WO2011065682A2 - Procédé de production de catalyseur cmb recyclé à partir d'une batterie au lithium-ion et de matières de cathode ternaires - Google Patents

Procédé de production de catalyseur cmb recyclé à partir d'une batterie au lithium-ion et de matières de cathode ternaires Download PDF

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Publication number
WO2011065682A2
WO2011065682A2 PCT/KR2010/007750 KR2010007750W WO2011065682A2 WO 2011065682 A2 WO2011065682 A2 WO 2011065682A2 KR 2010007750 W KR2010007750 W KR 2010007750W WO 2011065682 A2 WO2011065682 A2 WO 2011065682A2
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solvent
solution
cobalt
manganese
extraction
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PCT/KR2010/007750
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English (en)
Korean (ko)
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WO2011065682A3 (fr
Inventor
신선명
강진구
주성호
장한권
손정수
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한국지질자원연구원
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Priority to CN2010800535942A priority Critical patent/CN102665912A/zh
Priority to JP2012541932A priority patent/JP5572222B2/ja
Publication of WO2011065682A2 publication Critical patent/WO2011065682A2/fr
Publication of WO2011065682A3 publication Critical patent/WO2011065682A3/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/68—Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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 a method for recovering cobalt and manganese from waste battery materials, and to a method for producing a Co-Mn-Br liquid catalyst using the same, more specifically, in the process of manufacturing waste lithium ion battery powder and ternary cathode active material.
  • Cobalt and manganese recovery method characterized by recovering cobalt and manganese by sequentially applying a sulfuric acid reduction leaching, neutralization titration, solid-liquid separation, solvent extraction and water washing process to the generated scrap, and the cobalt and It relates to a method for preparing a Co-Mn-Br liquid catalyst using an extract containing manganese.
  • Lithium secondary batteries which have recently increased in usage among lithium batteries, are composed of a cathode, an anode, an organic electrolyte, and an organic separator.
  • lithium cobalt oxide which has excellent reversibility, low self discharge rate, high capacity and high energy density, and is easily synthesized, is commercially available as a positive electrode active material.
  • lithium-ion batteries are widely used as a power source for small portable devices due to their light weight, and in recent years, demand for them has increased in proportion to the explosion of mobile communication terminals.
  • the amount of generated lithium ion batteries is also rapidly increasing.
  • This waste lithium ion battery is simple in appearance and contains a large amount of valuable metals such as lithium and cobalt, which are relatively expensive as a cathode active material, and thus, it is recognized as an economically valuable waste resource and requires recycling.
  • valuable metals such as cobalt and lithium should be recycled, and for efficient recycling of lithium ion batteries, not only efficient recovery of valuable metals but also recycling of waste lithium batteries Hazardous wastes generated should be properly disposed of.
  • CMB liquid catalyst is a catalyst composed of Co-Mn-Br, and is used as a catalyst for producing TPA (Terephthalic Acid) by oxidizing para-xylene, one of petrochemical products.
  • TPA Tephthalic Acid
  • TPA becomes a raw material for polyester fiber, PET (Polyethylene Terephthalate) bottles, films, paints, and tire cords that are closely related to our lives. Korea is a major producer of TPA.
  • domestic TPA production amounted to 5.5 million tons.
  • the market for CMB catalysts is huge. Therefore, by recovering Co and Mn from the waste containing Co and Mn discarded in the process, it is possible to economically produce a CMB catalyst.
  • the present inventors have made diligent efforts to develop an efficient cobalt and manganese recovery method from scrap generated during the production of waste lithium ion batteries and ternary cathode active materials.
  • separation and solvent extraction and water washing processes were sequentially applied, it was confirmed that the high-purity cobalt and manganese from which impurities were removed were recovered, and that the CMB liquid catalyst could be prepared using the same, thereby completing the present invention. It became.
  • the present invention comprises the steps of: (a) leaching with respect to the spent battery material using sulfuric acid and a reducing agent; (b) neutralizing the leaching solution obtained in step (a) to remove impurities; (c) solid-liquid separation of the leaching solution obtained in step (b) into a solution and a residue; (d) extracting by adding a solvent to the solution liquid-separated in step (c); And (e) provides a method for recovering cobalt and manganese comprising the step of washing the extract obtained in step (d).
  • the present invention also comprises the steps of: (f) adding a HBr solution to the extract obtained in the recovery method of cobalt and manganese, back extraction to obtain a Co-Mn-Br stripping solution; And (g) adding a cobalt salt and a manganese salt to the Co-Mn-Br stripping solution to adjust an appropriate concentration to prepare a Co-Mn-Br liquid catalyst using cobalt and manganese recovered from a waste battery material.
  • a method is a method.
  • 1 is a process chart for the preparation of Co-Mn-Br-based liquid catalyst.
  • FIG. 2 is a schematic diagram of a recovery simulation test of major elements using 40% saponification solvent of 0.7M Cyanex 272.
  • FIG. 2 is a schematic diagram of a recovery simulation test of major elements using 40% saponification solvent of 0.7M Cyanex 272.
  • 3 is a schematic diagram of the recovery simulation test of the main elements using 45% saponification solvent of 0.85M Cyanex 272.
  • the present invention in one aspect, (a) leaching with respect to the spent battery material using sulfuric acid and a reducing agent; (b) neutralizing the leaching solution obtained in step (a) to remove impurities; (c) solid-liquid separation of the leaching solution obtained in step (b) into a solution and a residue; (d) extracting by adding a solvent to the solution liquid-separated in step (c); And (e) relates to a method for recovering cobalt and manganese comprising the step of washing the extract obtained in step (d).
  • the waste battery material may be scrap generated in the process of manufacturing the waste lithium ion battery and the ternary cathode active material.
  • the waste lithium ion battery may be in a powder state, it is preferable to use a powder of 8 mesh or less in the method of the present invention.
  • the waste lithium ion battery powder may be obtained by a physical treatment method of Korean Patent No. 860972, which is a prior patent of the present inventors.
  • the waste battery material may be a cathode material rejected material or a cathode active material scrap generated in the process of manufacturing a lithium ion battery cathode material, and ternary cathode by separating into a powder form through simple crushing and heat treatment. It may be recovered as an active material powder.
  • the waste battery material contains a large amount of impurities in addition to valuable metals such as cobalt and lithium. Therefore, in order to remove impurities from the solution obtained after leaching the waste battery material using sulfuric acid and a reducing agent in step (a), neutralization titration is performed.
  • the reducing agent may be H 2 , H 2 S, SO 2 , FeSO 4 , coal (pyal) or pyrite (Pyrite), preferably H 2 O 2 may be used.
  • the neutralization titration of step (b) is a calcium compound selected from the group consisting of CaO, Ca (OH) 2 and CaCO 3 ; Alkaline solution which is NaOH or NH 4 OH; And it can be adjusted to pH 5.5 ⁇ 6.5 by a material selected from the group consisting of a mixture thereof, preferably CaCO 3 can be used.
  • Impurities that can be removed from the leaching solution by neutralization titration may be selected from the group consisting of Fe, Cu, Al and mixtures thereof, but is limited to impurities other than recyclable valuable metals such as Co and Mn. It doesn't happen.
  • the solid-liquid separation of step (c) can be separated into a solution and a residue using a filter press or filter paper, and the solid-liquid separation means can be easily selected by those skilled in the art.
  • the solvent used in the step (d) is di-2-ethyl hexyl phosporic acid, 2-ethyl hexyl phosphonic acid, mono-2-ethyl hexyl ester, di-2,4,4- trimethyl penthyl phosphonic acid, di-2-ethyl hexyl phosphinic acid, di-2,4,4-trimethyl penthyl dithiophosphinic acid and di-2,4,4-trimethyl penthyl monothiophosphinic acid
  • the di-2-ethyl hexyl phosporic acid solvent may be used.
  • the solvent is preferably saponified by an alkaline solution, and in this case, 30 to 60% saponified solvent may be used, and preferably 40 to 50% saponified solvent may be used to increase the recovery rate of cobalt and manganese and to remove impurities. Occurrence can be minimized.
  • saponifying the solvent used during the solvent extraction can prevent the pH change during solvent extraction to increase the efficiency of solvent extraction.
  • the Cyanex 272 has a molecular weight of 290, viscosity 142cp (25 °C), specific gravity 0.92gm / cc (24 °C) and purity of 85%, the molecular formula is C 16 H 34 PO 2 H, has the same structure as formula (I).
  • Scheme (2) is a reaction formulating the saponification process of the solvent, and the H + ions of the solvent is replaced with Na + or NH 4 + ions, and thus when cobalt or manganese ions are extracted by the solvent as in Scheme (3)
  • the Na + or NH 4 + ions substituted in the reaction scheme (2) are discharged into the solution phase, it is possible to prevent the pH change of the solution.
  • the water washing step of step (e) of the present invention is a ratio of O / A (Organic / Aqueous) to the solvent extracted using a distilled water of 50 °C to 70 °C in a condition of 10: 1 to 1:10 It can be washed within minutes, and preferably, using distilled water at 60 ° C. under O / A (Organic / Aqueous) condition of 2: 1.
  • the 'extraction solution' may be mixed with 'extraction solvent' or 'extraction solvent' extracted by Cyanex 272, and the extraction solvent used in the Co-Mn-Br liquid catalyst preparation method is cobalt and manganese.
  • the extract obtained in step (d) or step (e) of the recovery method can be used as the starting solvent.
  • the waste battery material may be scrap generated in the process of manufacturing the waste lithium ion battery and the ternary cathode active material.
  • the waste lithium ion battery may be in a powder state, it is preferable to use a powder of 8 mesh or less in the method of the present invention.
  • the Co-Mn-Br stripping solution obtained by the reverse extraction (removal) step of the present invention may be used as a Co-Mn-Br liquid catalyst, and thus the content of each component may not reach an appropriate amount.
  • a stripping solution may be obtained using an HBr solution.
  • an appropriate concentration of cobalt salt and manganese salt may be further mixed with the stripping solution to achieve a proper content ratio of the Co-Mn-Br liquid catalyst.
  • the cobalt salt and manganese salt may be CoBr 2 (Cobalt bromide), MnBr 2 (Maganese Bromide) and Mn (OAc) 2 (maganese acetate), to prepare a Co-Mn-Br liquid catalyst.
  • the amount of cobalt, manganese, and bromine in the first Co-Mn-Br stripping solution was added so that the amount of Co, Mn, and Br, which are the CMB liquid catalyst components, was 0.51 M, 1.09 M, and 1.91 M, respectively. Can be determined.
  • the waste lithium ion battery powder was obtained by physical treatment as disclosed in Korean Patent No. 860972, and the scrap generated in the process of manufacturing the ternary positive electrode active material is formed in the form of powder through simple crushing and heat treatment. Separated and used in powder form.
  • the cobalt bromide, manganese bromide and manganese acetate were added to prepare the CMB liquid catalyst from the stripping solution, which is an intermediate product of the CMB liquid catalyst, because each component contained in the stripping solution was insufficient in forming the CMB liquid catalyst. It was prepared by.
  • the amount required to prepare the CMB liquid catalyst is different depending on the extraction conditions, and according to the component analysis was added to the concentration of Co-Mn-Br in the concentration of [Table 18] to the same as the CMB spec.
  • Table 20 2 step count-current simulation extraction using 40% saponified solvent Loading Co Ni Li Mn Cu Fe Al 1st stage extraction rate 6.9 -20.5 -1.0 79.9 71.9 -14.7 -83.9 2-stage extraction rate 99.6 -136.1 -7.5 99.7 93.3 -34.1 64.5
  • Table 22 2 step count-current simulation extraction using 45% saponified solvent (%) Loading Co Ni Li Mn 1st stage extraction rate -14.1 -34.4 -1.6 55.2 2-stage extraction rate 99.8 -25.1 0.3 100.0
  • the recovery solution Is useful as a raw material for the production of CMB liquid catalysts.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
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Abstract

La présente invention porte sur la récupération de cobalt et de manganèse à partir de matières de batteries mises au rebut et sur un procédé de fabrication de catalyseurs liquides à partir de Co-Mn-Br (CMB) récupéré. De façon plus spécifique, de la poudre de lithium-ion et des matières de cathode ternaires sont produites par lixiviation de matières de batteries mises au rebut avec réduction des sulfates et application séquentielle des trois étapes de traitement suivantes : un titrage de neutralisation, une séparation solide-liquide et une extraction au solvant, ce qui conduit à la récupération de cobalt et de manganèse sous forme d'un extrait liquide constitué d'un catalyseur Co-Mn-Br. Selon la présente invention, un catalyseur CMB en phase liquide qui est utile pour une application dans divers procédés de fabrication est fourni par récupération de cobalt et de manganèse à partir de matières de cathode ternaires et de batteries au lithium-ion mises au rebut, amélioration de l'élimination d'autres impuretés et récupération de cobalt et de manganèse de haute pureté.
PCT/KR2010/007750 2009-11-30 2010-11-04 Procédé de production de catalyseur cmb recyclé à partir d'une batterie au lithium-ion et de matières de cathode ternaires WO2011065682A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN2010800535942A CN102665912A (zh) 2009-11-30 2010-11-04 从锂离子电池和三元正极材料制备cmb催化剂的方法
JP2012541932A JP5572222B2 (ja) 2009-11-30 2010-11-04 リチウムイオン電池及び三元系正極活物質からのｃｍｂ液相触媒の製造方法

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KR10-2009-0116570 2009-11-30
KR20090116570A KR101089519B1 (ko) 2009-11-30 2009-11-30 리튬이온전지 및 3원계 양극활물질로부터 ｃｍｂ 촉매 제조방법

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JP2013076108A (ja) * 2011-09-29 2013-04-25 Jx Nippon Mining & Metals Corp アルミニウム及びマンガンの分離方法
JP2014156648A (ja) * 2013-02-18 2014-08-28 Jx Nippon Mining & Metals Corp 廃正極材及び廃電池からの金属回収方法
JP2014156649A (ja) * 2013-02-18 2014-08-28 Jx Nippon Mining & Metals Corp 廃正極材及び廃電池からの金属回収方法
CN107002171A (zh) * 2014-09-30 2017-08-01 捷客斯金属株式会社 锂离子电池废料的浸出方法、及来自于锂离子电池废料的金属的回收方法
EP3431619A4 (fr) * 2016-03-16 2019-11-20 JX Nippon Mining & Metals Corporation Procédé de traitement de déchets de batterie au lithium-ion
EP3431618A4 (fr) * 2016-03-16 2019-11-20 JX Nippon Mining & Metals Corporation Procédé de traitement de batteries lithium-ion usagées
CN116103499A (zh) * 2023-02-16 2023-05-12 西安金藏膜环保科技有限公司 一种双光电极光电催化废旧锂电池有价金属浸出的方法

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JP5706457B2 (ja) * 2013-02-27 2015-04-22 Jx日鉱日石金属株式会社 金属混合溶液からの金属の分離回収方法
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KR101528507B1 (ko) 2015-01-13 2015-06-12 한국지질자원연구원 리튬계 전지로부터 코발트 및 망간의 동시 회수 방법
CN108011144B (zh) * 2017-10-31 2019-09-13 合肥国轩高科动力能源有限公司 一种锂离子电池三元正极材料的回收处理工艺
EP3729554B1 (fr) * 2017-12-19 2022-03-09 Basf Se Recyclage des batteries par traitement du lixiviat avec du nickel métallique
KR102206952B1 (ko) * 2019-04-22 2021-01-25 코스모에코켐(주) 폐양극활물질분말로부터 전구체 제조를 위한 혼합금속화합물의 제조방법
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JP7365846B2 (ja) * 2019-10-16 2023-10-20 Ｊｘ金属株式会社 高純度硫酸コバルト溶液の製造方法及び、硫酸コバルトの製造方法
CN113802002B (zh) * 2021-08-17 2022-11-15 广东邦普循环科技有限公司 湿法回收锂电池中有价金属的方法
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JP2003203680A (ja) * 2002-01-08 2003-07-18 Sumitomo Metal Mining Co Ltd 使用済みニッケル水素二次電池からの有価金属回収方法
KR20090087801A (ko) * 2008-02-13 2009-08-18 닛코 킨조쿠 가부시키가이샤 Ｃｏ, Ｎｉ, Ｍｎ 함유 리튬 전지 찌꺼기로부터의 유가 금속 회수 방법

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JP2013076108A (ja) * 2011-09-29 2013-04-25 Jx Nippon Mining & Metals Corp アルミニウム及びマンガンの分離方法
JP2014156648A (ja) * 2013-02-18 2014-08-28 Jx Nippon Mining & Metals Corp 廃正極材及び廃電池からの金属回収方法
JP2014156649A (ja) * 2013-02-18 2014-08-28 Jx Nippon Mining & Metals Corp 廃正極材及び廃電池からの金属回収方法
CN107002171A (zh) * 2014-09-30 2017-08-01 捷客斯金属株式会社 锂离子电池废料的浸出方法、及来自于锂离子电池废料的金属的回收方法
EP3431619A4 (fr) * 2016-03-16 2019-11-20 JX Nippon Mining & Metals Corporation Procédé de traitement de déchets de batterie au lithium-ion
EP3431618A4 (fr) * 2016-03-16 2019-11-20 JX Nippon Mining & Metals Corporation Procédé de traitement de batteries lithium-ion usagées
US10807879B2 (en) 2016-03-16 2020-10-20 Jx Nippon Mining & Metals Corporation Processing method for lithium ion battery scrap
US10865462B2 (en) 2016-03-16 2020-12-15 Jx Nippon Mining & Metals Corporation Processing method for lithium ion battery scrap
CN116103499A (zh) * 2023-02-16 2023-05-12 西安金藏膜环保科技有限公司 一种双光电极光电催化废旧锂电池有价金属浸出的方法

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JP2013512345A (ja) 2013-04-11
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KR20110060089A (ko) 2011-06-08
KR101089519B1 (ko) 2011-12-05
CN102665912A (zh) 2012-09-12

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