WO2022062675A1 - Méthode de récupération de matériau d'électrode positive de batterie au lithium usagée - Google Patents

Méthode de récupération de matériau d'électrode positive de batterie au lithium usagée Download PDF

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Publication number
WO2022062675A1
WO2022062675A1 PCT/CN2021/110323 CN2021110323W WO2022062675A1 WO 2022062675 A1 WO2022062675 A1 WO 2022062675A1 CN 2021110323 W CN2021110323 W CN 2021110323W WO 2022062675 A1 WO2022062675 A1 WO 2022062675A1
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positive electrode
waste
lithium
powder
battery positive
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PCT/CN2021/110323
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English (en)
Chinese (zh)
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陈鑫根
唐红辉
黎亮
刘勇奇
曹磊军
李长东
Original Assignee
广东邦普循环科技有限公司
湖南邦普循环科技有限公司
湖南邦普汽车循环有限公司
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Publication of WO2022062675A1 publication Critical patent/WO2022062675A1/fr

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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
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • 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
    • 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 field of lithium ion battery recycling, and in particular relates to a recycling method for a positive electrode material of a waste lithium battery.
  • Lithium battery recycling has achieved rapid development in China in recent years.
  • Waste ternary lithium batteries are prepared after monomer disassembly (also called crushing, pretreatment), leaching, copper removal, iron and aluminum removal, extraction and co-precipitation.
  • the ternary precursor and lithium salt, and the by-product is Yuanming powder, which has achieved good economic benefits and formed a large scale.
  • the solution after copper removal contains ferrous ions.
  • ferrous ions are not easy to precipitate, it is necessary to oxidize ferrous ions into iron ions and then adjust the pH to precipitate iron ions.
  • sodium chlorate is commonly used to oxidize ferrous ion, which has the characteristics of high efficiency and fast speed, but chloride ion is introduced, so that the yuanming powder obtained by evaporation and crystallization of the lithium salt section contains chloride ions.
  • the value of yuanming powder is determined by Hundreds of yuan per ton has become tens of yuan per ton or even difficult to sell.
  • the valuable metals in the waste ternary electrode powder battery are nickel, cobalt, manganese and lithium, which themselves are a kind of raw material without copper in the waste ternary battery, and lithium cobalt oxide is also a raw material for the recycling of waste ternary battery.
  • the price of one metal ton of pyrolusite is 54 yuan. It can be considered that manganese is a low-value metal, and the price of lithium is currently at a low position.
  • the price of battery-grade lithium carbonate is more than 40,000 a ton. Because pole piece powder, lithium manganate and lithium cobaltate are all the raw materials of the battery recycling line, the raw materials come from a wide range of sources.
  • waste lithium cobalt oxide and waste pole piece powder are used as recycled raw materials.
  • waste lithium manganate cathode materials there is currently a patent number CN101538655A "A method of recycling from waste lithium manganate battery cathode materials", which uses sulfuric acid to leach lithium manganate, lithium leach into leaching solution, manganese in lithium manganate A disproportionation reaction occurs, and part of it becomes tetravalent and precipitates into manganese dioxide, and part of it becomes divalent manganese and leaches into the leaching solution.
  • the use of manganese dioxide can indeed achieve the method mentioned in the patent, but the waste lithium manganate cathode material contains impurities such as carbon black and alumina, which obviously cannot be used as super capacitors Material.
  • the main components in the leaching solution are lithium sulfate and manganese sulfate. It is necessary to add more expensive liquid alkali to precipitate the manganese ions, which shows that the recovery cost of the leaching solution is relatively high. As a result, its economic benefits are low, and the economic benefits of building a wet recycling production line alone are low, resulting in unmanned recycling and predicament of lithium manganate batteries.
  • the object of the present invention is to provide a method for recycling waste and old lithium battery positive electrode materials, which can recycle waste and old lithium manganate, waste and old lithium cobaltate and waste and old ternary positive electrode materials for parallel production, and can recover valuable metals at low cost. Lithium, high safety and the process of oxidizing ferrous ions does not introduce chloride ions.
  • the present invention adopts the following technical solutions:
  • a method for recycling a positive electrode material of a waste lithium battery comprising the following steps:
  • Oxidative acid leaching is performed on the positive electrode material of the waste lithium battery to obtain a leaching solution
  • the waste lithium battery is also pretreated to obtain battery positive electrode material powder.
  • the pretreatment includes discharging, disassembling, pulverizing, sorting, and sintering to obtain battery positive electrode material powder.
  • the temperature of the acid leaching is 60°C-90°C.
  • the solution used in the oxidative acid leaching is one of sulfuric acid and hydrogen peroxide.
  • the heating is to heat the solution after copper removal to 90°C-110°C.
  • the pH of the solution after copper removal is 1.0-3.5.
  • the content of ferrous ions in the solution after copper removal is greater than 0.5 g/L.
  • the waste battery positive electrode powder is at least one of waste ternary battery positive electrode flake powder, waste lithium manganate powder or waste lithium cobalt oxide powder.
  • the substance that does not participate in the reaction is graphite slag, and the waste ternary battery cathode powder can directly remove iron and aluminum without graphite slag.
  • the lithium content of the waste ternary battery cathode sheet powder is 3-5%, the nickel content is 12-17%, the cobalt content is 15-19%, and the manganese content is 13-19% .
  • Waste ternary battery cathode powder does not contain iron and copper.
  • the reaction time is 4-6 hours, and the reaction temperature is 90°C-110°C.
  • the pH adjustment to acidity is to adjust the pH to 3.5-4.5.
  • the solution used for adjusting pH to acidity is one of sodium hydroxide or sodium carbonate.
  • step (3) the iron-aluminum slag is returned to step (1) for acid leaching.
  • the lye is sodium carbonate.
  • step (3) reaction is as follows:
  • the present invention also provides the application of the above recovery method in recovering valuable metals from the positive electrode material of waste lithium batteries.
  • the method for recovering the positive electrode material of a waste lithium battery uses ferrous ions in the solution after copper removal as a reducing agent, and leaches lithium manganate, lithium cobaltate, and nickel, cobalt, and manganese in the positive electrode sheet powder of ternary batteries. element, the lithium in it is efficiently recovered, the parallel production of waste ternary cathode materials, waste lithium manganate and waste lithium cobaltate is achieved, and a safe, low-cost and chloride-free ferrous oxide is provided. ionic method.
  • Embodiment 1 is a process flow diagram of Embodiment 1 of the present invention.
  • FIG. 2 is a process flow diagram of Embodiment 2 of the present invention.
  • a method for recycling a positive electrode material of a waste lithium battery comprising the following steps:
  • Drying the iron-aluminum slag in step (3) can obtain a filter residue with a dry weight of about 1.36 tons, wherein the nickel content is 0.02%, the cobalt content is 0.03%, the manganese content is 0.04%, and the lithium content is 0.035%.
  • step (3) reaction is as follows:
  • Fig. 1 is the process flow chart of Example 1 (the black box represents the processing procedure, and the white box represents the obtained substance or the added substance, such as the leaching solution obtained by acid leaching of the battery).
  • a method for recycling a positive electrode material of a waste lithium battery comprising the following steps:
  • step (3) 0.34 kg of filter residue in step (3), wherein the manganese content is 6.8%, and the lithium content is 0.45%, it can be drawn that the ratio of nickel cobalt manganese entering the filtrate is more than 98%, and the ratio of lithium entering the filtrate is 97%, The economy is very good; the filter residue is returned to step (1), and sulfuric acid + hydrogen peroxide is used to carry out reducing acid leaching on the filter residue to obtain 0.22 kg of carbon black residue.
  • the manganese content in the carbon black residue is 0.14% and the lithium content is 0.003%. %, the total metal leaching rate is greater than 99%.
  • the reaction mechanism is as follows:
  • FIG. 2 is a process flow chart of Example 2 (the black box represents the processing procedure, and the white box represents the obtained substance or the added substance, such as battery powder obtained by pretreatment of the battery).
  • a method for recycling a positive electrode material of a waste lithium battery comprising the following steps:
  • Example 1 0.04 85.1 1.37 0
  • Example 2 0.04 85.2 1.36 0
  • Comparative Example 1 0.04 85.1 1.37 0
  • Table 3 Table of element content of iron-aluminum slag
  • the content of the main elements nickel and cobalt is basically the same, and the content of nickel, cobalt and manganese is 0.19% relative to the average manganese content of the filter residue added with sodium chlorate.
  • the slag is mainly graphite.

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

Abstract

La présente invention appartient au domaine de la récupération de batteries au lithium. L'invention concerne une méthode de récupération d'un matériau d'électrode positive de batterie au lithium usagée. La méthode comprend les étapes suivantes consistant à : (1) réaliser une lixiviation acide sur un matériau d'électrode positive de batterie au lithium usagée, de façon à obtenir un lixiviat ; (2) ajouter de la poudre de fer au lixiviat pour réduction, de façon à obtenir du cuivre spongieux et un liquide post-élimination de cuivre ; (3) chauffer le liquide post-élimination de cuivre, puis ajouter une poudre d'électrode positive de batterie usagée, les mélanger, réaliser une réaction, réguler le pH pour qu'il soit acide, et filtrer pour obtenir un résidu fer-aluminium et un filtrat ; et (4) réaliser une extraction sur le filtrat pour obtenir une solution de sulfate de nickel-cobalt-manganèse et un raffinat, effectuer une co-précipitation sur la solution de sulfate de nickel-cobalt-manganèse pour obtenir un précurseur ternaire, ajouter une liqueur alcaline au raffinat, et filtrer pour obtenir du carbonate de lithium. Dans la méthode de récupération d'un matériau d'électrode positive de batterie au lithium usagée selon la présente invention, des ions ferreux dans le liquide post-élimination de cuivre sont utilisés en tant qu'agent réducteur pour lixivier le manganate de lithium, l'oxyde de lithium cobalt, et les éléments métalliques nickel, cobalt et manganèse à partir d'une poudre de plaque d'électrode positive de batterie ternaire, de sorte que du lithium est efficacement récupéré à partir de celle-ci.
PCT/CN2021/110323 2020-09-24 2021-08-03 Méthode de récupération de matériau d'électrode positive de batterie au lithium usagée WO2022062675A1 (fr)

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CN114759285A (zh) * 2022-04-11 2022-07-15 中南大学 废旧锂离子电池浸出液的处理方法
CN114890441A (zh) * 2022-05-16 2022-08-12 昆明理工大学 从废旧钴酸锂电池正极片中回收氯化锂、氧化钴的方法
CN114899522A (zh) * 2022-07-11 2022-08-12 河北顺境环保科技有限公司 一种废旧三元软包锂电池的处理方法
CN114959272A (zh) * 2022-05-19 2022-08-30 江苏大学 从废旧锂离子电池中选择性回收锂的方法
CN115072688A (zh) * 2022-08-18 2022-09-20 矿冶科技集团有限公司 一种废旧磷酸铁锂电池全组分回收方法
CN115180661A (zh) * 2022-07-22 2022-10-14 余姚市鑫和电池材料有限公司 一种从铁铝废渣中回收镍钴铜混合硫酸盐的方法
CN115433825A (zh) * 2022-08-16 2022-12-06 湖南中邦再生资源科技有限公司 一种废旧锂电池中铁和硫的综合回收方法
CN115627356A (zh) * 2022-09-27 2023-01-20 暨南大学 一种废旧三元锂电池金属回收方法
CN115959829A (zh) * 2022-12-27 2023-04-14 重庆科技学院 退役锂电池回收过程中产生铁铝渣和废炭渣的回收方法
CN116706050A (zh) * 2023-08-07 2023-09-05 江门市科恒实业股份有限公司 中低镍单晶三元正极材料及其制备方法和电池
US11876196B2 (en) 2020-08-24 2024-01-16 Green Li-Ion Pte. Ltd. Process for removing impurities in the recycling of lithium-ion batteries
WO2024055071A1 (fr) * 2022-09-14 2024-03-21 Gelion Technologies Pty Ltd Procédé de recyclage pour la récupération d'éléments métalliques de valeur à partir de déchets de matériaux de batterie
CN114759285B (zh) * 2022-04-11 2024-06-04 中南大学 废旧锂离子电池浸出液的处理方法

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CN110983045A (zh) * 2019-11-26 2020-04-10 湖南邦普循环科技有限公司 一种镍钴锰溶液除铁铝的方法
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CN111270073A (zh) * 2020-02-03 2020-06-12 广东省稀有金属研究所 一种从废旧锂离子电池电极材料浸出液中回收有价金属的方法
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US11876196B2 (en) 2020-08-24 2024-01-16 Green Li-Ion Pte. Ltd. Process for removing impurities in the recycling of lithium-ion batteries
CN114759285A (zh) * 2022-04-11 2022-07-15 中南大学 废旧锂离子电池浸出液的处理方法
CN114759285B (zh) * 2022-04-11 2024-06-04 中南大学 废旧锂离子电池浸出液的处理方法
CN114890441A (zh) * 2022-05-16 2022-08-12 昆明理工大学 从废旧钴酸锂电池正极片中回收氯化锂、氧化钴的方法
CN114890441B (zh) * 2022-05-16 2023-05-23 昆明理工大学 从废旧钴酸锂电池正极片中回收氯化锂、氧化钴的方法
CN114959272A (zh) * 2022-05-19 2022-08-30 江苏大学 从废旧锂离子电池中选择性回收锂的方法
CN114899522A (zh) * 2022-07-11 2022-08-12 河北顺境环保科技有限公司 一种废旧三元软包锂电池的处理方法
CN114899522B (zh) * 2022-07-11 2022-09-30 河北顺境环保科技有限公司 一种废旧三元软包锂电池的处理方法
CN115180661A (zh) * 2022-07-22 2022-10-14 余姚市鑫和电池材料有限公司 一种从铁铝废渣中回收镍钴铜混合硫酸盐的方法
CN115180661B (zh) * 2022-07-22 2024-02-13 余姚市鑫和电池材料有限公司 一种从铁铝废渣中回收镍钴铜混合硫酸盐的方法
CN115433825B (zh) * 2022-08-16 2023-11-07 湖南中邦再生资源科技有限公司 一种废旧锂电池中铁和硫的综合回收方法
CN115433825A (zh) * 2022-08-16 2022-12-06 湖南中邦再生资源科技有限公司 一种废旧锂电池中铁和硫的综合回收方法
CN115072688A (zh) * 2022-08-18 2022-09-20 矿冶科技集团有限公司 一种废旧磷酸铁锂电池全组分回收方法
WO2024055071A1 (fr) * 2022-09-14 2024-03-21 Gelion Technologies Pty Ltd Procédé de recyclage pour la récupération d'éléments métalliques de valeur à partir de déchets de matériaux de batterie
CN115627356A (zh) * 2022-09-27 2023-01-20 暨南大学 一种废旧三元锂电池金属回收方法
CN115959829A (zh) * 2022-12-27 2023-04-14 重庆科技学院 退役锂电池回收过程中产生铁铝渣和废炭渣的回收方法
CN116706050B (zh) * 2023-08-07 2023-11-28 江门市科恒实业股份有限公司 中低镍单晶三元正极材料及其制备方法和电池
CN116706050A (zh) * 2023-08-07 2023-09-05 江门市科恒实业股份有限公司 中低镍单晶三元正极材料及其制备方法和电池

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