WO2022114868A1 - Procédé de fabrication d'un matériau actif recyclé d'électrode positive utilisant une batterie secondaire usagée - Google Patents

Procédé de fabrication d'un matériau actif recyclé d'électrode positive utilisant une batterie secondaire usagée Download PDF

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WO2022114868A1
WO2022114868A1 PCT/KR2021/017681 KR2021017681W WO2022114868A1 WO 2022114868 A1 WO2022114868 A1 WO 2022114868A1 KR 2021017681 W KR2021017681 W KR 2021017681W WO 2022114868 A1 WO2022114868 A1 WO 2022114868A1
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active material
positive electrode
electrode active
manufacturing
renewable
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PCT/KR2021/017681
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English (en)
Korean (ko)
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진홍수
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주식회사 엘아이비에너지
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Priority to CN202180003928.3A priority Critical patent/CN114830408A/zh
Publication of WO2022114868A1 publication Critical patent/WO2022114868A1/fr

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    • 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
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 a method for manufacturing a recycled positive electrode active material using a waste secondary battery, and more particularly, to a method for manufacturing a recycled positive electrode active material configured to be capable of regeneration at a high production rate and to provide an efficiency similar to that of the first secondary battery. It's about
  • Lithium transition metal oxide is used as a cathode active material for lithium secondary batteries, and lithium cobalt oxide (LiCoO 2 ), lithium manganese oxide (LiMnO 2 , LiMn 2 O 4 , etc.), lithium iron phosphate compound ( LiFePO 4 etc.) and lithium nickel oxide (LiNiO 2 etc.) are mainly used.
  • the cathode active material of such a lithium secondary battery for example, lithium cobalt oxide or transition metal constituting NCM-based lithium oxide is expensive, and in particular, cobalt is a strategic metal, and each country is interested in supply and demand, Since the number of cobalt producing countries is limited, it is known as a metal whose supply and demand is unstable worldwide. In addition, since these transition metals can cause environmental problems, it is necessary to respond to environmental regulations.
  • this conventional recycling method can be used only limited to lithium cobalt oxide (LCO) among waste positive electrode active materials, and lithium nickel cobalt manganese oxide (NCM) or lithium ion manganese oxide (LMO) for electric vehicles, which is increasingly used, is used.
  • LCO lithium cobalt oxide
  • NCM lithium nickel cobalt manganese oxide
  • LMO lithium ion manganese oxide
  • the conventional recycling method described above is not a preferable method in terms of cost, because when producing cobalt using oxalic acid, it is calcined to decompose oxalic acid into carbon dioxide and then re-dissolved cobalt oxide in sulfuric acid to make cobalt sulfate. .
  • the above-described conventional recycling method causes considerable difficulties in wastewater treatment due to an excess of oxalic acid that enters to selectively separate cobalt.
  • the positive electrode active material regenerated in this way has a high impurity content to be used as a secondary battery precursor raw material with high added value, and thus lacks value as an intact material, and thus lacks practical marketability.
  • the present inventors have completed the present invention, recognizing that it is urgent to develop a method for efficiently regenerating a cathode active material for a secondary battery.
  • Patent Document 1 Republic of Korea Patent Publication No. 10-2064668
  • Patent Document 2 Japanese Patent Laid-Open No. 1999-006020
  • An object of the present invention is to provide a method for manufacturing a recycled positive electrode active material that can be economically and easily regenerated from a waste secondary battery and can provide excellent electrochemical properties.
  • the present invention provides a method for manufacturing a recycled positive electrode active material using a waste secondary battery.
  • the method of manufacturing a renewable positive electrode active material of the present invention may be configured to include the following steps.
  • x and y each have a value between 0 and 10.
  • the positive electrode plate separated from the waste secondary battery in step (S1) may include an active material, a conductive material, and a binder.
  • step (S1) may be performed in an inert gas or reducing gas environment.
  • step (S1) the heat treatment of step (S1) is performed in a temperature range of 510 ° C. to 750 ° C., and as the anode plate is reduced by the heat treatment performed in step (S1), Co x O y material can be produced. have.
  • Co x O y generated in step (S1) may include at least one material selected from the group consisting of CoO, Co 2 O 3 and Co 3 O 4 .
  • the Co x O y material produced in step (S1) may be CoO.
  • the Co x O y material generated in step (S1) may be formed in a porous structure.
  • the Co x O y material produced in step (S1) may include pores in the range of 0.001 to 10.0 cm 3 /g.
  • the Co x O y material produced in step (S1) may have a specific surface area of 0.3 to 50.0 m 2 /g.
  • the lithium-containing material mixed in step (S2) may include at least one material selected from the group consisting of LiOH, Li 2 CO 3 , LiNO 3 and Li 3 PO 4 .
  • the material containing lithium mixed in step (S2) may be mixed so that the molar ratio of lithium to Co contained in the Co x O y material produced in step (S1) is 1.0 to 1.06. have.
  • the heat treatment in step (S3) may be performed in a temperature range of 800 °C to 1,050 °C.
  • the heat treatment in step (S3) may be performed by dry heat treatment or wet heat treatment.
  • the present invention provides a recycled positive electrode active material formed according to the above-described manufacturing method.
  • the method for manufacturing a recycled cathode active material using a waste secondary battery of the present invention can economically and easily regenerate a cathode active material from a waste secondary battery, and the electrochemical performance of the cathode active material is not deteriorated during the regeneration process, and has excellent resistance properties, electrical conductivity characteristics and capacity characteristics can be implemented.
  • FIG. 1 is a block diagram schematically showing a method for manufacturing a recycled positive electrode active material using a waste secondary battery of the present invention.
  • FIG. 2 is an X-ray photoelectron spectroscopy (XPS) spectrum obtained by analyzing the components of a positive electrode plate that can be used in a method of manufacturing a recycled positive electrode active material of the present invention.
  • XPS X-ray photoelectron spectroscopy
  • Example 3 is a scanning electron microscope (SEM) image confirming the pores formed on the CoO produced in Example 1 of the present invention.
  • step (S1) is an X-ray diffraction (XRD) of a material prepared by performing the heat treatment of step (S1) at 500° C., 600° C. and 700° C. in the method for manufacturing a recycled cathode active material using a waste secondary battery of the present invention. ) is the pattern.
  • XRD X-ray diffraction
  • Example 6 is an X-ray diffraction pattern (X-ray diffraction, XRD) of CoO produced in Example 1 of the present invention and a recycled cathode active material ((LCO) 1) prepared using this CoO.
  • XRD X-ray diffraction
  • LCO recycled cathode active material
  • FIG. 7 is a graph illustrating electrochemical performance evaluation at 3.0 to 4.3V for the recycled positive active material and the commercial positive active material prepared according to the present invention.
  • the present invention provides a method for manufacturing a renewable positive electrode active material comprising the following steps.
  • x and y may each have a value of 0 to 10.
  • “Anode active material” refers to an active material containing lithium oxide as the main component that generates electricity through a chemical reaction in a secondary battery.
  • the positive active material is a positive active material containing lithium and cobalt, preferably LCO (LiCoO 2 ), LCA (LiCoAlO 2 ), LCM (LiCoMnO 2 ) and LCMA (LiCoMnAlO 2 ) ) may be at least one selected from the group consisting of a positive active material having a layered structure of It may be at least one layered structure positive electrode active material selected from the group consisting of NCO, NCA, NCM and NCMA.
  • the LCO is in the form of oxides of lithium and cobalt having a layered structure, and has the advantage of very high stability and longevity.
  • the LCA is in the form of oxides of lithium, cobalt and aluminum having a layered structure, and has the advantage of being easy to apply industrially and having a long life by reducing the content of expensive cobalt.
  • the LCM is in the form of oxides of lithium, cobalt and manganese having a layered structure, and has the advantage of being easy to apply industrially by reducing the content of expensive cobalt, and having somewhat high stability.
  • the LCMA is in the form of oxides of lithium, cobalt, manganese, and aluminum having a layered structure, and can be said to be a combination of the LCA and the LCM, thereby exhibiting the advantages of the LCA and the LCM together.
  • the LMO is an oxide form of lithium and manganese having a spinel structure, has very high stability, and does not contain expensive cobalt, so it is economically very cheap.
  • the LFP is a material containing lithium, iron, phosphorus and oxygen having an olivine structure, and is relatively compared to the LCO (LiCoO 2 ), LCA (LiCoMnO 2 ), LCM (LiCoMnO 2 ) and LMO (LiMn 2 O 4 ). It has the best stability and has a long lifespan, so it can be applied to various fields.
  • the step (S1) may be a step of generating Co x O y by reducing heat treatment of the positive electrode plate separated from the waste secondary battery.
  • the positive electrode plate separated from the waste secondary battery used in step (S1) may include a positive electrode active material, a conductive material, a binder, and the like. That is, the positive electrode plate separated from the waste secondary battery used in step (S1) can be used as it is in the state used in the secondary battery (that is, the electrode plate is rolled by applying an active material, a conductive material, a binder, etc.). .
  • a Co x O y material can be generated due to the conductive material and the binder material attached to the positive electrode plate.
  • the binder is a component that assists in bonding the positive active material and the conductive material and bonding to the current collector, and examples thereof include polyvinylidene fluoride (PVDF), polyvinyl alcohol (PVOH, PVA). , PVAI), carboxymethyl cellulose (CMC), starch, hydroxypropyl cellulose (HPMC), polyvinyl pyrrolidone (Polyvinyl Pyrrolidone), tetrafluoroethylene (Polytetrafluoroethylene, PTFE) , polyethylene (PE), polypropylene (PP), ethylene-propylene-diene terpolymers (Ethylene, Propylene, Non-conjugated Diene, Ethylene Propylene Terpolymers, EPDM), styrene-butylene rubber, fluororubber and various public It may be at least one selected from the group consisting of coalescing, but any binders commonly used may be applied without limitation.
  • PVDF polyviny
  • the conductive material is not particularly limited as long as it has conductivity without causing a chemical change in the secondary battery.
  • graphite such as natural graphite and artificial graphite
  • carbon black such as carbon black, acetylene black, Ketjen black, channel black, furnace black, lamp black, and summer black
  • conductive fibers such as carbon fibers and metal fibers
  • metal powders such as carbon fluoride, aluminum, and nickel powder
  • conductive whiskeys such as zinc oxide and potassium titanate
  • conductive metal oxides such as titanium oxide
  • Conductive materials such as polyphenylene derivatives may be used.
  • step (S1) is preferably performed at 510° C. to 750° C. for the positive electrode plate, and most preferably, may be performed at a temperature range of 550° C. to 660° C. When the heat treatment of step (S1) is performed in a temperature range of less than 510° C., sufficient reduction is not performed properly, so that the phase of the initial active material can be maintained.
  • the step (S1) may be performed in an environment in which oxygen is lacking and the reduction reaction can be performed more easily, preferably in an inert gas environment or a reducing gas environment, preferably argon (Ar), nitrogen (N 2 ), carbon dioxide (CO 2 ), carbon monoxide (CO) or hydrogen (H 2 ) may be carried out in an environment, most preferably in an argon or nitrogen environment.
  • argon Ar
  • nitrogen N 2
  • carbon dioxide CO 2
  • CO carbon monoxide
  • H 2 hydrogen
  • the Co x O y material generated in step (S1) may include at least one material selected from the group consisting of CoO, Co 2 O 3 and Co 3 O 4 .
  • the Co x O y material produced in step (S1) may preferably be CoO.
  • Co x O y which is a material produced in step (S1), means a main material produced by heat treatment, and a case in which a small amount of other materials are included with these materials is not excluded.
  • the Co x O y material produced in step (S1) may have a porous structure in which pores are formed, and preferably, pores of 0.001 to 10.0 cm 3 /g may be included in the Co x O y material.
  • pores are formed by eluting oxygen (O 2 ) gas and lithium (Li) ions during the reduction process of the spent secondary battery. Due to the pores, the specific surface area of the positive electrode active material increases, so that the diffusion of lithium during the production of the recycled LCO can provide an effect that can improve
  • the Co x O y material produced in step (S1) may have a specific surface area of 0.3 to 50.0 m 2 /g.
  • the step (S2) is a step of mixing the generated Co x O y with a lithium-containing material, and the lithium-containing material mixed in the (S2) step includes LiOH, Li 2 CO 3 , LiNO 3 and Li At least one material selected from the group consisting of 3 PO 4 may be included, and preferably, at least one material selected from the group consisting of Li 2 CO 3 , LiNO 3 and Li 3 PO 4 may be included, and most preferably At least one material selected from the group consisting of Li 2 CO 3 and Li 3 PO 4 may be included.
  • the material containing lithium mixed in step (S2) may be mixed so that the molar ratio (Li/Co) of lithium to Co contained in Co x O y generated in step (S1) is 1.0 to 1.06. .
  • the heat treatment in step (S3) may be performed at 800 °C to 1,050 °C.
  • step (S3) may be performed through dry heat treatment performed by putting it in an oven, furnace, tube, etc. in the absence of moisture, or wet heat treatment through hydrothermal treatment.
  • the separated positive electrode plate was measured by X-ray photoelectron spectroscopy (XPS), and the measurement result is shown in FIG. 2 .
  • XPS X-ray photoelectron spectroscopy
  • the positive electrode plate separated from the waste lithium secondary battery contains lithium including an active material, an additive binder (PVDF), an electrolyte, and the like.
  • Example 1 According to the present invention (S1) in Example 1 using a specific surface area analyzer (Brunauer Emmett Teller, BET) to confirm that CoO with pores was generated by separating the positive electrode plate from the waste secondary battery and then heat-reducing it.
  • a specific surface area analyzer Brunauer Emmett Teller, BET
  • the specific surface areas of CoO, recycled positive electrode active material (LCO) 1, and commercial positive electrode active material (LCO) prepared by the method were analyzed, and are shown in [Table 1] below.
  • the CoO produced in step (S1) according to the present invention has pores having a denser pore size and a high specific surface area compared to the recycled cathode active material 1 and the commercial cathode active material. can confirm.
  • the CoO produced in Example 1 was measured with a scanning electron microscope to confirm the pore formation image and is shown in FIG. 3 .
  • the step (S1) for comparison according to the heat treatment environment (gas environment) of the step (S1), the step (S1) is performed in an oxygen environment with Examples 1 and 2 and as a comparison group therefor Comparative regenerated positive electrode active materials 1 to 3 heat-treated at 500° C., 600° C. and 700° C. were prepared and X-ray diffraction patterns were measured, and are shown in FIG. 4 .
  • Comparative Regenerated Positive Active Material 4 in which step (S1) was performed at 500° C., has an X-ray diffraction pattern in which CoO and the active material coexist regardless of the temperature range.
  • the regenerated positive electrode active materials 1 and 2 according to the present invention in which step (S1) was performed at 600° C. and 700° C. showed an X-ray diffraction pattern in which both the active materials were reduced and only CoO was present.
  • step (S1) in order to prepare pure CoO from which impurities are completely removed through step (S1), it is most preferable to perform the heat treatment of step (S1) in a temperature range of 510° C. to 750° C. in an inert gas argon gas environment. can be checked
  • the regenerated positive electrode active material (Example 1) prepared using the porous CoO prepared according to the present invention has a layered structure.
  • the commercial positive active material, the regenerated positive active material 1, and the regenerated positive active material 2 have substantially the same characteristics within an error range in charge capacity, discharge capacity and efficiency. From these results, it can be confirmed that the regenerated positive electrode active material prepared according to the present invention does not deteriorate electrochemical performance and can realize excellent electrochemical properties.

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

La présente invention concerne un procédé de fabrication d'un matériau actif recyclé d'électrode positive, le procédé comprenant : (S1) une étape de production d'un matériau CoxOy consistant à traiter thermiquement une plaque d'électrode positive séparée d'une batterie secondaire usagée ; (S2) une étape consistant à mélanger un matériau comprenant du lithium avec le matériau CoxOy produit ; et (S3) une étape consistant à traiter thermiquement le matériau mélangé pour former un matériau actif recyclé d'électrode positive. Dans CoxOy, x et y ont chacun une valeur de 0 à 10.
PCT/KR2021/017681 2020-11-27 2021-11-26 Procédé de fabrication d'un matériau actif recyclé d'électrode positive utilisant une batterie secondaire usagée WO2022114868A1 (fr)

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