WO2012169073A1 - Procédé de récupération de métaux de valeur dans les accumulateurs au lithium-ion mis aux rebuts - Google Patents

Procédé de récupération de métaux de valeur dans les accumulateurs au lithium-ion mis aux rebuts Download PDF

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Publication number
WO2012169073A1
WO2012169073A1 PCT/JP2011/063392 JP2011063392W WO2012169073A1 WO 2012169073 A1 WO2012169073 A1 WO 2012169073A1 JP 2011063392 W JP2011063392 W JP 2011063392W WO 2012169073 A1 WO2012169073 A1 WO 2012169073A1
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WIPO (PCT)
Prior art keywords
positive electrode
current collector
negative electrode
sieve
ion secondary
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Ceased
Application number
PCT/JP2011/063392
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English (en)
Japanese (ja)
Inventor
幹雄 原田
智 徳田
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Nippon Magnetic Dressing Co
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Nippon Magnetic Dressing Co
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Priority to PCT/JP2011/063392 priority Critical patent/WO2012169073A1/fr
Publication of WO2012169073A1 publication Critical patent/WO2012169073A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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 recovering valuable metals from waste lithium ion secondary batteries, and more specifically, waste lithium for recovering valuable metals such as lithium, cobalt, nickel, manganese, copper, aluminum and iron from used lithium ion secondary batteries.
  • waste lithium for recovering valuable metals such as lithium, cobalt, nickel, manganese, copper, aluminum and iron from used lithium ion secondary batteries.
  • the present invention relates to a method for recovering valuable metals from an ion secondary battery.
  • lithium ion secondary batteries have been widely used as power sources for portable small electronic devices such as mobile phones, personal digital assistants (PDAs), notebook personal computers, video cameras, and portable game machines.
  • a lithium ion secondary battery is a battery that performs charging and discharging when lithium ions move between a positive electrode body and a negative electrode body.
  • the battery configuration includes a stainless steel casing, an aluminum casing, or an outer case made of a plastic laminated composite body, and a positive electrode current collector made of aluminum foil and lithium metal oxide.
  • Cobalt (Co), nickel (Ni), manganese (Mn), and the like contained in lithium metal acid are valuable metals that are recovered and reused.
  • the roasting temperature of the lithium ion secondary battery is set to 800 ° C. described in Examples 1 and 2 of Patent Document 1, or 700 ° C. described in Examples 3 and 4, and the inside of the roasting furnace is set.
  • the roasting temperature of the lithium ion secondary battery is defined as 350 ° C. to 1000 ° C.
  • the inventor conducted a heat treatment of the lithium ion secondary battery in an atmosphere of oxygen-free superheated steam instead of the inert gas, and thereby the plastic outer case and the organic solvent in the electrolytic solution were removed. It can be thermally decomposed at low cost while suppressing metal oxidation and generation of dioxins, and the heat treatment temperature is set to 350 ° C. to 550 ° C., so that the aluminum casing and the positive electrode current collector having a melting point of 660 ° C.
  • vibration-type crushing such as a vibration ball mill It has been found that if secondary crushing is performed by a machine, the positive electrode material residue adhering to the positive electrode current collector can be sufficiently peeled off, and the recovery rate of valuable metals contained in the positive electrode material can be increased. This invention has been completed.
  • an object of the present invention is to provide a method for recovering valuable metals from a waste lithium ion secondary battery that can increase the recovery rate of valuable metals contained in a positive electrode material as compared with the conventional method.
  • a positive electrode body in which a positive electrode material made of lithium metalate is fixed to a positive electrode current collector made of aluminum foil inside the outer case, and a negative electrode material made of a negative electrode current collector made of metal foil.
  • a method for recovering valuable metals from a waste lithium ion secondary battery which contains a fixed negative electrode body, a separator disposed between the positive electrode body and the negative electrode body, and an electrolyte solution in which a lithium salt is dissolved in an organic solvent. And heating the waste lithium ion secondary battery with superheated steam at 350 ° C. to 550 ° C.
  • Waste lithium ion secondary batteries are primarily crushed by an impact crusher or shear crusher, and the primary crushed material obtained by the primary crushing is passed through a sieve with a classification point of 0.15 mm to 0.60 mm.
  • the positive electrode material and the negative electrode material are collected from under the sieve, and the positive electrode current collector and the negative electrode current collector are collected from the sieve. After the primary classification, the positive electrode collector on the sieve is collected.
  • the residue of the positive electrode material is peeled off from the positive electrode current collector, and the residue of the negative electrode material is peeled off from the negative electrode current collector,
  • the secondary crushed material obtained by the secondary crushing is secondarily classified with a sieve having a classification point of 0.15 to 0.60 mm, whereby the residue of the positive electrode material and the residue of the negative electrode material are recovered from under the sieve.
  • it is a method for recovering valuable metals from a waste lithium ion secondary battery in which the positive electrode current collector and the negative electrode current collector are recovered from a sieve.
  • the waste lithium ion secondary battery is heated with superheated steam at 350 ° C. to 550 ° C. to thermally decompose the outer case, the separator and the organic solvent (thermal decomposition step).
  • the superheated steam used at this time is the same oxygen-free gas as the inert gas. Therefore, ignition of flammable organic solvents is suppressed, deterioration due to metal oxidation is prevented, quality is not deteriorated, and heat treatment can be safely performed without risk of explosion, and generation of dioxins is also possible. Can be suppressed.
  • the heat medium for superheated steam is water. Thereby, it can heat-process cheaply compared with the conventional inert gas.
  • the heat treatment temperature of the waste lithium ion secondary battery is set to 350 ° C. to 550 ° C.
  • an organic substance containing an organic solvent can be efficiently heat treated in a short time.
  • the aluminum casing and the positive electrode current collector are not dissolved.
  • aluminum (melting point: 660 ° C.) contained in the melted casing and the positive electrode current collector adheres to the furnace wall and the melt is solidified and discharged.
  • the heated waste lithium ion secondary battery is primarily crushed by an impact crusher such as a Hanmark crusher or a shear crusher such as a uniaxial shear crusher.
  • an impact crusher such as a Hanmark crusher or a shear crusher such as a uniaxial shear crusher.
  • the positive electrode material containing rare metal is pulverized together with the negative electrode material, and the positive electrode current collector made of aluminum foil and the negative electrode current collector made of metal foil are crushed in a relatively large size (primary crushing step).
  • the primary crushed material is subjected to primary classification with a sieve having a classification point of 0.15 to 0.60 mm (primary classification step).
  • the positive electrode material containing a rare metal can be recovered together with the negative electrode material from under the sieve.
  • the residue of the positive electrode material adhering to the positive electrode current collector on the sieve cannot be sufficiently removed only by this primary crushing.
  • the material on the sieve is further subjected to secondary crushing by a vibration type crusher such as a vibration ball mill (secondary crushing step).
  • the secondary crushed material is subjected to secondary classification using a sieve having the same mesh (mesh) as that for primary classification (secondary classification step).
  • the exterior case for example, a case in which a casing made of stainless steel or aluminum is covered with a plastic case can be employed.
  • the plastic case is a composite with a laminated structure.
  • the first layer from the outside is polyethylene (PE), polypropylene (PP), nylon, ABS, vinyl chloride, polyester, etc.
  • the second layer is a crystalline polymer (LCP). ), Polyphenylene sulfide (PPS), polyethersulfone (PES), polybutylene terephthalate (PBT), polyamideimide (PAI), polyphthalamide (PPA), polyetheretherketone (PEEK), etc.
  • the third layer is fluorine.
  • the positive electrode body is obtained by fixing (coating) a positive electrode material to a surface of an aluminum foil with a binder.
  • a positive electrode material for example, lithium-containing transition metal oxides such as lithium cobaltate, lithium nickelate, and lithium manganate can be employed.
  • a modified body in which a part of the transition metal of the lithium-containing transition metal oxide is substituted with another element (aluminum, magnesium, etc.) may be used.
  • the negative electrode body is obtained by fixing (coating) a negative electrode material (negative electrode active substance) to the surface of a metal foil for a negative electrode with a binder.
  • a negative electrode material for example, carbon materials such as natural graphite and artificial graphite can be adopted.
  • metal materials such as silicon and tin, and alloy materials such as silicon alloy and tin alloy may be used. These materials may be used alone or in combination of two or more.
  • a copper foil can be employed.
  • copper alloy foil, nickel-plated iron foil, stainless steel foil, and the like may be used.
  • a non-aqueous solvent in which a lithium salt is dissolved can be employed.
  • a carbonate such as ethylene carbonate (EC), a carboxylic acid ester such as methyl acetate, or an ether such as dimethyl ether
  • a lithium salt for example, LiPF 6 , LiBF 4 and the like can be employed.
  • the separator is an isolation film interposed between the positive electrode body and the negative electrode body, and is made of a plastic sheet such as polyethylene.
  • Examples of the organic substance in the waste lithium ion secondary battery include a plastic case for an exterior case, a separator made of plastic, and the like in addition to an organic solvent.
  • Lithium ion secondary batteries have a positive electrode material fixed on the surface of an aluminum foil to form a positive electrode body, a negative electrode material fixed to the surface of a metal foil to form a negative electrode body, and a separator inserted between the positive electrode body and the negative electrode body These are wound and compressed in accordance with a predetermined standard, the obtained roll is inserted into the outer case, and the electrolytic solution is filled in the inner space of the outer case. Then, parts such as a conductive handle, a leak pressure safety valve and an end cover are attached. In addition, these are sealed in an outer case.
  • the heat treatment of the waste lithium ion secondary battery with superheated steam is performed by a superheated steam pyrolysis apparatus.
  • a superheated steam thermal decomposition apparatus capable of continuously heat treating a waste lithium ion secondary battery.
  • This superheated steam generator is an apparatus that further heats dry saturated steam generated by a boiler or the like to generate higher temperature superheated steam corresponding to the pressure of the saturated steam, and the superheated steam is an oxygen-free gas.
  • the organic matter containing the electrolyte contained in the lithium ion secondary battery is thermally decomposed at 350 ° C.
  • the thermal decomposition temperature is low, the treatment time becomes long and the efficiency is poor.
  • the thermal decomposition temperature is too high, aluminum (melting point: 660 ° C.) contained in the casing and the positive electrode current collector may be melted, and the processing cost is increased, so the thermal decomposition temperature is preferably 350 ° C. to 550 ° C. Is carried out at 400 ° C to 500 ° C. In the case of 400 ° C. to 500 ° C., the thermal decomposition is further promoted, so that a more preferable effect can be obtained that the plastic is easily carbonized and hardly melted.
  • the heat treatment time of the lithium ion secondary battery is 20 to 60 minutes. If it is less than 20 minutes, thermal decomposition becomes insufficient, and the plastic is not carbonized and becomes dross. Moreover, if it exceeds 60 minutes, the loss of heat energy will generate
  • the impact crusher for example, a hammer mark crusher, a rotary impact mill, or the like can be employed.
  • a shearing type crusher a uniaxial shear crusher, a biaxial shear crusher, etc. are employable, for example. If the classification point at the time of primary classification is less than 0.15 mm, the recovery rate of the rare metal recovered under the sieve is low. Moreover, if this classification point exceeds 0.60 mm, the collection of the recovered material collected under the sieve increases the mixing of copper, aluminum, etc., and the rare metal quality of the recovered product is lowered.
  • the vibration mill for example, a vibration ball mill, a vibration rod mill, or the like can be employed.
  • the classification points for secondary classification are the same as those for primary classification. Therefore, the primary classification sieve can be reused even in the secondary classification.
  • a sieve for secondary classification may be used. If the classification point of secondary classification is less than 0.15 mm, the recovery rate of the rare metal recovered under the sieve is low. Moreover, if this classification point exceeds 0.60 mm, the collection of the recovered material collected under the sieve increases the mixing of copper, aluminum, etc., and the rare metal quality of the recovered product is lowered. Examples of rare metals recovered from the sieve after the secondary classification include cobalt, nickel, manganese, and lithium obtained from the positive electrode material.
  • the invention according to claim 2 is the method for recovering valuable metals from the waste lithium ion secondary battery according to claim 1, wherein the lithium metal oxide contains one or more of cobalt, nickel and manganese and lithium. It is.
  • the waste lithium ion secondary battery is subjected to a thermal decomposition process using superheated steam, a primary crushing process using an impact crusher or a shear crusher, and a classification point of 0.15 mm to 0.
  • Primary classification step with 60 mm sieve, secondary crushing step with vibration mill of positive electrode current collector and negative electrode current collector obtained from sieve, secondary classification step with sieve having classification point of 0.15 mm to 0.60 mm Are applied sequentially.
  • the organic substance contained in the lithium ion secondary battery can be thermally decomposed at a low cost while suppressing the oxidation of metal and the generation of dioxins, and the aluminum (melting point 660) contained in the casing and the positive electrode current collector.
  • the recovery rate of valuable metals contained in the positive electrode material can be increased as compared with the conventional method.
  • the thermal decomposition step (S101) and the primary are performed on the waste lithium ion secondary battery.
  • the crushing step (S102), the primary classification step (S103), the secondary crushing step (S104), and the secondary classification step (S105) are sequentially performed.
  • these steps will be specifically described.
  • a waste lithium ion secondary battery from which valuable metals are recovered is a negative electrode made of copper foil by applying a positive electrode material made of lithium cobalt oxide (LiCoO 2 ) to the front and back surfaces of a positive electrode current collector made of aluminum foil.
  • a negative electrode material which is a carbon material (graphite) is applied to the front and back surfaces of the current collector to form a negative electrode body.
  • a separator is inserted between the positive electrode body and the negative electrode body, and these are wound and compressed. These are sealed in the outer case by attaching accessory parts such as a conductive handle, a leakage pressure safety valve, and an end lid after the inner case is inserted and the electrolyte solution is filled in the inner space of the outer case.
  • the exterior case is a case in which a casing made of stainless steel and aluminum is covered with a plastic case made of a plastic laminated composite.
  • a plastic case made of a plastic laminated composite.
  • accessory parts such as a conductive handle, a leak pressure safety valve and an end cover is not mentioned.
  • the waste lithium ion secondary battery is heat-treated using a superheated steam pyrolyzer capable of continuously heat-treating.
  • the superheated steam thermal decomposition apparatus continuously supplies a waste lithium ion secondary battery to the heat treatment chamber, a heat treatment chamber for heat treating the waste lithium ion secondary battery, a superheated steam generator for supplying the heat treatment chamber with the superheated steam.
  • a conveyor A large number of waste lithium ion secondary batteries are put into a heat treatment chamber by a conveyor, where they are heated for 45 minutes by superheated steam at 600 to 750 ° C (the actual heat treatment temperature of the secondary battery is 400 ° C) generated by the superheated steam generator. Then, organic solvents and organic substances such as plastic cases and separators are pyrolyzed.
  • the superheated steam used at this time is the same oxygen-free gas as the inert gas. Therefore, ignition of flammable organic solvents is suppressed, deterioration due to metal oxidation is prevented, quality is not deteriorated, and heat treatment can be safely performed without risk of explosion, and generation of dioxins is also possible. Can be suppressed.
  • the heating medium of superheated steam is water, it can be heat-treated at a lower cost than conventional inert gases.
  • the heat treatment temperature of the waste lithium ion secondary battery is set to 400 ° C., an organic substance containing an organic solvent can be efficiently heat-treated in a short time.
  • the heat-treated waste lithium ion secondary battery (heat-treated product) is first crushed by a Hanmark crusher which is a kind of impact crusher.
  • the Hanmark lasher has a rooster in which a large number of holes having a diameter of 18 mm are formed.
  • the cathode material containing cobalt and lithium as rare metals and the anode material of graphite are pulverized, and the casing made of stainless steel and aluminum in the outer casing, the cathode current collector made of aluminum foil, and the anode made of copper foil
  • the current collector is crushed with a relatively large size.
  • the primary crushed material of the waste lithium ion secondary battery discharged from the Hanmark crusher is subjected to primary classification using a sieve having a classification point (sieve) of 0.15 mm.
  • a sieve having a classification point (sieve) of 0.15 mm.
  • the secondary crushing step (S104) a large number of steel balls having a diameter of 20 to 30 mm are introduced into the casing, the positive electrode current collector, and the negative electrode current collector obtained from the screen of the primary classification sieve, and vibration crushing is performed. Secondary crushing with a vibrating ball mill. At this time, the residue of the positive electrode material adhering to the positive electrode current collector and the residue of the negative electrode material adhering to the negative electrode current collector are pulverized and peeled off from the front and back surfaces of the corresponding current collector.
  • the secondary crushed material discharged from the vibration ball mill is subjected to secondary classification using a sieve having the same mesh as that for primary classification (secondary classification step).
  • casing stainless steel, aluminum
  • a positive electrode collector aluminum
  • and a negative electrode collector can be collect
  • cobalt and lithium in the positive electrode material and graphite in the negative electrode material can be recovered from under the sieve.
  • the recovery rate of valuable metals including rare metals from waste lithium ion secondary batteries can be increased as compared with the conventional method.
  • the recovered rare metal (lithium, cobalt, nickel, manganese, etc.) is reused as a catalyst, a battery positive electrode material, a refining raw material, etc., for example, after being wet-treated or dry-treated.
  • This invention is useful as a technique for reducing the amount of waste disposal of used lithium ion secondary batteries and securing metal resources through circulation.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Selon l'invention, les accumulateurs au lithium-ion mis aux rebuts sont chauffés à l'aide d'une vapeur surchauffée à une température de 350-550°C afin de pyrolyser les substances organiques présentes dans les accumulateurs. Ensuite, les résidus sont soumis successivement à un broyage primaire dans un broyeur, à un classement primaire avec un point de classement de 0,15-0,60 mm et à un broyage secondaire dans lequel les collecteurs de courant qui restent sur le tamis sont broyés dans un broyeur à vibration. Un classement secondaire est ensuite réalisé, dans lequel le produit du broyage secondaire est classé en utilisant le même point de classement et les résidus des matériaux d'électrodes positives qui contiennent des métaux rares sont récupérés au-dessous du tamis. De cette manière, les substances organiques présentes dans les accumulateurs peuvent être pyrolysées économiquement tout en empêchant une oxydation des métaux et une production de dioxines. Par ailleurs, comme les collecteurs de courant pour électrodes positives, qui sont faits en aluminium, ne fondent pas, les métaux de valeur présents dans les matériaux des électrodes positives sont récupérés dans une large mesure.
PCT/JP2011/063392 2011-06-10 2011-06-10 Procédé de récupération de métaux de valeur dans les accumulateurs au lithium-ion mis aux rebuts Ceased WO2012169073A1 (fr)

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EP4198151A1 (fr) * 2021-12-16 2023-06-21 Northvolt Revolt AB Procédé de récupération de concentré de matériau actif de batterie
JP2023158921A (ja) * 2022-04-19 2023-10-31 松田産業株式会社 リチウムイオン二次電池からの有価物の回収方法
KR20240106688A (ko) * 2022-12-29 2024-07-08 한국지질자원연구원 폐리튬이온전지내 금속 회수를 위한 부유선별방법, 다단 부유선별방법 및 시스템
US12370557B2 (en) 2017-05-30 2025-07-29 Li-Cycle Corp. Process, apparatus, and system for recovering materials from batteries
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