JP5112526B2 - リチウム二次電池用金属酸化物系正極活物質の再処理及び合成方法 - Google Patents
リチウム二次電池用金属酸化物系正極活物質の再処理及び合成方法 Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/049—Manufacturing of an active layer by chemical means
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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
- 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
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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
- 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
-
- 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
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- 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
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
[実施例1]
リチウム二次電池の3成分系正極活物質LiCo1/3Ni1/3Mn1/3O2を採取して粉末に粉砕した原料10grを、亜硫酸ガスを飽和するまで注入した体積モル濃度が0.5Mの硫酸水溶液1000mlと共に反応器に入れた。この状態で、常温で攪拌しながら1時間溶解した。
実施例1と同一のリチウム二次電池の3成分系正極活物質LiCo1/3Ni1/3Mn1/3O2粉末原料50grを取り、亜硫酸ガスを飽和するまで注入した体積モル濃度が2Mの硫酸水溶液1000mlと共に実施例1と同一の装置の反応器に入れた。この状態で、実施例1と同様に常温で攪拌しながら1時間溶解した。
実施例1及び2とは異なり、原料物質としてリチウム二次電池の3成分系正極活物質LiNi0.5Co0.2Mn0.3O2を採取して粉末に粉砕した原料10grを取り、亜硫酸ガスを飽和するまで注入した体積モル濃度が0.5Mの硫酸水溶液1000mlと共に反応器に入れた。この状態で、実施例1と同様に常温で攪拌しながら1時間溶解した。
リチウム二次電池の2成分系正極活物質LiNi0.8Co0.18Al0.02O2を採取して粉末に粉砕した原料10grを、亜硫酸ガスを飽和するまで注入した体積モル濃度が0.5Mの硫酸水溶液1000mlと共に反応器に入れた。この状態で、実施例1と同様に常温で攪拌しながら1時間溶解した。
実施例1のリチウム二次電池の3成分系正極活物質LiCo1/3Ni1/3Mn1/3O2を採取して粉末に粉砕した原料10grを取り、体積モル濃度が6Mの硫酸水溶液1000mlと共に反応器に入れた。亜硫酸ガスの飽和は実施しなかった。このとき、還元剤として濃度35%の過酸化水素100mlを共に添加して、硫酸水溶液の体積が1000mlとなるようにした。この状態で、70℃で攪拌しながら1時間溶解した。
実施例3のリチウム二次電池の3成分系正極活物質LiNi0.5Co0.2Mn0.3O2を採取して粉末に粉砕した原料10grを取り、体積モル濃度が6Mの硫酸水溶液1000mlと共に反応器に入れた。比較例1と同様に亜硫酸ガスの飽和は実施しなかった。このとき、還元剤として濃度35%の過酸化水素100mlを共に添加して、硫酸水溶液の体積が1000mlとなるようにした。この状態で、70℃で攪拌しながら1時間溶解した。
Claims (9)
- (a)亜硫酸ガスを含む硫酸水溶液を用いて廃リチウム二次電池から正極活物質を溶解して金属イオンを含む溶液を形成する第1段階と、
(b)前記金属イオンを含む溶液に水酸化ナトリウム溶液及びアンモニア水溶液を注入して電極活物質前駆体を形成する第2段階と、
を含むリチウム二次電池用金属酸化物系正極活物質の再処理方法。 - (c)前記電極活物質前駆体を濾過、乾燥、及び粉砕して固体状の正極活物質前駆体を得る第3段階をさらに含む請求項1に記載のリチウム二次電池用金属酸化物系正極活物質の再処理方法。
- 前記硫酸水溶液の体積モル濃度が0.5M〜2Mであり、前記亜硫酸ガスが前記硫酸水溶液に飽和状態で含まれる請求項1に記載のリチウム二次電池用金属酸化物系正極活物質の再処理方法。
- 前記金属イオンを含む溶液中の正極活物質の濃度が10g/L〜50g/Lである請求項1に記載のリチウム二次電池用金属酸化物系正極活物質の再処理方法。
- 前記第2段階(b)において、
前記金属イオンを含む溶液中の金属イオンの体積モル濃度が1M〜6Mであり、注入される前記水酸化ナトリウム溶液の体積モル濃度は前記金属イオンを含む溶液中の前記金属イオン濃度の2倍である請求項1に記載のリチウム二次電池用金属酸化物系正極活物質の再処理方法。 - 前記第2段階(b)において、
前記アンモニア水溶液の体積モル濃度が6M〜13Mである請求項1に記載のリチウム二次電池用金属酸化物系正極活物質の再処理方法。 - 請求項1に記載の方法で形成された電極活物質前駆体と、炭酸リチウム又は水酸化リチウムとを混合して熱処理し、金属酸化物系正極活物質を形成するリチウム二次電池用金属酸化物系正極活物質の合成方法。
- 前記電極活物質前駆体と、炭酸リチウム又は水酸化リチウムとのモル比が1:1.0〜1:1.3である請求項7に記載のリチウム二次電池用金属酸化物系正極活物質の合成方法。
- 前記熱処理が空気又は酸素雰囲気下で600℃〜1000℃で行われる請求項7に記載のリチウム二次電池用金属酸化物系正極活物質の合成方法。
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KR20100092676A KR101191154B1 (ko) | 2010-09-20 | 2010-09-20 | 리튬이차전지용 금속산화물계 양극활물질의 재처리 및 합성 방법 |
KR10-2010-0092676 | 2010-09-20 |
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JP2012064557A JP2012064557A (ja) | 2012-03-29 |
JP2012064557A5 JP2012064557A5 (ja) | 2012-10-18 |
JP5112526B2 true JP5112526B2 (ja) | 2013-01-09 |
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JP2011007943A Expired - Fee Related JP5112526B2 (ja) | 2010-09-20 | 2011-01-18 | リチウム二次電池用金属酸化物系正極活物質の再処理及び合成方法 |
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US (1) | US8835026B2 (ja) |
JP (1) | JP5112526B2 (ja) |
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US11955613B2 (en) | 2012-04-04 | 2024-04-09 | Worcester Polytechnic Institute | Charge material for recycled lithium-ion batteries |
KR101294335B1 (ko) | 2012-05-25 | 2013-08-16 | 한국과학기술연구원 | 재활용을 통한 리튬 이차전지용 리튬인산철 양극활물질의 제조 방법, 이에 따라 제조된 리튬 이차전지용 리튬인산철 양극활물질, 리튬인산철 양극 및 리튬 이차전지 |
JP6159228B2 (ja) | 2012-11-07 | 2017-07-05 | 株式会社半導体エネルギー研究所 | 非水系二次電池用正極の製造方法 |
KR101439427B1 (ko) | 2013-03-14 | 2014-09-11 | 한국과학기술연구원 | 리튬이차전지용 올리빈계 양극소재의 재활용 방법, 이에 의하여 제조된 양극소재, 이를 포함하는 리튬이차전지용 양극 및 리튬이차전지 |
WO2015041381A1 (ko) * | 2013-09-17 | 2015-03-26 | 국립대학법인 울산과학기술대학교 산학협력단 | 리튬 이차 전지 및 리튬 이차 전지 시스템 |
CN103618093A (zh) * | 2013-10-31 | 2014-03-05 | 中南大学 | 一种铝电池用铝合金阳极材料热处理方法 |
JP6312576B2 (ja) * | 2014-10-29 | 2018-04-18 | 信越化学工業株式会社 | リチウム複合酸化物の再生方法、電気化学デバイスの製造方法、並びに、リチウムイオン二次電池の製造方法 |
JP6294219B2 (ja) * | 2014-12-25 | 2018-03-14 | 信越化学工業株式会社 | リチウムコバルト系複合酸化物の製造方法 |
JP6374348B2 (ja) * | 2015-05-18 | 2018-08-15 | 信越化学工業株式会社 | リチウムリン系バナジウム複合酸化物炭素複合体、及びその製造方法、リチウムイオン二次電池、並びに、電気化学デバイス |
CN107326181B (zh) * | 2017-05-26 | 2018-11-09 | 金川集团股份有限公司 | 废旧锂离子电池剥离浸出一步完成的回收方法 |
CN109921120B (zh) * | 2017-12-13 | 2020-12-22 | 中国科学院过程工程研究所 | 一种三元正极材料制备过程中废弃耐火材料回收处理的方法 |
CN109449434B (zh) * | 2018-09-20 | 2021-08-20 | 广东佳纳能源科技有限公司 | 一种利用废旧锂离子电池制备三元锂电池正极材料前驱体的方法 |
KR20200133459A (ko) * | 2019-05-20 | 2020-11-30 | 에스케이이노베이션 주식회사 | 리튬 전구체 분리 방법 및 리튬 전구체 분리 시스템 |
KR20210147597A (ko) * | 2020-05-29 | 2021-12-07 | 주식회사 엘지에너지솔루션 | 양극 스크랩을 이용한 활물질 재사용 방법 |
KR20220025410A (ko) * | 2020-08-24 | 2022-03-03 | 주식회사 엘지에너지솔루션 | 양극 스크랩을 이용한 활물질 재사용 방법 |
KR20220042663A (ko) * | 2020-09-28 | 2022-04-05 | 주식회사 엘지에너지솔루션 | 양극 스크랩을 이용한 활물질 재사용 방법 |
KR102689694B1 (ko) * | 2020-10-16 | 2024-07-29 | 주식회사 엘지에너지솔루션 | 양극 스크랩을 이용한 활물질 재사용 방법 |
CN113151680B (zh) * | 2021-02-08 | 2023-06-16 | 中国科学院宁波材料技术与工程研究所 | 一种废旧锂电池回收再利用的方法 |
CN113522868B (zh) * | 2021-06-29 | 2022-12-13 | 格林美(湖北)新能源材料有限公司 | 一种去除正极材料表面残碱的洗涤方法 |
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CA2319285A1 (en) * | 2000-09-13 | 2002-03-13 | Hydro-Quebec | A method for neutralizing and recycling spent lithium metal polymer rechargeable batteries |
JP4475941B2 (ja) | 2003-12-12 | 2010-06-09 | 日本化学工業株式会社 | リチウムマンガンニッケル複合酸化物の製造方法 |
JP4767798B2 (ja) * | 2006-09-05 | 2011-09-07 | 住友大阪セメント株式会社 | 電極材料の製造方法、リチウムの回収方法、正極材料及び電極並びに電池 |
KR100975317B1 (ko) | 2009-11-20 | 2010-08-12 | 한국지질자원연구원 | 망간 및 아연을 함유하는 폐전지로부터의 황산망간 및 황산아연 제조방법 |
KR101069807B1 (ko) * | 2010-04-14 | 2011-10-04 | 한국과학기술연구원 | 리튬전지 양극활물질로부터 코발트를 전해 환원 추출하는 방법 |
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US20120068107A1 (en) | 2012-03-22 |
KR101191154B1 (ko) | 2012-10-15 |
KR20120030865A (ko) | 2012-03-29 |
JP2012064557A (ja) | 2012-03-29 |
US8835026B2 (en) | 2014-09-16 |
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