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WO2014042136A1 - Procédé de recyclage de batteries au lithium-ion et dispositif associé - Google Patents

Procédé de recyclage de batteries au lithium-ion et dispositif associé Download PDF

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Publication number
WO2014042136A1
WO2014042136A1 PCT/JP2013/074327 JP2013074327W WO2014042136A1 WO 2014042136 A1 WO2014042136 A1 WO 2014042136A1 JP 2013074327 W JP2013074327 W JP 2013074327W WO 2014042136 A1 WO2014042136 A1 WO 2014042136A1
Authority
WO
WIPO (PCT)
Prior art keywords
lithium
peeling
crystallization
oil phase
leaching
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2013/074327
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English (en)
Japanese (ja)
Inventor
佐伯　智則
芝田　隼次
田中　智史
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hitachi Ltd
Original Assignee
Hitachi Ltd
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Filing date
Publication date
Application filed by Hitachi Ltd filed Critical Hitachi Ltd
Publication of WO2014042136A1 publication Critical patent/WO2014042136A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
    • B09B3/35—Shredding, crushing or cutting
    • 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
    • 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
    • C22B3/44—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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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 and apparatus for recycling lithium ion batteries, and more particularly, to a method for producing lithium salts, cobalt salts, and the like from waste lithium ion batteries.
  • Lithium ion batteries are widely used in a wide range of electronic and electrical devices such as mobile phones, notebook computers, digital cameras and video as small and large capacity secondary batteries. The amount of use is said to increase further in the future for hybrid electric vehicles (HEV) and electric vehicles (EV). While the amount of use increases, many waste products are born.
  • Lithium ion batteries include iron-based materials or aluminum as containers, copper as negative electrode current collector materials, carbon as negative electrode active material, aluminum as positive electrode current collector material, lithium compounds as positive electrode active material, etc.
  • the positive electrode active material includes rare metals (so-called rare metals) such as lithium, cobalt, and nickel, although there are some contents depending on the battery. There is a growing need for product recycling.
  • waste lithium ion batteries Conventional recycling technology for waste lithium ion batteries includes firing, pulverizing waste lithium ion batteries and dissolving them using strong acids such as nitric acid, sulfuric acid, hydrochloric acid, etc. And then back-extracted into the aqueous phase with acid (exfoliation from the organic solvent phase), and then added with an aqueous alkaline solution or reacted with an aqueous carbonate solution to precipitate hydroxide or carbonate. It was collected as. As such a conventional technique, there is JP 2011-74410 A (Patent Document 1).
  • Patent Document 2 lithium cobaltate which is a battery positive electrode active material is reduced and roasted together with hydrogen or carbon, thereby changing the compound form of lithium cobaltate and leaching the roasted product with water.
  • Patent Document 3 JP 2011-94227 A
  • Patent Document 1 requires a large amount of acid for dissolution and alkali for neutralization, and has a problem that the operation cost is high because the process is complicated.
  • the product obtained by firing or pulverizing a waste battery may be mixed with iron, which is a battery container material, or aluminum, which is a positive electrode current collector material. . That is, in the solvent extraction method, since aluminum, iron, and the like are extracted with priority over lithium, there is a problem that even if lithium is to be recovered, they are extracted at the same time and high purity cannot be achieved. If iron or aluminum is extracted first in order to avoid such a problem, the number of steps until lithium is extracted increases, resulting in an increase in recovery cost.
  • the relatively high solubility of carbonates and hydroxides also causes the following problems. That is, even if it is attempted to recover lithium as a carbonate or hydroxide precipitate, an amount of lithium corresponding to the solubility is present in the aqueous phase, which is discarded. Therefore, there is a problem that the recovery rate is low in the method in which an alkaline aqueous solution or a carbonate aqueous solution is used.
  • Patent Documents 2 and 3 in the method of applying Patent Documents 2 and 3 to the recycling of the waste lithium ion battery, there is a problem that there is no step of removing when a current collector material or a case other than the positive electrode active material is mixed. .
  • the present invention provides a method for separating and recovering lithium, cobalt, etc. in a high yield, which can be operated at a low cost with a simple process using a minimum of acid and alkali. To do.
  • the present application includes a plurality of means for solving the above-described problems.
  • An example of the means is as follows.
  • the inventors performed firing, pulverization, and sieving on a waste lithium ion battery at a temperature of 500 ° C. or less and a reduced pressure of 10 Pa or less, and then leaching deionized water or lithium. It has been found that when an acid whose pH is adjusted so that the equilibrium pH of the solution is 8.6 or more is allowed to act, lithium is selectively leached and can be separated from copper, iron, cobalt and the like. This made it possible to recover lithium preferentially over other elements. Furthermore, when an acid was made to act on the said residue which leached lithium, it discovered that cobalt was selectively leached and can be isolate
  • the inventors conducted reverse extraction of lithium selectively extracted into the oil phase by solvent extraction into the aqueous phase, for example, using a solution containing a high concentration of lithium compound, and simultaneously crystallizing the lithium compound. It was found that the precipitation generation efficiency of the lithium compound can be remarkably improved by carrying out under the proceeding conditions, and a crystallization peeling apparatus was configured. As a result, the purity and recovery rate of the recovered lithium compound can be dramatically improved.
  • lithium, cobalt and the like can be separated and recovered from waste lithium ion batteries at a low cost using a minimum amount of chemicals.
  • deionized water (pure water) is allowed to act on the sieving product obtained by crushing and sieving, and lithium is selectively leached and recovered. A method will be described.
  • the leachate thus obtained is applied to the drum surface by spraying it into a heated carbon dioxide atmosphere or by spraying it onto a rotating drum at about 200 ° C. placed in a carbon dioxide atmosphere.
  • the obtained leachate was dried and peeled to obtain lithium carbonate powder. Further, carbon dioxide was passed through the leachate to obtain a lithium carbonate precipitate.
  • FIG. 3 is a plot of leaching rates of lithium, manganese, aluminum, and cobalt against pH.
  • the pH on the horizontal axis in the figure is the equilibrium pH after leaching.
  • the point where the equilibrium pH is about 11 is when deionized water having a pH of 7 is used, and the equilibrium pH is highest in this example.
  • the leaching rate of manganese and cobalt can be suppressed to 1% or less.
  • the transition of the lithium leaching rate with respect to the other elements described above is high as shown in FIG. 3 (a), and in the leachate having an equilibrium pH of 8.6 or more, the lithium content is the same as in Example 1.
  • the leach rate is about 89%.
  • EDTA ethylenediaminetetraacetic acid
  • the pH is The pH was adjusted with hydrochloric acid to be in the range of 3-7.
  • the mixed aqueous solution is a solution simulating the filtrate after treatment with deionized water described in Example 1.
  • the composition change of the crystallization stripping solution is as follows.
  • the crystallization stripping solution before being put into the stripping tank 501 contains the stripping aid containing the main component water, the lithium salt to be deposited, and the same ion as the counter ion of lithium in the lithium salt. .
  • the stripping tank 501 when the oil phase obtained by solvent extraction comes into contact with the crystallization stripping solution, lithium ions try to move from the oil phase to the crystallization stripping solution, but the square of the lithium ion activity of the aqueous phase. Since the product of the counter ion activity has already substantially reached the solubility product of the lithium salt to be precipitated, crystals of the lithium salt are precipitated.
  • FIG. 1 An example of a process flow for recovering a lithium salt and a cobalt salt from the lithium ion batteries disclosed in Examples 1 to 5 is collectively shown in FIG.
  • water extraction 10 is performed in the same manner as in Example 1 on the sieved product 5 obtained after subjecting the waste battery 1 to roasting / pulverization 2 including vacuum roasting, pulverization, and sieving.
  • a residue (including Co) 111 and a solution (mainly leaching Li) 211 are obtained.
  • the solvent extraction 220 in the same manner as in Example 4, the oil phase 221 mainly containing lithium and the water phase 222 containing aluminum and iron are separated.
  • the oil phase 231 is separated into a precipitate (Li salt is precipitated) 232 and an aqueous phase 233.
  • the oil phase 231 is used again for the solvent extraction 220 as an extraction solvent, and the aqueous phase 233 is used for the crystallization peeling 230 as a crystallization peeling liquid after adding the counter ion.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)
  • Removal Of Specific Substances (AREA)
  • Secondary Cells (AREA)
PCT/JP2013/074327 2012-09-11 2013-09-10 Procédé de recyclage de batteries au lithium-ion et dispositif associé Ceased WO2014042136A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2012199564A JP5898021B2 (ja) 2012-09-11 2012-09-11 リチウムイオン電池の再資源化方法、およびその装置
JP2012-199564 2012-09-11

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WO2014042136A1 true WO2014042136A1 (fr) 2014-03-20

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CN105244560A (zh) * 2014-06-16 2016-01-13 上海奇谋能源技术开发有限公司 一种锂离子电池的资源化回收方法
CN105355959A (zh) * 2015-11-12 2016-02-24 惠州金源精密自动化设备有限公司 铜环卸料与回收系统
WO2017091562A1 (fr) * 2015-11-24 2017-06-01 Worcester Polytechnic Institute Procédé et appareil permettant de recycler des batteries au lithium-ion
CN106941199A (zh) * 2017-04-18 2017-07-11 中航锂电（洛阳）有限公司 一种锂离子电池回收利用前的安全处理方法及装置，锂离子电池的安全回收方法
WO2018076994A1 (fr) * 2016-10-31 2018-05-03 湖南金源新材料股份有限公司 Procédé de récupération du lithium contenu dans de l'eau d'aval d'extraction à faible teneur en celui-ci, et procédé de recyclage d'eau d'aval d'extraction
WO2018181607A1 (fr) * 2017-03-31 2018-10-04 Ｊｘ金属株式会社 Procédé de récupération de lithium
CN108677014A (zh) * 2018-04-28 2018-10-19 长沙理工大学 一种废旧动力电池的回收方法
CN109088117A (zh) * 2018-08-03 2018-12-25 许成林 一种新能源汽车电池材料回收系统
CN109687052A (zh) * 2019-02-18 2019-04-26 广东山摩新材料科技有限公司 锂电池正极材料烧结用废旧匣钵自动回收正极材料设备
CN110144460A (zh) * 2019-04-28 2019-08-20 北京点域科技有限公司 一种锂离子电池正极废料中金属的浸出及回收工艺
CN110468280A (zh) * 2019-09-12 2019-11-19 金川集团股份有限公司 一种离子交换法回收废旧钴酸锂电池中有价金属的方法
US10522884B2 (en) 2012-04-04 2019-12-31 Worcester Polytechnic Institute Method and apparatus for recycling lithium-ion batteries
JP2020045576A (ja) * 2017-03-31 2020-03-26 Ｊｘ金属株式会社 リチウム回収方法
EP3604570A4 (fr) * 2017-03-30 2020-12-09 JX Nippon Mining & Metals Corporation Procédé de récupération de lithium
CN112646974A (zh) * 2020-11-12 2021-04-13 四川顺应动力电池材料有限公司 一种从废旧三元锂电池正极材料中回收有价金属的方法
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CA3178825A1 (fr) 2020-06-09 2021-12-16 David Henry SNYDACKER Extraction de lithium en presence de scalants
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CA3199218A1 (fr) 2020-11-20 2022-05-27 David Henry SNYDACKER Production de lithium avec de l'acide volatil
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KR20240014047A (ko) 2021-04-23 2024-01-31 리락 솔루션즈, 인크. 리튬 추출을 위한 이온 교환 장치
CN113003589B (zh) * 2021-04-25 2023-04-25 湖南金源新材料股份有限公司 从p507萃余液中提取制备电池级碳酸锂的方法及萃取装置
WO2023192192A1 (fr) 2022-03-28 2023-10-05 Lilac Solutions, Inc. Extraction de lithium améliorée par une phase alternative
EP4504988A2 (fr) 2022-04-01 2025-02-12 Lilac Solutions, Inc. Extraction de lithium avec des additifs chimiques
CN115415283B (zh) * 2022-07-21 2023-05-09 广东邦普循环科技有限公司 一种废旧电池的高效预处理回收设备
HUP2300329A1 (hu) 2022-07-21 2024-07-28 Guangdong Brunp Recycling Tech Co Berendezés hulladék akkumulátor hatékony elõkezelésére és újrahasznosítására

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