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WO2022252602A1 - Procédé de lixiviation en toute sécurité d'une batterie usagée et son application - Google Patents

Procédé de lixiviation en toute sécurité d'une batterie usagée et son application Download PDF

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Publication number
WO2022252602A1
WO2022252602A1 PCT/CN2021/142932 CN2021142932W WO2022252602A1 WO 2022252602 A1 WO2022252602 A1 WO 2022252602A1 CN 2021142932 W CN2021142932 W CN 2021142932W WO 2022252602 A1 WO2022252602 A1 WO 2022252602A1
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WIPO (PCT)
Prior art keywords
leaching
filter residue
waste
agent
roasting
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/CN2021/142932
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English (en)
Chinese (zh)
Inventor
余海军
钟应声
谢英豪
李长东
张学梅
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.)
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Brunp Vehicles Recycling Co Ltd
Original Assignee
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Brunp Vehicles Recycling Co Ltd
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Publication date
Application filed by Hunan Brunp Recycling Technology Co Ltd, Guangdong Brunp Recycling Technology Co Ltd, Hunan Brunp Vehicles Recycling Co Ltd filed Critical Hunan Brunp Recycling Technology Co Ltd
Publication of WO2022252602A1 publication Critical patent/WO2022252602A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • 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
    • C22B47/00—Obtaining manganese
    • 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
    • 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
    • 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 invention belongs to the technical field of recycling waste batteries, and in particular relates to a method and application for safe leaching of waste batteries.
  • Waste lithium-ion batteries are composed of positive electrodes, negative electrodes, electrolytes, and separators.
  • the negative electrode is composed of graphite, binder, conductive agent and current collector
  • the positive electrode is made of active material powder, binder and conductive agent coated on the current collector.
  • Metals with potential recycling value include Ni, Mn, Co, Li, Al, etc.
  • the current recycling of waste lithium-ion batteries mainly includes a series of operations such as coarse crushing, physical screening, and fine crushing of waste lithium-ion batteries to obtain the particulate matter of waste lithium battery powder, but the recycled waste lithium battery powder contains a low amount of aluminum.
  • Slag particle impurities whose particle size is similar to that of waste lithium-ion battery powder, are mixed with active material powder, binder and other particles, and can react with acid and alkali, so the treatment of aluminum slag impurity particles is difficult. Due to the generation of flammable and explosive hydrogen during the recovery process of aluminum and subsequent valuable metals, it is dangerous.
  • the current use of hydrometallurgical recycling to prepare positive electrode materials mostly faces the problem of excessive aluminum content.
  • the treatment methods mainly focus on the front-end treatment of the battery, using acid leaching, high-temperature heat treatment or alkali leaching, but these three methods have their own advantages.
  • the disadvantages of each are high cost of acid leaching and the generation of unsafe hydrogen, high-temperature treatment consumes a lot of energy and cannot remove aluminum, and the aluminum content in the positive electrode material prepared after alkaline leaching is still higher than the battery-grade standard. Therefore, it is necessary to improve the removal rate of aluminum slag particles in battery powder particles and improve the safety of metal leaching processes such as Ni, Co, and Li.
  • the present invention aims to solve at least one of the technical problems in the above-mentioned prior art. For this reason, the present invention proposes a method and application of safe leaching of waste batteries.
  • This method combines safe, efficient, and low-energy physical methods such as roasting, sorting, and flotation with chemical methods such as dilute alkali dissolution. to remove aluminum from waste lithium batteries.
  • the present invention adopts the following technical solutions:
  • a method for leaching waste batteries comprising the following steps:
  • the calcination temperature is 240°C-580°C
  • the calcination time is 1.5-5h
  • the calcination heating rate is 5-30°C/min.
  • step (1) the gas generated by the roasting is collected with lye.
  • the lye is at least one of sodium hydroxide, magnesium hydroxide, potassium hydroxide, barium hydroxide, zinc hydroxide or calcium hydroxide.
  • the concentration of the lye is 0.01-0.15 mol/L.
  • the solid-to-liquid ratio of the battery powder and water is 1:(1.5-4) g/ml.
  • the flotation agent is one of oxidized paraffin soap, sodium oleate or laurylamine.
  • the density of the flotation agent in the flotation is 1.80-2.65 g/cm 3 .
  • the lye is at least one of sodium hydroxide, magnesium hydroxide, potassium hydroxide or calcium hydroxide.
  • the concentration of the lye is 0.10-0.80 mol/L.
  • the solid-to-liquid ratio of the floating material and the lye is 5g/L-15g/L.
  • the density of aluminum slag is 2.70g/cm 3
  • the density of waste lithium battery powder is for example: the bulk density of lithium iron phosphate is 1.523g/cm 3
  • the tap density is 1.2g/cm 3
  • the tap density of nickel cobalt lithium manganate is 2.0- 2.4 g/cm 3 .
  • the density difference is used for flotation, and the density of aluminum slag is higher than that of waste lithium battery powder.
  • the leaching time is 10-120 min, and the leaching temperature is 30-90°C.
  • step (3) ventilate the gas that produces in the process of described leaching, utilize hydrogen detection instrument to monitor the concentration of hydrogen at exhaust port simultaneously; Ventilation keeps hydrogen concentration lower than 0.5% VOL (air volume ratio) or 5000ppm.
  • VOL air volume ratio
  • the solid-to-liquid ratio during leaching is 2-30 g/L.
  • the leaching time is 1-6 hours, and the leaching temperature is 40-95°C.
  • the leaching agent is an organic acid.
  • the concentration of the organic acid is 0.5-5 mol/L.
  • the organic acid is tartaric acid.
  • the reducing agent is hydrogen peroxide.
  • step (4) the washed washing solution e is mixed with the filtrate d of step (3) to obtain a mixed solution, which can be used as lye in step (3) for recycling.
  • the present invention also provides the application of the above-mentioned waste battery leaching method in recycling valuable metals.
  • the leaching solution obtained by the above method of leaching waste batteries is an acid solution containing Li + , Co 2+ , Mn 2+ , and Ni 2+ , and Li, Co, Mn, and Ni can be recovered further.
  • the present invention combines safe, efficient, and low-energy physical methods such as roasting, screening, and flotation with chemical methods such as dilute alkali dissolution to remove aluminum in waste lithium batteries from the source.
  • the present invention uses roasting and screening to separate aluminum foil and battery powder first, and then uses flotation agent to sink the aluminum slag, copper and other impurities in the battery powder to the bottom, further removes aluminum, avoids a large amount of hydrogen gas generated in the subsequent leaching process, and improves the leaching process. Therefore, the residual aluminum slag can be removed, which is also to avoid the generation of hydrogen gas during the leaching of the positive active material powder and improve the safety of leaching.
  • the positive electrode material produced by leaching with leaching solution meets the battery-grade standard, and there will be no safety problems during storage, which is especially suitable for industrial production.
  • the present invention is roasting the waste lithium battery powder
  • the bonding performance of the binder polyvinylidene fluoride, polytetrafluoroethylene
  • the waste lithium battery powder becomes brittle.
  • the fluid falls off, and the binder and conductive agent graphite gradually decompose and burn at high temperature.
  • the roasting process changes the molecular structure of the positive electrode material, reduces the charge of transition metal ions in the positive electrode material, and creates conditions for subsequent leaching and recovery.
  • the waste lithium battery powder is mainly black, the aluminum foil is bright silver, and the copper foil is light yellow. It is very convenient to sort and remove most of the aluminum foil and copper foil by using a color sorter.
  • the present invention adopts a low solid-liquid ratio for both leaching, which can reduce the amount of acid-base consumption, further efficiently leaching aluminum and positive electrode active material powder, and at the same time mixing the filtrate b and washing liquid d to obtain a mixed solution that can be recycled, reducing Alkali dosage.
  • the leaching of the present invention adopts organic acid tartaric acid, while ensuring the leaching rate of valuable metal elements, its leaching reaction is relatively mild, avoiding the production of sulfur dioxide, Adverse effects of gases such as hydrochloric acid on the environment and equipment.
  • the boiling point of tartaric acid is about 399°C.
  • hydrochloric acid it is less volatile at the leaching reaction temperature of 30-95°C. Therefore, tartaric acid is used for leaching, and the whole leaching process is more environmentally friendly and safer.
  • Fig. 1 is a flowchart of a method for safely leaching waste batteries according to Embodiment 1 of the present invention.
  • the recovered lithium iron phosphate battery is disassembled and discharged, and after being coarsely crushed by machinery, the broken waste lithium battery is placed in a sintering kiln for roasting.
  • the roasting temperature is controlled at 350°C, and the roasting is stable for 4.8 hours.
  • the heating rate is controlled At about 15°C/min, the gas generated by roasting is collected with 0.01mol/L sodium hydroxide lye, and the waste lithium batteries after roasting are vibrated and screened, and the aluminum foil and copper foil are sorted by the color sorter, and then sorted
  • the finished waste lithium battery powder is ground by a ball mill;
  • step (3) On the basis of step (3), the filter residue a is washed 4 times with pure water, the washing liquid d is collected by filtration, and the filter residue c is separated, and the filter residue c is 1.5% hydrogen peroxide with 0.5mol/L tartaric acid and a volume ratio
  • the solid-to-liquid ratio during leaching is 5g/L
  • the temperature of the leaching reaction system is controlled at 42°C
  • Residue f, filtrate b, and washing liquid d are mixed in a volume ratio of 1:1, and the mixed solution is used for leaching in step (3).
  • Fig. 1 is the flow chart of the method for safe leaching of waste batteries according to Example 1 of the present invention. It can be seen from Fig. 1 that in the leaching of waste batteries, aluminum is mainly removed through four steps of sieving, sorting, flotation and adding lye.
  • the recovered lithium iron phosphate battery is disassembled and discharged, and after being roughly crushed mechanically, the broken waste lithium battery is placed in a sintering kiln for roasting.
  • the roasting temperature is controlled at 580°C, and the roasting is stable for 2.4 hours. During the period, the heating rate is controlled.
  • the gas generated by roasting is collected with 0.04mol/L sodium hydroxide lye, and the waste lithium batteries after roasting are vibrated and screened.
  • the color sorter sorts aluminum foil and copper foil, and then the sorting is completed.
  • the waste lithium battery powder is ground by a ball mill;
  • step (3) On the basis of step (3), the filter residue a is washed with pure water for 2 times, the washing liquid d is collected by filtration, and the filter residue c is separated, and the filter residue c is 3.4% hydrogen peroxide with 2.5mol/L tartaric acid and a volume ratio Carry out leaching, the solid-to-liquid ratio during leaching is 5g/L, the temperature of the leaching reaction system is controlled at 58°C, and after leaching is completed, filter to obtain an acid solution containing Li + , Co 2+ , Mn 2+ , Ni 2+ , residue f, and filtrate b. Washing solution d is mixed according to the volume ratio of 1:1.4, and the mixed solution is used for leaching in step (3).
  • the recovered lithium iron phosphate battery is disassembled and discharged, and after being coarsely crushed by machinery, the broken waste lithium battery is placed in a sintering kiln for roasting.
  • the roasting temperature is controlled at 420°C, and the roasting is stable for 3.5 hours. During the period, the heating rate is controlled.
  • the gas generated by roasting is collected with 0.09mol/L sodium hydroxide lye, and the waste lithium batteries after roasting are vibrated and screened, and the color sorter sorts aluminum foil and copper foil, and then the sorting is completed
  • the waste lithium battery powder is ground by a ball mill;
  • step (3) On the basis of step (3), the filter residue a is washed 3 times with pure water, the washing liquid d is collected by filtration, and the filter residue c is separated, and the filter residue c is 5.5% hydrogen peroxide with tartaric acid of 3.8mol/L and a volume ratio Carry out leaching, the solid-to-liquid ratio during leaching is 12g/L, the temperature of the leaching reaction system is controlled at 61°C, and after leaching is completed, the acid solution containing Li + , Co 2+ , Mn 2+ , Ni 2+ , residue f, filtrate b. Washing solution d is mixed according to the volume ratio of 1:1.8, and the mixed solution is used for leaching in step (3).
  • step (3) On the basis of step (3), the filter residue a is washed 3 times with pure water, the washing liquid d is collected by filtration, and the filter residue c is separated, and the filter residue c is 8.0% hydrogen peroxide with tartaric acid of 4.78mol/L and a volume ratio of 8.0%.
  • the solid-to-liquid ratio during leaching is 15g/L
  • the temperature of the leaching reaction system is controlled at 94°C
  • filter to obtain an acid solution containing Li + , Co 2+ , Mn 2+ , Ni 2+ , residue f, filtrate b.
  • Washing solution d is mixed according to the volume ratio of 1:2.3, and the mixed solution is used for leaching in step (3).
  • a method for leaching waste batteries comprising the following specific steps:
  • Example 1 The difference from Example 1 is that no flotation is carried out in step (2).
  • a method for leaching waste batteries comprising the following specific steps:
  • Example 1 The difference from Example 1 is that no sodium hydroxide is added in step (3) for leaching.
  • Example 1 adopt sulfuric acid leaching leaching in the step (4), other reaction conditions are all the same. Including: 1.3mol/L sulfuric acid and 1.5% hydrogen peroxide for leaching, the solid-liquid ratio during leaching is 5g/L, and the temperature of the leaching reaction system is controlled at 60°C.
  • step (2) As known from Table 1, compared with the quality of aluminum in the waste lithium battery powder in step (1) of Examples 1, 2, 3, and 4, the quality of aluminum in the filter residue c in step (3) decreased by 0.53%, 0.16%, and 0.60%, 0.26%; Comparative Example 1 and Comparative Example 1, step (2) has reduced the 0.23% hydrogen concentration through flotation; Comparative Example 1 and Comparative Example 2, utilize alkali leaching aluminum in the step (3), reduce The mass of aluminum in filter residue c was 0.11%; comparative example 3 was leached by sulfuric acid, and the reaction was violent, while the leaching reactions in examples 1, 2, 3, 4 and ratios 1 and 2 were mild. Therefore, it can be concluded that steps (2) and (3) can effectively reduce the aluminum content in the waste lithium battery powder, reduce the generation of hydrogen, and improve the safety during leaching.
  • the leaching of organic acid tartaric acid Compared with the leaching of inorganic acids such as sulfuric acid, the leaching of organic acid tartaric acid has a relatively mild leaching reaction while ensuring the leaching rate of valuable metal elements, and avoids the adverse effects of the generated gas on the environment and equipment.

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  • Manufacturing & Machinery (AREA)
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Abstract

La présente invention concerne le domaine technique de la récupération de batteries usagées. La divulgation concerne un procédé de lixiviation en toute sécurité d'une batterie usagée et son application. Le procédé comprend les étapes suivantes consistant à : décharger, griller, et tamiser une batterie au lithium usagée pour obtenir une feuille d'aluminium de cuivre et une poudre de batterie ; ajouter la poudre de batterie à de l'eau, puis ajouter un agent de flottaison pour effectuer une flottaison afin d'obtenir un matériau flottant et un sédiment ; utiliser une lessive pour lixivier le matériau flottant et filtrer pour obtenir un filtrat b et un résidu de filtre a ; et laver le résidu de filtre a, filtrer pour obtenir un résidu de filtre c, et ajouter un agent de lixiviation et un agent réducteur pour lixiviation afin d'obtenir un liquide de lixiviation. Dans la présente invention, des procédés physiques sûrs, efficaces, et à faible consommation d'énergie tels que le grillage, le tamisage et la flottaison sont combinés à des procédés chimiques tels que la dissolution à l'alcali dilué, et l'aluminium dans la batterie au lithium usagée peut être retiré de la source.
PCT/CN2021/142932 2021-05-31 2021-12-30 Procédé de lixiviation en toute sécurité d'une batterie usagée et son application Ceased WO2022252602A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202110601341.4A CN113502396A (zh) 2021-05-31 2021-05-31 一种废旧电池安全浸出的方法和应用
CN202110601341.4 2021-05-31

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CN116281918A (zh) * 2023-03-09 2023-06-23 中国科学院广州能源研究所 一种退役磷酸铁锂黑粉全组分精细分离回收的方法
CN117263189A (zh) * 2023-09-20 2023-12-22 四川长虹格润环保科技股份有限公司 一种利用光伏切方湿硅粉制备硅碳复合材料的方法
WO2024130843A1 (fr) * 2022-12-22 2024-06-27 广东邦普循环科技有限公司 Poudre noire de batterie sans carbone à faible teneur en cuivre-aluminium et procédé de préparation s'y rapportant
CN118811809A (zh) * 2024-08-13 2024-10-22 湖北景焕新能源科技有限公司 一种锂离子电池石墨负极再生方法及再生石墨
CN119702634A (zh) * 2024-12-20 2025-03-28 中南大学 一种废旧锂离子电池极片色选分离的方法
WO2025091238A1 (fr) * 2023-10-31 2025-05-08 广东邦普循环科技有限公司 Procédé de traitement basé sur drt pour des batteries usagées

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CN113502396A (zh) * 2021-05-31 2021-10-15 广东邦普循环科技有限公司 一种废旧电池安全浸出的方法和应用
CN115367732B (zh) * 2022-09-20 2023-08-22 中南大学 一种工业硫酸盐固废和废弃镍钴锰锂系电池协同资源化回收方法

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