CN113314710A - Method for recovering and regenerating anode material from waste lithium ion battery - Google Patents
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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- 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
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- 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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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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- Y02P10/00—Technologies related to metal processing
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention provides a method for recovering heavy metal elements in a lithium ion battery anode material and regenerating the anode material. Firstly, completely discharging, disassembling, calcining and alkali washing the waste lithium ion battery to obtain anode material powder; leaching valuable metal elements in the positive electrode material by using a leaching agent to obtain leaching solution rich in valuable metals; heating and evaporating ammonia in the leaching solution and adjusting the pH value of the solution to obtain a nickel cobalt manganese hydroxide precipitate precursor; and mixing and grinding the precursor and proper excessive lithium carbonate, and calcining by adopting a two-stage heating method to synthesize the ternary cathode material. The ammonia gas evaporated from the leachate can be absorbed by sulfuric acid to generate ammonium salt, so that the ammonia can be recycled. The method can realize the recycling of the ternary cathode material, has simple process, can effectively reduce the production cost, and can realize the recycling of ammonia.
Description
Technical Field
The invention relates to the technical field of valuable metal recovery of waste lithium ion batteries, in particular to a valuable metal recovery and positive electrode material regeneration method for a positive electrode material of a lithium ion battery.
Background
With the rapid development of new energy automobiles, people pay more and more attention to the problem of recycling a huge number of power lithium ion batteries after being scrapped. The waste lithium ion battery contains a large amount of heavy metals and organic compounds, and if the waste lithium ion battery is not treated, the waste lithium ion battery can cause serious damage to water, soil and air and harm the health and safety of human beings. The waste ternary lithium ion battery contains a large amount of valuable metals, 5-20% of cobalt, 5-10% of nickel, 5-7% of lithium, 5-10% of other metals, 15% of organic compounds and 7% of plastics, and has a remarkable economic value. The recycling of waste lithium ion batteries and the elimination of the harmful effects of the batteries are the necessary ways for the sustainable development of the application field of power lithium ion batteries.
At present, the mainstream recovery method for waste lithium ion batteries focuses on the recovery of valuable metal elements of a positive electrode material, and mainly comprises dry recovery, wet recovery and the like. The recovered metal material can be used as a battery material raw material and put into the production process of the battery material again. In the cycle of "scrap electrode material → raw material → electrode material", the metal exists in a different state, causing a large amount of energy waste during the migration process. Early lithium ion battery cathode materials were predominantly LiCoO2Since Co has a high recovery value and Li has an important significance in recovery, researchers have a strong interest in recovering metal elements. However, with the ternary material LiNixCoyMn1-x-yO2The advantages of the method are highlighted, the utilization range is expanded, and the recycling and the cyclic utilization of the materials are gradually paid attention. At present, most of researches on recycling lithium ion batteries are carried out by wet acid leaching. The method needs a large amount of acid and organic solvent, increases the production cost, and releases toxic and harmful gases in the recovery process. And the solid-liquid ratio adopted by the prior recovery technology is lower, so that the method is not suitable for large-scale production. Recovery may be combined with synthesis in view of the particular components of the recovered product. The waste anode material is used as the raw material to recover and regenerate the new anode material, so that the complexity of separation and purification in a recovery stage can be avoided, the closed-loop utilization of substances in the lithium battery industry can be realized, the production cost of the anode material is reduced, and the economic benefit is improved。
Based on the current situation of recycling lithium ion cathode materials in the prior art, improvement is needed, the recycling process is simplified, the production procedures of the materials are greatly reduced, the improvement of the recycling process of the lithium ion battery is realized, and economic benefits are realized.
Disclosure of Invention
In view of the technical problems, the invention provides a method for recycling valuable metals and positive electrode materials from waste lithium ion batteries, which has the advantages of simple preparation process, mild process conditions, short process time, no need of consuming a large amount of acid and alkali, low cost, effective realization of recycling of ternary positive electrode materials, environmental protection and no generation of a large amount of solid waste and wastewater.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) discharging, disassembling and calcining the waste lithium ion battery to obtain anode material powder;
(2) adding the anode material powder into the leaching solution, carrying out high-temperature leaching reaction in a hydrothermal reaction kettle, filtering to obtain leaching solution rich in valuable metals, and controlling the ratio of the anode material powder to the leaching solution to be 10-20 g/L;
(3) adjusting the content of transition metal elements in the leachate, then heating the leachate in a nitrogen atmosphere, evaporating ammonia in the solution, and adjusting the pH of the solution to 10.5-11.2 to obtain a precursor;
(4) and mixing the precursor with a lithium source, uniformly ball-milling, and calcining to complete the regeneration of the anode material.
In the above technical scheme, in the step (1), most of aluminum, carbon and binder can be removed from the waste ternary lithium ion battery through discharging, disassembling, screening and calcining, so as to obtain waste anode material powder.
Preferably, the waste lithium ion battery positive electrode material is one of a lithium cobaltate positive electrode material, a lithium nickelate positive electrode material and a nickel-cobalt-manganese positive electrode material.
Preferably, the calcination temperature in the step (1) is 400-500 ℃, and the calcination time is 1.5-5 h.
Preferably, the leaching solution in the step (2) is a mixed solution of ammonia water, ammonium nitrate and ammonium sulfite.
The total concentration of ammonia water and ammonium nitrate is 4-6 mol/L, the concentration of ammonium sulfite is 0.1-0.6 mol/L, and the pH value of the mixed solution is 7-12.
Preferably, the reaction temperature in the hydrothermal reaction kettle in the step (2) is 110-.
Preferably, the target ratio of the transition metal elements in the step (3) is as follows: ni: co: mn = 1: (0-1):(0.125-1).
Preferably, the heating evaporation temperature in the step (3) is 60-95 ℃, and the heating time is 10-20 h.
Preferably, 0.5-1.2 mol/L sodium hydroxide is selected to adjust the pH of the solution in the step (3).
Preferably, the molar ratio of the precursor to the lithium source in the step (4) is 1 (1.02-1.06).
Preferably, in the step (4), the temperature is raised to 430-480 ℃ at a speed of 2-6 ℃/min, the temperature is maintained for 4-6 h, and then the temperature is raised to 870 ℃ at a speed of 2-6 ℃/min, and the temperature is maintained for 10-15 h.
The technical scheme can effectively recover the waste ternary lithium ion positive electrode material, avoids the problems of resource waste and environmental pollution, has short, green and efficient recovery process, can regenerate ammonia water and ammonium sulfate added in the alkaline leaching process through subsequent processes, realizes the closed-loop utilization of resources and reduces the generation of waste liquid, and the process not only can efficiently recover valuable metals in the waste lithium ion battery positive electrode material, but also can regenerate a new lithium ion battery positive electrode material.
Detailed Description
The present invention is described in detail with reference to the following embodiments by providing a method for recovering and regenerating a positive electrode material from a waste lithium ion battery.
In the following examples, the used lithium ion battery is a Nickel Cobalt Manganese (NCM) ternary battery, and the positive electrode material is LiNi0.6Co0.2Mn0.2O2
Example 1
1) Discharging NCM lithium ion waste batteries in 2 mol/L potassium chloride solution; disassembling the battery and separating out a positive plate; calcining the obtained positive plate for 4 hours at 440 ℃, grinding and screening to obtain waste positive material LiNi0.6Co0.2Mn0.2O2。
2) Adding 2 g of positive electrode material powder into 100 mL of mixed solution of ammonia water, ammonium nitrate and ammonium sulfite, wherein the molar ratio of the ammonia water to the ammonium nitrate is 2: 1, the concentration of ammonium sulfite is 0.5 mol/L. And transferring the mixed solution into a 150 mL hydrothermal reaction kettle, reacting for 90min at the reaction temperature of 120 ℃ and the stirring speed of 300 rpm, and filtering to obtain the leaching solution.
3) Adding 0.5 mol/L nickel sulfate, 0.2 mol/L cobalt sulfate and 0.2 mol/L manganese sulfate into the leachate obtained in the step 2), so that the ratio of Ni, Co and Mn is 6:2: 2; then heating the leaching solution at 70 ℃ in a nitrogen atmosphere for 15 hours, adjusting the pH of the solution to 11.2 by using 0.5 mol/L sodium hydroxide, and controlling the flow rate of nitrogen at 0.2L/min to ensure that ammonia in the leaching solution is fully volatilized. And after the reaction is finished, filtering, washing and drying to obtain a precursor.
4) And (3) absorbing the ammonia evaporated in the step 3) by using dilute nitric acid to obtain an ammonium nitrate solution, and reusing the ammonium nitrate solution in the step 2) to leach valuable metals in the anode material, so that the ammonia can be recycled.
5) Mixing and grinding the precursor material obtained in the step 3) and lithium hydroxide uniformly, then calcining in a muffle furnace, heating from room temperature to 420 ℃ at a heating rate of 3 ℃/min, preserving heat for 4 h, continuing heating to 830 ℃ at 3 ℃/min, preserving heat for 12 h, and naturally cooling to obtain the anode material. The molar ratio of the precursor to the lithium hydroxide is 1: 1.05.
example 2
1) Discharging NCM lithium ion waste batteries in 2 mol/L potassium chloride solution; disassembling the battery and separating out a positive plate; calcining the obtained positive plate for 4 hours at the temperature of 450 ℃, grinding and screening to obtain waste positive material LiNi1/3Co1/3Mn1/ 3O2。
2) Adding 3 g of positive electrode material powder into 100 mL of mixed solution of ammonia water, ammonium nitrate and ammonium sulfite, wherein the molar ratio of the ammonia water to the ammonium nitrate is 3: 1, the concentration of ammonium sulfite is 0.3 mol/L. And transferring the mixed solution into a 150 mL hydrothermal reaction kettle, reacting for 80 min at the reaction temperature of 140 ℃ and the stirring speed of 300 rpm, and filtering to obtain the leachate.
3) Adding 0.5 mol/L nickel sulfate, 0.2 mol/L cobalt sulfate and 0.2 mol/L manganese sulfate into the leachate obtained in the step 2), so that the ratio of Ni, Co and Mn is 1:1: 1; then heating the leaching solution at 60 ℃ in a nitrogen atmosphere for 20 hours, adjusting the pH of the solution to 11.0 by using 0.6 mol/L sodium hydroxide, and controlling the flow rate of nitrogen at 0.5L/min to ensure that ammonia in the leaching solution is fully volatilized. And after the reaction is finished, filtering, washing and drying to obtain a precursor.
4) And (3) absorbing the ammonia evaporated in the step 3) by using dilute nitric acid to obtain an ammonium nitrate solution, and reusing the ammonium nitrate solution in the step 2) to leach valuable metals in the anode material, so that the ammonia can be recycled.
5) Mixing and grinding the precursor material obtained in the step 3) and lithium hydroxide uniformly, then calcining in a muffle furnace, heating from room temperature to 440 ℃ at the heating rate of 4 ℃/min, preserving heat for 4.5 h, continuing heating to 840 ℃ at 4 ℃/min, preserving heat for 12 h, and naturally cooling to obtain the cathode material. The molar ratio of the precursor to the lithium hydroxide is 1: 1.05.
example 3
1) Discharging NCM lithium ion waste batteries in 2 mol/L potassium chloride solution; disassembling the battery and separating out a positive plate; calcining the obtained positive plate at 400 ℃ for 5 h, grinding and screening to obtain waste positive material LiNi1/3Co1/3Mn1/ 3O2。
2) Adding 5 g of positive electrode material powder into 100 mL of mixed solution of ammonia water, ammonium nitrate and ammonium sulfite, wherein the molar ratio of the ammonia water to the ammonium nitrate is 2: and 3, the concentration of ammonium sulfite is 0.6 mol/L. And transferring the mixed solution into a 150 mL hydrothermal reaction kettle, reacting for 30 min at the reaction temperature of 180 ℃ and the stirring speed of 300 rpm, and filtering to obtain the leaching solution.
3) Adding 2 mol/L nickel sulfate, 2 mol/L cobalt sulfate and 2 mol/L manganese sulfate into the leachate obtained in the step 2), wherein the ratio of Ni, Co and Mn is 1:1: 1; then heating the leaching solution at 80 ℃ in a nitrogen atmosphere for 12 hours, adjusting the pH of the solution to 10.5 by using 0.5 mol/L sodium hydroxide, and controlling the flow rate of nitrogen at 0.4L/min to ensure that ammonia in the leaching solution is fully volatilized. And after the reaction is finished, filtering, washing and drying to obtain a precursor.
4) And (3) absorbing the ammonia evaporated in the step 3) by using dilute nitric acid to obtain an ammonium nitrate solution, and reusing the ammonium nitrate solution in the step 2) to leach valuable metals in the anode material, so that the ammonia can be recycled.
5) Mixing and grinding the precursor material obtained in the step 3) and lithium hydroxide uniformly, then calcining in a muffle furnace, heating from room temperature to 400 ℃ at the heating rate of 2 ℃/min, preserving heat for 5 h, continuing heating to 850 ℃ at 2 ℃/min, preserving heat for 10 h, and naturally cooling to obtain the anode material. The molar ratio of the precursor to the lithium hydroxide is 1: 1.05.
example 4
1) Discharging NCM lithium ion waste batteries in 5 mol/L potassium chloride solution; disassembling the battery and separating out a positive plate; calcining the obtained positive plate at 500 ℃ for 2 h, grinding and screening to obtain waste positive material LiNi1/3Co1/3Mn1/ 3O2。
2) Adding 1 g of positive electrode material powder into 100 mL of mixed solution of ammonia water, ammonium nitrate and ammonium sulfite, wherein the molar ratio of the ammonia water to the ammonium nitrate is 1:1, the concentration of ammonium sulfite is 0.4 mol/L. And transferring the mixed solution into a 150 mL hydrothermal reaction kettle, reacting for 90min at the reaction temperature of 120 ℃ and the stirring speed of 300 rpm, and filtering to obtain the leaching solution.
3) Adding 2 mol/L nickel sulfate, 2 mol/L cobalt sulfate and 2 mol/L manganese sulfate into the leachate obtained in the step 2), so that the ratio of Ni, Co and Mn is 1:1: 1; then heating the leaching solution at 90 ℃ in a nitrogen atmosphere for 10 hours, adjusting the pH of the solution to 10.8 by using 0.5 mol/L sodium hydroxide, and controlling the flow rate of nitrogen at 0.2L/min to ensure that ammonia in the leaching solution is fully volatilized. And after the reaction is finished, filtering, washing and drying to obtain a precursor.
4) And (3) absorbing the ammonia evaporated in the step 3) by using dilute nitric acid to obtain an ammonium nitrate solution, and reusing the ammonium nitrate solution in the step 2) to leach valuable metals in the anode material, so that the ammonia can be recycled.
5) Mixing and grinding the precursor material obtained in the step 3) and lithium hydroxide uniformly, then calcining in a muffle furnace, heating from room temperature to 460 ℃ at the heating rate of 5 ℃/min, preserving heat for 4 h, continuing heating to 870 ℃ at 5 ℃/min, preserving heat for 10 h, and naturally cooling to obtain the anode material. The molar ratio of the precursor to the lithium hydroxide is 1: 1.05.
Claims (5)
1. a process for recycling valuable metal elements and positive electrode materials from waste lithium ion batteries is characterized by comprising the following steps:
1) discharging, disassembling and calcining the waste lithium ion battery to obtain anode material powder;
2) adding the anode material powder into the leaching solution, carrying out high-temperature leaching reaction in a hydrothermal reaction kettle, filtering to obtain leaching solution rich in valuable metals, and controlling the ratio of the anode material powder to the leaching solution to be 10-20 g/L;
3) adjusting the content of transition metal elements in the leachate, then heating the leachate in a nitrogen atmosphere, evaporating ammonia in the solution, and adjusting the pH of the solution to 10.5-11.2 to obtain a precursor;
4) and mixing the precursor with a lithium source, uniformly ball-milling, and calcining to complete the regeneration of the anode material.
2. The process for recycling valuable metal elements and positive electrode materials from waste lithium ion batteries as claimed in claim 1, wherein the leaching reaction temperature in step 2) is 110-.
3. The process for recycling valuable metal elements from waste lithium ion batteries and regenerating positive electrode materials according to claim 1, wherein the temperature required for evaporating ammonia in the leachate in the step 3) is 60-95 ℃, and the evaporation time is 10-20 h.
4. The process for recovering valuable metallic elements from waste lithium ion batteries and regenerating positive electrode materials according to claim 1, wherein the evaporation of ammonia from the leachate in step 3) is carried out under a nitrogen atmosphere, and the pH of the leachate is adjusted by 0.5 to 1.2 mol/L sodium hydroxide solution.
5. The process for recycling valuable metal elements and regenerating positive electrode materials from waste lithium ion batteries according to claim 1, wherein the calcination in the step 4) specifically comprises: calcining at 480 ℃ for 4-6 h and then at 870 ℃ for 760 ℃ for 10-15 h.
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Cited By (7)
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CN113862476A (en) * | 2021-09-16 | 2021-12-31 | 格林美股份有限公司 | Method for pre-extracting lithium from waste lithium ion battery |
CN113904016A (en) * | 2021-10-11 | 2022-01-07 | 格林美股份有限公司 | Method for reconstructing single crystal electrode material from waste lithium ion battery |
CN114497792A (en) * | 2022-01-25 | 2022-05-13 | 宁波大学 | Efficient electrode material recovery and re-preparation method and application |
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CN114956199A (en) * | 2022-03-08 | 2022-08-30 | 西安交通大学 | Recycling and regenerating method for anode of waste nickel-cobalt-manganese ternary lithium ion battery |
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CN114497792A (en) * | 2022-01-25 | 2022-05-13 | 宁波大学 | Efficient electrode material recovery and re-preparation method and application |
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CN115449636A (en) * | 2022-09-05 | 2022-12-09 | 中南大学 | Recovery and regeneration process and equipment for lithium ion battery anode material |
CN115449636B (en) * | 2022-09-05 | 2023-11-21 | 中南大学 | Recycling and regenerating process of lithium ion battery anode material |
CN115724474A (en) * | 2022-11-16 | 2023-03-03 | 清华大学深圳国际研究生院 | Repairing method of failed layered positive electrode material, positive electrode material and application of positive electrode material |
CN115724474B (en) * | 2022-11-16 | 2023-12-08 | 清华大学深圳国际研究生院 | Repairing method of failed layered positive electrode material, positive electrode material and application of positive electrode material |
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