WO2012072619A1 - Procédé pour la récupération de lithium et de fer à partir de batteries lfp - Google Patents

Procédé pour la récupération de lithium et de fer à partir de batteries lfp Download PDF

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Publication number
WO2012072619A1
WO2012072619A1 PCT/EP2011/071249 EP2011071249W WO2012072619A1 WO 2012072619 A1 WO2012072619 A1 WO 2012072619A1 EP 2011071249 W EP2011071249 W EP 2011071249W WO 2012072619 A1 WO2012072619 A1 WO 2012072619A1
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WO
WIPO (PCT)
Prior art keywords
lithium
iron
batteries
recovery
lifep0
Prior art date
Application number
PCT/EP2011/071249
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English (en)
Inventor
Maarten Schurmans
Ben Thijs
Original Assignee
Umicore
Priority date (The priority date 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 date listed.)
Filing date
Publication date
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Publication of WO2012072619A1 publication Critical patent/WO2012072619A1/fr

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Classifications

    • 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
    • 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
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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

Definitions

  • a lithium iron phosphate (LiFeP0 4 ) battery also called LFP battery, is a type of rechargeable battery, specifically a lithium ion battery, which uses LiFeP0 4 as cathode material.
  • LiFeP0 4 when compared to the typical current consumer products based on LiCo0 2 is the higher current or peak-power rating.
  • Such LFP batteries are therefore particularly suitable for use in electrical vehicles or in hybrid electrical vehicles. Consequently, considerable quantities of such batteries are expected on the scrap market, being production refuses or end-of-live batteries. The need for recycling of the valuable metals in these batteries will arise with the expected popularity of electrical vehicles.
  • the recovery of the metals in this kind of materials can be performed according to either pyrometallurgical or hydrometallurgical routes.
  • hydrometallurgical processes may be advantageous.
  • lithium and iron are recovered from this fine LiFeP0 4 -bearing fraction in a process comprising the steps of: contacting this fraction with an acidic solution in presence of an oxidizing agent, thereby precipitating iron phosphate and solubilizing lithium; separating the iron phosphate from the lithium-bearing solution by solid/liquid separation; and, separating the lithium from the solution by its precipitation as a salt.
  • the acidic solution can be based on sulfuric acid, whereby the contacting step is performed at a pH lower than 3. It is useful to add the oxidizing agent so as to maintain a redox potential of at least 200 mV vs. Ag/AgCl, and preferably of at least 300 mV, so as to maximally suppress the leaching of iron.
  • the reactor is a pressure reactor, allowing for a process temperature of more than 100 °C.
  • lithium can be precipitated as a salt, in particular as a carbonate.
  • lithium and iron are recovered from LFP batteries in a process comprising the steps of: shredding the LFP batteries; separating the shreds into fractions by physical methods, thereby obtaining a LiFeP0 4 -bearing phase as a fine fraction; and, said LiFeP0 4 -bearing phase being further processed according to any one of the above- described processes.
  • the separation of fine and coarse fractions can be made by conventional means such as by dry or wet sieving. A cutoff at about 25 ⁇ is appropriate, although the optimal value depends upon the particle size distribution of the LiFeP0 4 powder used in the batteries.
  • the selective leaching of lithium can be represented by the reaction:
  • the batteries may be partially or fully discharged before shredding, to lower the risk of fire.
  • the lithium is then mainly present in the cathode material, which is LiFeP0 4 .
  • partially or fully charged batteries have a significant part of the lithium under metallic form, in the anode, e.g. as LiC 6 .
  • Anode material typically also is collected in the fine fraction after shredding. The contained lithium readily reacts and dissolves in the acidic medium used to leach the LiFeP0 4 .
  • the acidity of the solution in reaction (1) has to be chosen so as to avoid the formation of L13PO4, a species that precipitates at pH values above 3. This determines the minimum pH to ensure Li vs. Fe selectivity.
  • the need for the oxidation of Fe to Fe imposes a minimal oxidation power to the reaction medium. This is most adequately achieved using oxygen, with a partial pressure of at least 1 hPa. This can be realized e.g. by bubbling pure oxygen at atmospheric pressure through the reaction mixture, or by using a pressure reactor with an oxygen-bearing atmosphere.
  • the use of a pressure vessel has the advantage of faster kinetics as reaction temperatures of more than 100 °C will typically be used.
  • pressure leaching allows for a higher p0 2 , ensuring a more selective leaching of lithium.
  • Li-rich liquor can be further processed for the precipitation of Li, e.g. as a carbonate by addition of Na 2 CC>3, leading to the formation of Li 2 CC>3, an insoluble species that can be separated by filtration.
  • the FeP0 4 can be reused in agriculture or gardening, or even as a precursor for the manufacture of cathode material for new lithium battery. Examples
  • Either an open reactor or a pressure reactor is used.
  • a solids load of about 100 g/1 is chosen, although higher loads of e.g. 400 g/1 could easily be achieved.
  • the reaction conditions are maintained for about 2 h.
  • oxygen Examples 1, 3, 6, 8 and 10
  • air Comparative Example 7
  • This ensures a pC of 1 hPa in the solution with pure oxygen, and of only 0.21 hPa with air.
  • the redox potential vs. Ag/AgCl amounts to 300 to 550 mV using pure oxygen, and to only 120 mV using air.
  • the oxidation is performed with H2O2. This is continuously added so as to maintain a redox potential of about 500 mV vs. Ag/AgCl.
  • the pH is kept sufficiently acidic by continuous addition of H 2 SO 4 9N. Alternatively, it is allowed to start the reaction with an excess of acid, this excess being determined by the expected consumption and by the desire to arrive at a pH below 3 when the reaction terminates.
  • Example 6 When using a pressurized reactor, thus working under pressure (Examples 2, 4 and 5), oxygen is added to the gas phase of the reactor at a constant inlet pressure being the sum of the pH 2 0 (about 2 hPa at 120 °C and 0.5 hPa at 80 °C) and the desired p0 2 of at least 1 hPa. Obviously, the oxygen could also in this case be injected directly into the solution, as this would tend to further increase the oxidizing potential.
  • Example 6 is comparative, showing a marginally low lithium yield because the leaching solution has a marginally low acidity. A pH of less than 3 (such as 2.5 or 2) is therefore recommended.
  • Example 7 is also comparative, showing an undesirably high iron leaching yield, and thus an unsatisfactory selectivity with respect to lithium. This is due to the lack of oxidizing power of air at atmospheric pressure.
  • oxygen as oxidizing agent
  • a partial pressure of 1 hPa or more is recommended.
  • H 2 SO 4 as leaching acid
  • satisfactory results are obtained when the pH is less than 3
  • oxygen as an oxidizing agent
  • satisfactory results are obtained when its partial pressure is 1 hPa or more. This is illustrated in Table 1.
  • the selective leaching process is further illustrated on a 75:25 mixture of LiFeP0 4 and graphite, which is the typical composition of the fine fraction after shredding LFP batteries.
  • Graphite is quantitatively recovered in the iron phosphate residue. Any lithium in the anode material (as LiC 6 ) is extracted with excellent yields. This is illustrated in Table 2.
  • LFP batteries contain titanium-based anodes, such as Li 4 Ti50i 2 instead of graphite.
  • Li is selectively leached with respect to both Fe and Ti.
  • Titanium is quantitatively recovered in the iron phosphate, presumably as Ti0 2 .
  • Any lithium in the anode material (as L1 4 T1 5 O ) is extracted with excellent yields. This is illustrated in Table

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Secondary Cells (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

On s'attend à ce que les batteries au phosphate de lithium et de fer (LFP) deviennent très répandues dans les véhicules électriques. La nécessité de récupérer les métaux contenus, et le lithium en particulier, des batteries LFP en fin de vie deviendra par conséquent pressante dans le futur. L'invention porte sur un procédé permettant la lixiviation sélective et la récupération de lithium à partir de phosphate de lithium et de fer. Il comprend les étapes consistant à : mettre en contact la phase avec une solution acide en présence d'un agent oxydant, ce qui fait précipiter de cette manière le phosphate de fer et solubilise le lithium ; séparer le phosphate de fer de la solution renfermant du lithium par séparation solide/liquide ; et séparer le lithium de la solution par précipitation sous forme d'un sel. Ce procédé est particulièrement écologique en présentant une consommation minimale d'acide puisque seul le lithium est lixivié.
PCT/EP2011/071249 2010-11-29 2011-11-29 Procédé pour la récupération de lithium et de fer à partir de batteries lfp WO2012072619A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP10192947.9 2010-11-29
EP10192947 2010-11-29
US34499910P 2010-12-06 2010-12-06
US61/344,999 2010-12-06

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WO2012072619A1 true WO2012072619A1 (fr) 2012-06-07

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Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013035048A1 (fr) * 2011-09-07 2013-03-14 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de recyclage de batteries au lithium et/ou d'electrodes de telles batteries
DE102013016671A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium, Nickel, Kobalt aus der Lithium-Übergangsmetalloxid haltigen Fraktion gebrauchter galvanischer Zellen
DE102013016672A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium aus der Lithium-Manganoxid haltigen Fraktion gebrauchter galvanischer Zellen
DE102013016670A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium aus der Lithium-Eisen-Phosphat haltigen Fraktion gebrauchter galvanischer Zellen
CN105024106A (zh) * 2015-07-31 2015-11-04 合肥国轩高科动力能源股份公司 一种从废旧锂离子电池及报废正极片中回收磷酸铁的方法
CN106191445A (zh) * 2016-06-30 2016-12-07 南昌航空大学 一种锂离子电池浸出液中锂离子的分离方法
CN106910959A (zh) * 2017-05-04 2017-06-30 北京科技大学 一种从磷酸铁锂废料中选择性回收锂的方法
CN106986545A (zh) * 2017-02-27 2017-07-28 万柯楠 一种无熔融工艺制备烧结微晶玻璃的方法
CN107069132A (zh) * 2016-12-19 2017-08-18 天齐锂业股份有限公司 一种回收废旧磷酸铁锂正极材料的方法
CN108899601A (zh) * 2018-06-11 2018-11-27 衢州华友钴新材料有限公司 一种从磷酸铁锂中回收锂的方法
CN109075407A (zh) * 2016-05-20 2018-12-21 魁北克电力公司 再循环锂电池电极材料的方法
RU2676806C1 (ru) * 2017-10-10 2019-01-11 Общество с ограниченной ответственностью "ТЕХНОХИТ" Способ утилизации отработанных литиевых источников тока
CN110484726A (zh) * 2016-08-26 2019-11-22 湖南金源新材料股份有限公司 磷酸铁锂电池废料选择性浸取锂的方法
WO2020134773A1 (fr) * 2018-12-29 2020-07-02 宁德时代新能源科技股份有限公司 Méthode de récupération et de préparation de matériau de cathode de phosphate de fer-lithium
CN112142077A (zh) * 2020-09-08 2020-12-29 北京科技大学 磷酸铁锂正极废料回收制备电池级碳酸锂和磷酸铁的方法
CN112723330A (zh) * 2020-12-03 2021-04-30 广东邦普循环科技有限公司 一种异磷锰铁矿型磷酸铁的制备方法及其应用
CN113603119A (zh) * 2021-08-03 2021-11-05 广东邦普循环科技有限公司 一种从废旧磷酸铁锂材料回收锂的方法
CN113816353A (zh) * 2021-09-14 2021-12-21 中南大学 一种铁铝共沉淀去除废旧磷酸铁锂电池酸浸出液中铝的方法
WO2022134749A1 (fr) * 2020-12-25 2022-06-30 湖南邦普循环科技有限公司 Méthode de récupération de lithium dans des déchets de lithium fer phosphate et application associée
FR3125634A1 (fr) 2021-07-26 2023-01-27 Totalenergies Se Procédé vert de récupération de lithium et de fer de batteries au lithium
US20230038978A1 (en) * 2021-08-02 2023-02-09 Ascend Elements, Inc. Lithium Iron Phosphate (LFP) battery recycling
WO2023010971A1 (fr) * 2021-08-03 2023-02-09 广东邦普循环科技有限公司 Procédé de valorisation intégrale de batteries au phosphate de fer-lithium usagées
EP4210149A1 (fr) 2022-01-05 2023-07-12 Toyota Jidosha Kabushiki Kaisha Procédé de récupération de matériau actif d'électrode positive

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Cited By (46)

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US9312581B2 (en) 2011-09-07 2016-04-12 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for recycling lithium batteries and/or electrodes of such batteries
WO2013035048A1 (fr) * 2011-09-07 2013-03-14 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de recyclage de batteries au lithium et/ou d'electrodes de telles batteries
WO2014056608A2 (fr) * 2012-10-10 2014-04-17 Rockwood Lithium GmbH Procédé de récupération hydrométallurgique de lithium à partir de la fraction de cellules galvaniques usagées contenant du lithium, du fer et du phosphate
DE102013016671A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium, Nickel, Kobalt aus der Lithium-Übergangsmetalloxid haltigen Fraktion gebrauchter galvanischer Zellen
WO2014056610A1 (fr) 2012-10-10 2014-04-17 Rockwood Lithium GmbH Procédé de récupération hydrométallurgique de lithium à partir de la fraction de cellules galvaniques usagées contenant de l'oxyde manganeux de lithium
RU2648807C2 (ru) * 2012-10-10 2018-03-28 Роквуд Литиум Гмбх Способ гидрометаллургического извлечения лития, никеля, кобальта из фракции отработанных гальванических элементов, содержащей оксид лития и переходного металла
WO2014056608A3 (fr) * 2012-10-10 2015-01-08 Rockwood Lithium GmbH Procédé de récupération hydrométallurgique de lithium à partir de la fraction de cellules galvaniques usagées contenant du lithium, du fer et du phosphate
CN104903475A (zh) * 2012-10-10 2015-09-09 罗克伍德锂有限责任公司 从旧原电池的含有磷酸铁锂的级分中湿法冶金回收锂的方法
RU2639416C2 (ru) * 2012-10-10 2017-12-21 Роквуд Литиум Гмбх Способ гидрометаллургического обратного извлечения лития из фракции гальванических батарей, содержащей оксид лития и марганца
JP2016500753A (ja) * 2012-10-10 2016-01-14 ロックウッド リチウム ゲゼルシャフト ミット ベシュレンクテル ハフツングＲｏｃｋｗｏｏｄ Ｌｉｔｈｉｕｍ ＧｍｂＨ 使用済みガルバニ電池のリン酸鉄リチウム含有部分からの、湿式冶金法によるリチウムの回収方法
DE102013016672A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium aus der Lithium-Manganoxid haltigen Fraktion gebrauchter galvanischer Zellen
DE102013016670A1 (de) 2012-10-10 2014-04-10 Rockwood Lithium GmbH Verfahren zur hydrometallurgischen Rückgewinnung von Lithium aus der Lithium-Eisen-Phosphat haltigen Fraktion gebrauchter galvanischer Zellen
US9677153B2 (en) 2012-10-10 2017-06-13 Rockwood Lithium GmbH Method for the hydrometallurgical recovery of lithium from the fraction of used galvanic cells containing lithium, iron and phosphate
RU2638481C2 (ru) * 2012-10-10 2017-12-13 Роквуд Литиум Гмбх Способ гидрометаллургического обратного извлечения лития из фракции гальванических батарей, содержащей фосфат лития и железа
US9702024B2 (en) 2012-10-10 2017-07-11 Rockwood Lithium GmbH Method for the hydrometallurgical recovery of lithium, nickel and cobalt from the lithium transition metal oxide-containing fraction of used galvanic cells
US10711326B2 (en) 2012-10-10 2020-07-14 Albemarle Germany Gmbh Method for the hydrometallurgical recovery of lithium from the lithium manganese oxide-containing fraction of used galvanic cells
CN105024106A (zh) * 2015-07-31 2015-11-04 合肥国轩高科动力能源股份公司 一种从废旧锂离子电池及报废正极片中回收磷酸铁的方法
CN105024106B (zh) * 2015-07-31 2018-01-12 合肥国轩高科动力能源有限公司 一种从废旧锂离子电池及报废正极片中回收磷酸铁的方法
EP3459138B1 (fr) 2016-05-20 2023-11-01 Hydro-Québec Procédé pour le recyclage de matériaux d'électrode de batterie au lithium
EP4276208A3 (fr) * 2016-05-20 2023-12-27 Hydro-Québec Procédé pour le recyclage de matériaux d'électrode de batterie au lithium
CN109075407A (zh) * 2016-05-20 2018-12-21 魁北克电力公司 再循环锂电池电极材料的方法
EP3459138A4 (fr) * 2016-05-20 2020-05-06 Hydro-Québec Procédé pour le recyclage de matériaux d'électrode de batterie au lithium
CN106191445A (zh) * 2016-06-30 2016-12-07 南昌航空大学 一种锂离子电池浸出液中锂离子的分离方法
CN110484726A (zh) * 2016-08-26 2019-11-22 湖南金源新材料股份有限公司 磷酸铁锂电池废料选择性浸取锂的方法
CN107069132A (zh) * 2016-12-19 2017-08-18 天齐锂业股份有限公司 一种回收废旧磷酸铁锂正极材料的方法
CN106986545B (zh) * 2017-02-27 2020-03-06 万柯楠 一种无熔融工艺制备烧结微晶玻璃的方法
CN106986545A (zh) * 2017-02-27 2017-07-28 万柯楠 一种无熔融工艺制备烧结微晶玻璃的方法
CN106910959A (zh) * 2017-05-04 2017-06-30 北京科技大学 一种从磷酸铁锂废料中选择性回收锂的方法
RU2676806C1 (ru) * 2017-10-10 2019-01-11 Общество с ограниченной ответственностью "ТЕХНОХИТ" Способ утилизации отработанных литиевых источников тока
CN108899601A (zh) * 2018-06-11 2018-11-27 衢州华友钴新材料有限公司 一种从磷酸铁锂中回收锂的方法
WO2020134773A1 (fr) * 2018-12-29 2020-07-02 宁德时代新能源科技股份有限公司 Méthode de récupération et de préparation de matériau de cathode de phosphate de fer-lithium
CN112142077B (zh) * 2020-09-08 2021-10-29 北京科技大学 磷酸铁锂正极废料回收制备电池级碳酸锂和磷酸铁的方法
CN112142077A (zh) * 2020-09-08 2020-12-29 北京科技大学 磷酸铁锂正极废料回收制备电池级碳酸锂和磷酸铁的方法
CN112723330A (zh) * 2020-12-03 2021-04-30 广东邦普循环科技有限公司 一种异磷锰铁矿型磷酸铁的制备方法及其应用
WO2022134749A1 (fr) * 2020-12-25 2022-06-30 湖南邦普循环科技有限公司 Méthode de récupération de lithium dans des déchets de lithium fer phosphate et application associée
EP4230751A2 (fr) 2021-07-26 2023-08-23 Totalenergies Onetech Procédé écologique de récupération de lithium et de fer à partir de batteries au lithium
FR3125634A1 (fr) 2021-07-26 2023-01-27 Totalenergies Se Procédé vert de récupération de lithium et de fer de batteries au lithium
WO2023007242A2 (fr) 2021-07-26 2023-02-02 Totalenergies Onetech Procédé écologique de récupération de lithium et de fer à partir de batteries au lithium
US20230038978A1 (en) * 2021-08-02 2023-02-09 Ascend Elements, Inc. Lithium Iron Phosphate (LFP) battery recycling
US12071677B2 (en) * 2021-08-02 2024-08-27 Ascend Elements, Inc. Lithium iron phosphate (LFP) battery recycling
WO2023010971A1 (fr) * 2021-08-03 2023-02-09 广东邦普循环科技有限公司 Procédé de valorisation intégrale de batteries au phosphate de fer-lithium usagées
CN113603119B (zh) * 2021-08-03 2022-11-15 广东邦普循环科技有限公司 一种从废旧磷酸铁锂材料回收锂的方法
CN113603119A (zh) * 2021-08-03 2021-11-05 广东邦普循环科技有限公司 一种从废旧磷酸铁锂材料回收锂的方法
CN113816353A (zh) * 2021-09-14 2021-12-21 中南大学 一种铁铝共沉淀去除废旧磷酸铁锂电池酸浸出液中铝的方法
CN113816353B (zh) * 2021-09-14 2023-11-14 中南大学 一种铁铝共沉淀去除废旧磷酸铁锂电池酸浸出液中铝的方法
EP4210149A1 (fr) 2022-01-05 2023-07-12 Toyota Jidosha Kabushiki Kaisha Procédé de récupération de matériau actif d'électrode positive

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