalt and/or nickel. According to a particularly advantageous embodiment, the waste battery also comprises manganese.
• Battery scrap may also include aluminum.
• the waste battery is a positive electrode whose active material may be UC0O2 (lithium cobalt oxide (LCO)), LiMn0 2 , LiNi0 2 , LiNiCoAl0 2 (nickel-cobalt-aluminum (NCA)) or LiNi x Mn yCoz 0 2 . (NMC (nickel-manganese-cobalt)).
• LCO lithium cobalt oxide
• LiMn0 2 LiNi0 2
• LiNiCoAl0 2 nickel-cobalt-aluminum (NCA))
• NCA nickel-cobalt-aluminum
• NMC nickel-manganese-cobalt
• an NMC or LiMn0 2 electrode will be chosen.
• the NMC electrode can have different ratios of nickel, cobalt and manganese.
• the ratio can be 1/1/1, 5/3/2, 6/2/2, 8/1/1 or 9/0, 5/0, 5.
• Battery waste may also contain other species.
• the other species can be metals, alkali metals and/or rare earths.
• the following elements may be mentioned: Fe, Zn, Al, Mg, Cu, Ca, Pb, Cd, La, Ti, V, Nd and Ce.
• the battery waste is advantageously ground before the dissolution step, whereby a ground material is formed.
• the particles of the ground material have, for example, a largest dimension of less than 1 cm.
• the method can also be carried out directly on unground battery waste.
• the process for dissolving a battery positive electrode material according to the invention comprises the following steps:
• a positive electrode material comprising lithium and, optionally, cobalt and/or nickel and/or manganese
• the method according to the invention also makes it possible to treat a concentrated powder of positive electrode material which has been obtained, for example, after a step of separating the active material from the current collector.
• the selective dissolution phase ensures complete dissolution of valuable elements (lithium, nickel and/or cobalt) and, if necessary, separation of manganese in a single step.
• the positive electrode material preferably NMC, LiMn0 2
• preferably in powder form is introduced in a solid/liquid ratio of 5% to 40%, and advantageously between 15% and 30% (g/mL ).
• the solution is preferably an aqueous solution. It could also be an organic solution.
• the acid is advantageously chosen from mineral acids, for example from hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid or a mixture thereof.
• sulfuric acid will be chosen since it is the least corrosive for the materials used in the process, it presents fewer dangers during its use and it is readily available at a relatively low cost.
• the pH is between 0 and 4, preferably between 1 and 2.5. For example, we will choose a pH of 2.
• a control device is used to maintain a constant pH (within 10%) throughout the treatment.
• the leaching solution contains a manganese salt.
• the manganese salt is added in a stoichiometric amount or in excess to ensure complete dissolution.
• the manganese salt can be a salt of manganese chloride, manganese nitrate, manganese sulphate. These salts advantageously have good solubility in water.
• a manganese sulphate salt will be chosen, to avoid the presence of nitrate or chloride in solution. It could also be manganese hydroxide.
• the leaching solution contains hydrogen peroxide.
• concentration by volume of hydrogen peroxide is preferably between 0.1% and 16%, and preferably between 1% and 12%, for example between 1% and 10%.
• the leaching solution additionally contains a manganese salt.
• the manganese salt can be a salt of manganese chloride, manganese nitrate, manganese sulphate. These salts advantageously have good solubility in water.
• a manganese sulphate salt will be chosen, to avoid the presence of nitrate or chloride in solution. It could also be manganese hydroxide.
• the concentration by volume of hydrogen peroxide will be chosen as a function of the S/L ratio.
• the ratio between the concentration by volume of hydrogen peroxide and the S/L ratio is between 0.1 and 0.4, and even more preferably between 0.2 and 0.3.
• the duration of the leaching stage can be between 1 h and 24 h.
• the duration of the leaching step can be adapted according to the temperature of the solution.
• the temperature of the solution can be between 70°C and 110°C, for example between 70°C and 100°C, preferably in the vicinity of 80°C to 85°C. With such temperatures, the duration of the treatment is for example of the order of 3 hours.
• the pressure during the leaching step is preferably atmospheric pressure (of the order of 1 bar).
• the method may comprise another step during which another element present in the solution to be treated and having a high added value is advantageously recovered.
• the cobalt, lithium and/or nickel ions will advantageously be recovered. It is also possible to recover aluminum.
• nickel ions for example, it is possible to separate the nickel ions, by precipitation in a basic medium by increasing the pH between 7 and 10, by adding a base such as NaOH, NH4OH or Na2CÜ3, whereby the nickel is precipitated.
• a base such as NaOH, NH4OH or Na2CÜ3
• Example 1 Treatment of NMC in ratio (1/1/1): total dissolution of the electrode material and extraction of the manganese
• FIG. 1 represents the dissolution kinetics of the NMC electrode in the sulfuric acid solution.
• the mass composition of the manganese precipitate is largely enriched in Mn, with a residual cobalt and nickel. If necessary, the manganese precipitate can be completely pure by adapting the quantity of manganese sulphate.
• the mass composition of the metals in the manganese residue is listed in the following table:
• Example 2 Treatment of NMC in relation (6/2/2): total dissolution of the electrode material and extraction of manganese:
• FIG. 2 represents the dissolution kinetics of the NMC electrode in the sulfuric acid solution.
• manganese which passes from the ionic state in solution to a solid of manganese oxyhydroxide.
• the dissolution of lithium, nickel and cobalt is observed.
• the mass composition of the manganese precipitate is largely enriched in Mn, with a residual of cobalt. If necessary, the manganese precipitate can be completely pure by adapting the quantity of manganese sulphate.
• the mass composition of the metals in the manganese residue is listed in the following table:
• the mass composition of the metals in the manganese residue is listed in the following table:
• Example 4 Treatment of NMC in ratio (8/1/1): total dissolution of the electrode material and extraction of the manganese
• Example 5 Treatment of NMC in relation (1/1/1): selective dissolving of nickel, cobalt and lithium and extraction of manganese with control of the H2O2 supply.
• the volume concentrations of hydrogen peroxide are 0% vol, 2% vol, 4% vol and 6% vol.
• the quantity of H2O2 which is transcribed in volume percentage with respect to the quantity of liquid.
• FIG. 3 represents the dissolution yield of the NMC electrode in the sulfuric acid solution according to the volume percentage of H2O2 at 30% added. It has been observed that not all concentrations achieve complete dissolution of cobalt and nickel, and simultaneous precipitation of manganese (i.e. absence of manganese in solution).
• Example 6 Treatment of NMC in relation (6/2/2): selective dissolving of nickel, cobalt and lithium and extraction of manganese with control of the H2O2 supply :
• Figure 4 represents the dissolution yield of the NMC electrode in the sulfuric acid solution according to the volume percentage of H2O2.
• the optimum is determined in the vicinity of 2% by volume (arrow on the graph).
• those skilled in the art will adapt the quantity for a totally optimized reaction. It is nevertheless observed that for a lower concentration the dissolution is incomplete, which is to the detriment of the efficiency of the process. For a much higher concentration, there is concomitant dissolution of the manganese which does not allow it to be completely removed.
• Example 7 Treatment of NMC in relation (8/1/1): selective dissolving of nickel, cobalt and lithium and extraction of manganese with control of the H2O2 supply
• Figure 5 represents the dissolution yield of the NMC electrode in the sulfuric acid solution according to the volume percentage of H2O2. There is an optimum for achieving complete dissolution of cobalt and nickel (i.e. 100%), with absence of manganese in solution (% extraction in solution of 0%).

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• 2021
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