CN111987381A - Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries - Google Patents
Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries 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
- 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
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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
- 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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Abstract
The invention provides a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps: pretreating a waste lithium ion battery to obtain electrode powder, uniformly mixing the electrode powder with concentrated sulfuric acid, carrying out acidizing roasting, controlling the temperature of the acidizing roasting to be 220-750 ℃, and the time to be 1.0-24.0 h, adding a leaching agent into the roasted material for leaching after the roasting is finished, and filtering after the leaching is finished to obtain the valuable metal leaching solution with low fluorine content. According to the method, the removal of fluorine in the electrode powder and the leaching of valuable metals are organically combined, the fluorine in the electrode powder is removed through acidification and roasting, the valuable metals in the electrode powder are further leached by adopting an acid leaching method, and finally the valuable metal leaching solution is low in fluorine content, short in process flow, simple to operate, low in process cost and easy to realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of waste lithium ion battery resource recovery, and particularly relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries.
Background
Lithium ion batteries have been widely used in the field of portable consumer electronics such as mobile phones, notebook computers, digital cameras, and the like. Particularly, in recent years, under the double promotion of energy and environmental crisis, new energy automobiles are rapidly developed, and the demand of large-scale lithium ion batteries is brought. According to the statistics of authoritative data, the demand of the power lithium ion battery reaches 125Gwh only by 2020 in China. The service life of the power lithium ion battery is generally 3-5 years, so the number of scrapped lithium ion batteries is also sharply increased year by year, and the scrapped amount of the waste lithium ion batteries in China is estimated to reach 50 ten thousand tons in 2020 and 116 ten thousand tons in 2023 years. If the waste batteries are discarded at will, not only can the environment be seriously polluted, but also a great deal of resource waste is caused. The method has the advantages that the waste lithium ion batteries are subjected to harmless treatment, and resources in the waste lithium ion batteries are recycled, so that the method is not only relevant to environmental safety and resource guarantee safety, but also has important significance for sustainable development of new energy automobile industry.
The anode materials of the ion lithium battery widely applied to the market mainly comprise lithium cobaltate, lithium nickelate, lithium manganate, lithium iron phosphate, nickel cobalt aluminum ternary anode materials, nickel cobalt manganese ternary anode materials and the like. The ternary positive electrode material integrates the advantages of the positive electrode materials such as lithium cobaltate, lithium nickelate, lithium manganate and the like, has the characteristics of high energy density, long cycle life, good safety, relatively low cost and the like, becomes one of the novel positive electrode materials of the lithium ion battery with the development prospect at present, and the foreign lithium ion battery for the vehicle clearly uses the ternary lithium ion battery and is also closed to the ternary material at home.
The ternary lithium ion battery mainly comprises a positive electrode, a negative electrode, electrolyte, a diaphragm, a shell, a plastic fastener and the like, wherein the positive electrode active material contains various valuable metals such as cobalt, nickel, manganese, lithium and the like, and has high recovery value. At present, the recovery of waste lithium ion batteries mainly comprises three major types of dry recovery technology, wet recovery technology and biological recovery technology, wherein the wet recovery technology is mainly used in China, and the recovery method comprises the steps of pretreating the waste lithium ion batteries through the steps of discharging, disassembling, crushing, sorting, roasting and the like, then transferring valuable metals into a solution by selecting a proper chemical reagent, and then separating and recovering the valuable elements by means of chemical precipitation, solvent extraction, ion exchange and the like.
Chinese patent application CN101599563A discloses a method for recovering a positive active material of a waste lithium ion battery, which comprises the following processing steps: adding the crushed battery cell into hot water, stirring, filtering, drying, and screening to separate out most of active materials; dissolving the aluminum foil on the screen part by alkaline leaching, filtering and drying, and then carrying out secondary vibration screening to separate out residual powder materials; separating the plastic diaphragm on the screen, washing the copper sheet by dilute sulfuric acid and sodium thiosulfate solution to loosen and drop the carbon powder and active substances adhered on the copper sheet, separating the residual electrode powder by spinning after washing, combining the obtained electrode powder, soaking the electrode powder by NaOH solution after magnetic separation, and filtering, drying and calcining the active powder after alkaline soaking to obtain the active powder for subsequent treatment. In the method, during the processes of crushing and washing the battery cell and alkali dissolution of the aluminum foil, electrolyte lithium hexafluorophosphate is heated or is in contact with acid, alkali, water and the like to generate decomposition and hydrolysis reaction to generate hydrogen fluoride, the hydrogen fluoride can further react to form metal fluoride and remains in electrode powder, and in the process of calcining the electrode powder, a binder PVDF can also decompose to generate fluorine-containing compounds and remain in the electrode powder. The residue of fluorine has the following adverse effects: firstly, fluorine enters the leaching solution to increase the wastewater treatment cost; secondly, the precursor prepared by fluorine-containing nickel, cobalt and manganese has corrosion effect on equipment in the roasting process.
Chinese patent application CN207602724U discloses a system for continuously recycling waste ternary lithium ion batteries, which mainly comprises the steps of crushing waste lithium ion batteries or monomers by a crusher, feeding the crushed positive and negative electrode powders into a positive and negative electrode powder bin through a pulse dust collector, separating the metal and the positive and negative electrode powders by introducing the crushed material into a separator, leaching the obtained positive and negative electrode mixed powder by sulfuric acid, and recycling valuable metals such as nickel, cobalt, manganese, lithium and the like by operations such as impurity removal, coprecipitation and the like. According to the method, lithium hexafluorophosphate is largely decomposed due to heating or moisture contact in the crushing process, metal fluoride is finally formed and left in the electrode powder, the metal fluoride enters the leaching solution after acid leaching, and lithium fluoride precipitate is formed in the subsequent impurity removal process, so that a large amount of lithium is lost.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries comprises the following steps: pretreating a waste lithium ion battery to obtain electrode powder, uniformly mixing the electrode powder with concentrated sulfuric acid (firstly, adding a small amount of water to wet the surface of the electrode powder, so that the electrode powder and the concentrated sulfuric acid can be uniformly mixed), carrying out acidification roasting, controlling the temperature of the acidification roasting to be 220-750 ℃, and the time to be 1.0-24.0 h, wherein in the acidification roasting process, fluoride in the electrode powder can react with acid to generate fluoride, removing the fluoride through volatilization, adding a leaching agent into a roasting material for leaching after the roasting is finished, and then filtering to obtain the valuable metal leaching solution with low fluorine content. The parameters of the acidification roasting need to be controlled within the scope of the invention, if the parameters exceed the scope of the invention, the residual aluminum in the electrode powder can be melted and form insoluble aluminum oxide to wrap part of the electrode powder, so that valuable metals are difficult to leach; if the amount is less than the range of the present invention, the effect of removing fluorine is poor.
In the method, the pretreatment comprises discharging, disassembling, crushing and sorting, in order to thoroughly remove organic matters and avoid the influence of the organic matters remained in the electrode powder on the leaching of valuable metals, the temperature of the acidification roasting is controlled to be 400-750 ℃.
In the above method, preferably, the pretreatment includes discharging, dismantling, crushing, sorting, and removing organic substances; the organic matter removal means that a cracking method, an oxidation roasting method or an organic solvent dissolving method is adopted to remove organic matters contained in the sorted materials. In order to promote the sulfuric acid to fully react with the electrode powder and improve the fluorine removal efficiency, the temperature of the acidification roasting is controlled to be 220-400 ℃.
In the above method, preferably, the mass ratio of the concentrated sulfuric acid to the electrode powder is (0.5-1.0): 1, the mass concentration of the concentrated sulfuric acid is more than 75%.
In the method, preferably, the leaching temperature is 50-100 ℃ and the leaching time is 1.0-5.0 h. Leaching parameters need to be controlled within the scope of the invention, and if the leaching parameters exceed the scope of the invention, not only energy consumption is increased, but also the decomposition speed or the oxidation speed of the reducing agent is increased due to the temperature rise, so that metal can not be leached completely, or the dosage of the reducing agent is increased; if the temperature is lower than the range of the invention, the activation temperature required for the acid dissolution and reduction of the nickel-cobalt-manganese metal oxide can not be reached, and the reaction can not be completely carried out.
In the above method, preferably, the leaching agent is a mixture of concentrated sulfuric acid, water and a reducing agent, and in order to avoid introducing impurity ions, the reducing agent is at least one of hydrogen peroxide, sodium sulfite, sodium thiosulfate, ferrous sulfate, sulfur dioxide and ascorbic acid.
In the method, preferably, in order to reduce the amount of neutralizing agent and extracting agent used in the subsequent valuable metal separation process and improve the leaching rate of valuable metals, the mass ratio of concentrated sulfuric acid to electrode powder in the leaching agent is (0.5-5): 1, the liquid-solid ratio of water in the leaching agent to the electrode powder is (5-10): 1, the unit of the ratio is L/kg; in order to improve the leaching rate of valuable metals, the mass ratio of the reducing agent to the electrode powder in the leaching agent is (0.06-0.15): 1.
in the method, the fluorine content in the valuable metal leaching solution is preferably less than 0.3 g/L.
Compared with the prior art, the invention has the advantages that:
according to the method, the removal of fluorine in the electrode powder and the leaching of valuable metals are organically combined, the fluorine in the electrode powder is removed through acidification and roasting, the valuable metals in the electrode powder are further leached by adopting an acid leaching method, and finally the valuable metal leaching solution is low in fluorine content, short in process flow, simple to operate, low in process cost and easy to realize large-scale production.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps:
the waste ternary lithium ion battery is discharged, crushed and sorted to obtain electrode powder, and the main element content of the electrode powder is Ni 16.26%, Co 6.40%, Mn 11.81%, Li 3.89% and F2.73%. Weighing 100.0g of electrode powder, adding 54.2ml of 80.0% sulfuric acid, stirring uniformly, placing in a muffle furnace, carrying out acidification roasting for 2.0 hours at 550 ℃ to obtain 97.4g of roasted material, wherein the F content in the roasted material is 0.21%, adding 28.0ml of 98.0% sulfuric acid, 500.0ml of water and 65.0ml of hydrogen peroxide into the roasted material, heating to 70 ℃, carrying out stirring leaching for 3.0 hours, and filtering after leaching to obtain 550ml of valuable metal leaching solution with low fluorine content. The valuable metal leaching solution with low fluorine content mainly comprises 29.51g/L, Co 11.58.58 g/L, Mn 21.40.40 g/L, Li 6.36.36 g/L, F0.24.24 g/L of Ni, and the removal rate of F is 95.16%.
Comparative example 1:
a method for leaching valuable metals from waste lithium ion batteries comprises the following steps:
weighing 100.0g of the electrode powder sorted in the embodiment 1, roasting the electrode powder at 550 ℃ for 2.0h without adding sulfuric acid, supplementing 60.0ml of 98.0% sulfuric acid, 500.0ml of water and 40.0ml of hydrogen peroxide after roasting, then heating to 70 ℃, stirring and leaching for 3.0h, filtering after leaching to obtain 555ml of valuable metal leaching solution, wherein the main components are Ni 29.48g/L, Co 11.60.60 g/L, Mn 21.39.39 g/L, Li 6.40.40 g/L, F4.86g/L, and the removal rate of F is only 2.09%.
Example 2:
the invention relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps:
the method comprises the following steps of discharging, crushing, sorting and removing organic matters from a waste ternary 18650 lithium ion battery to obtain electrode powder, wherein the specific process of removing the organic matters comprises the following steps: placing the sorted materials in a tubular furnace, introducing air, heating to 600 ℃, roasting for 3.0h, absorbing roasting tail gas by using alkali liquor, and obtaining electrode powder after roasting is finished; the main element content of the electrode powder is 23.65 percent of Ni, 8.80 percent of Co, 12.77 percent of Mn, 4.78 percent of Li and 5.23 percent of F. Weighing 100.0g of electrode powder of the roasted material, adding 35.0ml of 98% sulfuric acid, mixing uniformly, then placing the electrode powder into a muffle furnace, heating to 300 ℃, carrying out acidizing roasting for 2.0 hours to obtain 145.2g of the roasted material, wherein the F content in the roasted material is 0.18%, adding 50ml of 98% sulfuric acid, 700ml of water and 80ml of hydrogen peroxide into the roasted material, heating to 60 ℃, stirring and leaching for 2.0 hours, and filtering after leaching is finished to obtain 750ml of valuable metal leaching solution with low fluorine content. The valuable metal leaching solution with low fluorine content mainly comprises Ni 31.49g/L, Co 11.70.70 g/L, Mn 17.00.00 g/L, Li 6.32.32 g/L and F0.32g/L, and the removal rate of F is 95.69%.
Comparative example 2:
a method for leaching valuable metals from waste lithium ion batteries comprises the following steps:
weighing 100.0g of electrode powder roasted in the tube furnace in example 2, adding 70.0ml of 98.0% sulfuric acid, 700.0ml of water and 40.0ml of hydrogen peroxide, heating to 70 ℃, stirring and leaching for 3.0h, filtering after leaching to obtain 750ml of valuable metal leaching solution, wherein the main components are Ni 31.52g/L, Co 11.65.65 g/L, Mn16.96g/L, Li 6.37.37 g/L and F6.83g/L, and the removal rate of F is only 2.06%.
Claims (10)
1. A method for synchronously defluorinating valuable metals leached from waste lithium ion batteries is characterized by comprising the following steps: pretreating a waste lithium ion battery to obtain electrode powder, uniformly mixing the electrode powder with concentrated sulfuric acid, carrying out acidizing roasting, controlling the temperature of the acidizing roasting to be 220-750 ℃, and the time to be 1.0-24.0 h, adding a leaching agent into the roasted material for leaching after the roasting is finished, and filtering after the leaching is finished to obtain the valuable metal leaching solution with low fluorine content.
2. The method according to claim 1, wherein the pretreatment comprises discharging, disassembling, crushing and sorting, and the temperature of the acidizing roasting is 400-750 ℃.
3. The method according to claim 1, wherein the pretreatment comprises discharging, dismantling, crushing, sorting and organic matter removal, and the temperature of the acidizing roasting is 220-400 ℃.
4. The method according to claim 3, wherein the removing of the organic substances is removing of organic substances contained in the sorted materials by a cracking method, an oxidizing roasting method or an organic solvent dissolving method.
5. The method according to claim 1, 2, 3 or 4, wherein the mass ratio of the concentrated sulfuric acid to the electrode powder is (0.5-1.0): 1, the mass concentration of the concentrated sulfuric acid is more than 75%.
6. A method according to claim 1, 2, 3 or 4, characterized in that the leaching temperature is 50-100 ℃ and the time is 1.0-5.0 h.
7. A method according to claim 1, 2, 3 or 4, characterized in that the leaching agent is a mixture of concentrated sulphuric acid, water and a reducing agent.
8. The method of claim 7, wherein the reducing agent is at least one of hydrogen peroxide, sodium sulfite, sodium thiosulfate, ferrous sulfate, sulfur dioxide, and ascorbic acid.
9. The method according to claim 8, wherein the mass ratio of concentrated sulfuric acid to electrode powder in the leaching agent is (0.5-5): 1, the liquid-solid ratio of water in the leaching agent to the electrode powder is (5-10): 1, the unit of the ratio is L/kg; the mass ratio of the reducing agent to the electrode powder in the leaching agent is (0.06-0.15): 1.
10. the method of claim 1, 2, 3 or 4, wherein the value metal leach solution has a fluorine content of less than 0.3 g/L.
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Cited By (5)
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| CN113415813A (en) * | 2021-06-22 | 2021-09-21 | 四川长虹格润环保科技股份有限公司 | Method for recovering lithium nickel cobalt manganese from waste ternary battery material |
| CN113481368A (en) * | 2021-05-26 | 2021-10-08 | 广东佳纳能源科技有限公司 | Method for leaching valuable metals from waste lithium cobaltate battery powder |
| CN113897488A (en) * | 2021-09-01 | 2022-01-07 | 格林美股份有限公司 | Method for recovering valuable metals from waste lithium ion batteries |
| CN115304059A (en) * | 2022-07-06 | 2022-11-08 | 中南大学 | Recycling treatment method for retired battery carbon slag |
| WO2024014521A1 (en) * | 2022-07-14 | 2024-01-18 | Jx Metals Corporation | Method for removing aluminum and method for recovering metals |
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| CN115304059A (en) * | 2022-07-06 | 2022-11-08 | 中南大学 | Recycling treatment method for retired battery carbon slag |
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| WO2024014521A1 (en) * | 2022-07-14 | 2024-01-18 | Jx Metals Corporation | Method for removing aluminum and method for recovering metals |
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