CN112813270A - Method for recycling anode material of waste nickel-cobalt-manganese ternary lithium battery - Google Patents
Method for recycling anode material of waste nickel-cobalt-manganese ternary lithium battery Download PDFInfo
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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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- 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
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- C22B47/00—Obtaining manganese
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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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- 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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- 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
Abstract
A method for recycling a waste nickel-cobalt-manganese ternary lithium battery positive electrode material belongs to the technical field of material recycling. The recovery method comprises the following steps: s1, leaching the anode material of the waste nickel-cobalt-manganese ternary lithium battery by using dilute acid, and then performing filter pressing to obtain a leachate A; s2, adding dilute acid and hydrogen peroxide into the leaching solution A for pretreatment to obtain a leaching solution B; s3, adjusting the pH value of the leaching solution B, precipitating and removing aluminum ions to obtain a leaching solution C; s4, adopting chelate resin to adsorb manganese and cobalt in the leaching solution C in sequence, and then obtaining adsorbed effluent; carrying out dilute acid desorption on the chelate resin, and recovering manganese and cobalt after alkali liquor precipitation; s5, neutralizing the adsorbed effluent by using alkali liquor, precipitating, and recovering nickel to obtain filtrate; and S6, reacting at a certain temperature, treating the filtrate by adopting a saturated crystallization method, and crystallizing to obtain the lithium carbonate for recovery. The method has the advantages of simple process, low cost and environmental friendliness, and can ensure high recovery rate and high purity.
Description
Technical Field
The invention relates to a technology in the field of material recovery, in particular to a method for recovering a waste nickel-cobalt-manganese ternary lithium battery positive electrode material.
Background
In recent years, with the deepening of the energy crisis of China, the enhancement of the environmental awareness of the people, the subsidy of government policies and other stimulation, the new energy automobile industry develops rapidly. Under the background that the technology of the hybrid electric vehicle is gradually mature and the cost of the power battery is gradually reduced, a plurality of large enterprises are bundled and piled up to enter the industry of new energy vehicles. The related data show that the recovery amount of the domestic automobile power battery in China will reach 25.7 ten thousand tons in 2020, and 42.2 ten thousand tons in 2022 is expected. With the rapid development of the new energy automobile industry, China has become the first new energy automobile producing and selling country in the world, the producing and selling quantity of the power storage battery is also increased year by year, and the recycling of the power storage battery is urgent. China is the biggest world in the production of ternary lithium batteries, the ternary lithium battery industry becomes one of high and new technology industries which are key supports of China, and with the expiration of the service life of the ternary lithium battery, the recovery of waste ternary lithium batteries also becomes a difficult problem which needs to be solved urgently for environmental protection, and meanwhile, the recovery of metals such as cobalt, nickel, lithium and the like in the ternary lithium battery also has higher economic value.
In the prior art, the whole recovery process is complex, the cost is high, the recovery rate is low, and the purity of the recovered product is low.
The Chinese patent application with the publication number of CN105591171A discloses a method for recovering a positive electrode material of a waste nickel-cobalt-manganese ternary lithium ion battery, which comprises the steps of adding alkali to the positive electrode material for dissolving, and separating to obtain a dissolved solution I and insoluble substances; carrying out acidolysis on insoluble substances to obtain a dissolved solution II, adjusting the pH value to be alkaline, forming a precipitate, and obtaining a filtrate I and a precipitate I; carrying out acidolysis on the precipitate I to obtain a dissolved solution III, adding ammonia water for complexing, adjusting the pH value to be alkaline, then adding soluble carbonate, and filtering to obtain a filtrate II and a precipitate II; adding soluble carbonate into the filtrate II, and heating to obtain a precipitate III; and after acidolysis, adjusting the pH value to 3.0-3.5, adding hypochlorite to adjust the pH value to 2.0-3.0, and filtering to obtain filtrate III and precipitate IV. The method does not need to use an extracting agent and an organic solvent, reduces pollution, but has more complex recovery operation.
Therefore, there is a need for a process that is simple, cost effective, environmentally friendly, and ensures high recovery and high purity.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for recovering a waste nickel-cobalt-manganese ternary lithium battery positive electrode material, which has the advantages of simple process, low cost and environmental friendliness, and can ensure high recovery rate and high purity.
The invention comprises the following steps:
s1, leaching the anode material of the waste nickel-cobalt-manganese ternary lithium battery by using dilute acid, and then performing filter pressing to obtain a leachate A;
s2, adding dilute acid and hydrogen peroxide into the leaching solution A for pretreatment to obtain a leaching solution B;
s3, adjusting the pH value of the leaching solution B, precipitating and removing aluminum ions to obtain a leaching solution C;
s4, adopting chelate resin to adsorb manganese and cobalt in the leaching solution C in sequence, and then obtaining adsorbed effluent; carrying out dilute acid desorption on the chelate resin, and recovering manganese and cobalt after alkali liquor precipitation;
s5, neutralizing the adsorbed effluent by using alkali liquor, precipitating, and recovering nickel to obtain filtrate;
and S6, reacting at a certain temperature, treating the filtrate by adopting a saturated crystallization method, and crystallizing to obtain the lithium carbonate for recovery.
In step S1, the positive electrode material is obtained by discharging, disassembling and stripping the waste nickel-cobalt-manganese ternary lithium battery, the leaching time of the positive electrode material is 10-60 min, the leaching adopts at least one of sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid and acetic acid, and the acid concentration is 1.0-10.0 wt%; the solid-to-liquid ratio of the anode material to the dilute acid is 20-100 g/g.
In step S2, sulfuric acid is preferably used as the dilute acid.
In the step S3, dilute acid is adopted to adjust the pH value of the leaching solution B, and precipitation is carried out at 55-95 ℃; the pH value after adjustment is 2.2-4.1; preferably, the dilute acid is sulfuric acid with the concentration of 1.0-5.0 wt%.
In step S4, the chelating resin for adsorbing manganese is HPMn-1, and contains phosphate groups, phosphite groups and sulfonic acid groups; the chelating resin for adsorbing cobalt is HP-C/N-1, and contains a hypophosphite group and an amino group; the dilute acid is preferably sulfuric acid, and the concentration of the dilute acid is 1.5-10.3 wt%.
In step S5, the alkali solution contains at least one of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, sodium oxalate, and potassium oxalate.
In step S6, the precipitant used in the saturated crystallization method is sodium carbonate and/or potassium carbonate, and the crystallization temperature is 50-95 ℃.
Technical effects
Compared with the prior art, the invention has the following technical effects:
valuable metals such as nickel, cobalt and lithium are separated and recovered by adopting an adsorption method, so that the environmental protection problem of the recovery of the waste ternary lithium battery is solved, the valuable metals are recovered, and the cyclic utilization of resources is realized; the process flow is simple, the cost is low, the recovery process is green and environment-friendly, and the recovery rate and the purity of nickel, cobalt and lithium can reach 95 percent or higher.
Drawings
FIG. 1 is a process flow diagram of examples 1-2.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description. The experimental procedures, in which specific conditions are not specified in the examples, were carried out according to the conventional methods and conditions.
Example 1
As shown in fig. 1, the recycling process of the positive electrode material of the waste nickel-cobalt-manganese ternary lithium battery in this embodiment is as follows:
s1, placing the waste nickel-cobalt-manganese ternary lithium battery in 1.5mol/L NaCl solution for discharging treatment, cleaning and drying the discharged waste nickel-cobalt-manganese ternary lithium battery, and disassembling and stripping to obtain a powder-form positive electrode material; leaching the anode material of the waste nickel-cobalt-manganese ternary lithium battery for 10-60 min by adopting a sulfuric acid solution with the concentration of 5.0 wt%, wherein the solid-to-liquid ratio of the anode material to the sulfuric acid solution is 50 g/g; carrying out filter pressing on the slurry obtained after leaching to obtain a leaching solution A containing nickel, cobalt, manganese and lithium;
s2, adding a sulfuric acid solution with the concentration of 2.0 wt% and hydrogen peroxide with the concentration of 5.0 wt% into the leaching solution A, and stirring for 3 hours at 90 ℃ to obtain a leaching solution B;
s3, adding 3.0 wt% sodium hydroxide solution into the leaching solution B, adjusting the pH value to 3.7, converting aluminum ions in the leaching solution B into aluminum hydroxide precipitate, and filtering to obtain leaching solution C;
s4, adding the leachate C into an adsorption column filled with chelate resin HPMn-1 (provided by Jiangsu Hepu functional materials Co., Ltd.) for adsorption to obtain adsorbed effluent D; desorbing manganese by using 6.0 wt% sulfuric acid, and precipitating by using 10.0 wt% sodium hydroxide solution to recover manganese; adding the adsorption effluent D into an adsorption column filled with chelating resin HP-C/N-1 (provided by Jiangsu Heipu functional materials Co., Ltd.) for adsorption to obtain adsorption effluent E; desorbing cobalt by using sulfuric acid with the concentration of 5.0 wt%, and then precipitating and recovering cobalt by using sodium hydroxide solution with the concentration of 10.0 wt%;
s5, neutralizing the adsorbed effluent E by using a sodium hydroxide solution with the concentration of 10.0 wt%, precipitating, recovering nickel, and filtering to obtain a filtrate F;
s6, adding a saturated sodium carbonate solution into the filtrate F at the temperature of 85 ℃, reacting for 2-3h, crystallizing to separate out lithium carbonate, and recovering.
The ion concentrations before and after recovery were compared to obtain tables 1 and 2.
TABLE 1 summary of various ion concentrations before and after aluminum removal
| Item | Al | Mn | Co | Ni | Li |
| Before precipitation and aluminum removal | 4536ppm | 3724ppm | 3012ppm | 7712ppm | 3612ppm |
| After precipitation and aluminum removal | 135ppm | 3653ppm | 2873ppm | 7546ppm | 3500ppm |
TABLE 2 summary of various ion concentrations before and after adsorption
| Item | Mn | Co | Ni | Li |
| Before treatment | 3653ppm | 2873ppm | 7546ppm | 3500ppm |
| After treatment | 14.3ppm | 36.7ppm | 159ppm | 62.1ppm |
| Recovery rate | 98.4％ | 97.3％ | 97.1％ | 97.2％ |
In the embodiment, the removal rate of aluminum is 97%, the recovery rates of nickel, cobalt and manganese are 97.1%, 97.3% and 98.4% respectively, and the purity can reach 98.3%; the recovery rate of lithium is as high as 97.2%, and the purity reaches 98.21%.
Example 2
As shown in fig. 1, the recycling process of the positive electrode material of the waste nickel-cobalt-manganese ternary lithium battery in this embodiment is as follows:
s1, placing the waste nickel-cobalt-manganese ternary lithium battery in 1.5mol/L NaCl solution for discharging treatment, cleaning and drying the discharged waste nickel-cobalt-manganese ternary lithium battery, and disassembling and stripping to obtain a powder-form positive electrode material; leaching the anode material of the waste nickel-cobalt-manganese ternary lithium battery for 10-60 min by adopting a sulfuric acid solution with the concentration of 5.0 wt%, wherein the solid-to-liquid ratio of the anode material to the sulfuric acid solution is 50 g/g; carrying out filter pressing on the slurry obtained after leaching to obtain a leaching solution A containing nickel, cobalt, manganese and lithium;
s2, adding 1.0 wt% sulfuric acid solution and 5.0 wt% hydrogen peroxide into the leaching solution A, and stirring for 3h at 90 ℃ to obtain leaching solution B;
s3, adding 8.0 wt% of sodium hydroxide solution into the leaching solution B, adjusting the pH value to 3.7, converting aluminum ions in the leaching solution B into aluminum hydroxide precipitate, and filtering to obtain leaching solution C;
s4, adding the leachate C into an adsorption column filled with chelate resin HPMn-1 for adsorption to obtain adsorbed effluent D; desorbing manganese by using 5.0 wt% sulfuric acid, and precipitating by using 10.0 wt% sodium hydroxide solution to recover manganese; adding the adsorption effluent D into an adsorption column filled with chelating resin HP-C/N-1 for adsorption to obtain adsorption effluent E; desorbing cobalt by using sulfuric acid with the concentration of 4.0 wt%, and then precipitating and recovering cobalt by using sodium hydroxide solution with the concentration of 10.0 wt%;
s5, neutralizing the adsorbed effluent E by using a sodium hydroxide solution with the concentration of 10.0 wt%, precipitating, recovering nickel, and filtering to obtain a filtrate F;
s6, adding a saturated sodium carbonate solution into the filtrate F at the temperature of 50 ℃, reacting for 2-3h, crystallizing to separate out lithium carbonate, and recovering.
The ion concentrations before and after recovery were compared to obtain tables 1 and 2.
TABLE 3 summary of various ion concentrations before and after aluminum removal
| Item | Al | Mn | Co | Ni | Li |
| Before precipitation and aluminum removal | 4536ppm | 3724ppm | 3012ppm | 7712ppm | 3612ppm |
| After precipitation and aluminum removal | 135ppm | 3653ppm | 2873ppm | 7546ppm | 3500ppm |
TABLE 4 summary of various ion concentrations before and after adsorption
| Item | Mn | Co | Ni | Li |
| Before treatment | 3653ppm | 2873ppm | 7546ppm | 3500ppm |
| After treatment | 20.1ppm | 41.7ppm | 176ppm | 1254ppm |
| Recovery rate | 99.1％ | 96.7％ | 96.4％ | 62.2％ |
In the embodiment, the removal rate of aluminum is 97%, the recovery rates of nickel, cobalt and manganese are 96.4%, 96.7% and 99.1%, respectively, and the purity can reach 97.9%; the recovery rate of lithium is as high as 62.2%, and the purity reaches 75.3%.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (7)
1. A method for recycling a positive electrode material of a waste nickel-cobalt-manganese ternary lithium battery is characterized by comprising the following steps:
s1, leaching the anode material of the waste nickel-cobalt-manganese ternary lithium battery by using dilute acid, and then performing filter pressing to obtain a leachate A;
s2, adding dilute acid and hydrogen peroxide into the leaching solution A for pretreatment to obtain a leaching solution B;
s3, adjusting the pH value of the leaching solution B, precipitating and removing aluminum ions to obtain a leaching solution C;
s4, adopting chelate resin to adsorb manganese and cobalt in the leaching solution C in sequence, and then obtaining adsorbed effluent; carrying out dilute acid desorption on the chelate resin, and recovering manganese and cobalt after alkali liquor precipitation;
s5, neutralizing the adsorbed effluent by using alkali liquor, precipitating, and recovering nickel to obtain filtrate;
and S6, reacting at a certain temperature, treating the filtrate by adopting a saturated crystallization method, and crystallizing to obtain the lithium carbonate for recovery.
2. The method for recycling the positive electrode material of the waste nickel-cobalt-manganese ternary lithium battery as claimed in claim 1, wherein in step S1, the positive electrode material is obtained by discharging, disassembling and stripping the waste nickel-cobalt-manganese ternary lithium battery, the leaching treatment time of the positive electrode material is 10-60 min, the leaching adopts at least one of dilute acid, sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid and acetic acid, and the acid concentration is 1.0-10.0 wt%; the solid-to-liquid ratio of the anode material to the dilute acid is 20-100 g/g.
3. The method for recycling the anode material of the waste nickel cobalt manganese ternary lithium battery as recited in claim 1, wherein in step S2, the dilute acid is sulfuric acid.
4. The method for recycling the positive electrode material of the waste nickel-cobalt-manganese ternary lithium battery as claimed in claim 1, wherein in step S3, dilute acid is used for adjusting the pH value of the leaching solution B, and precipitation is performed at 55-95 ℃; the pH value after adjustment is 2.2-4.1; the dilute acid is sulfuric acid, and the concentration of the dilute acid is 1.0-5.0 wt%.
5. The method for recycling the anode material of the waste nickel-cobalt-manganese ternary lithium battery as recited in claim 1, wherein in step S4, the chelating resin for adsorbing manganese is HPMn-1, and contains phosphate group, phosphite group, and sulfonic acid group; the chelating resin for adsorbing cobalt is HP-C/N-1, and contains a hypophosphite group and an amino group; the dilute acid is sulfuric acid, and the concentration of the dilute acid is 1.5-10.3 wt%.
6. The method for recycling the anode material of the waste nickel-cobalt-manganese ternary lithium battery as recited in claim 1, wherein in step S5, the alkaline solution contains at least one of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, sodium oxalate and potassium oxalate.
7. The method for recycling the positive electrode material of the waste nickel-cobalt-manganese ternary lithium battery as claimed in claim 1, wherein in the step S6, the precipitant adopted in the saturated crystallization method is sodium carbonate and/or potassium carbonate, and the crystallization temperature is 50-95 ℃.
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Cited By (4)
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| CN113355520A (en) * | 2021-06-08 | 2021-09-07 | 金川镍钴研究设计院有限责任公司 | Treatment process of nickel-containing alloy powder in hydrochloric acid system |
| CN113943864A (en) * | 2021-09-30 | 2022-01-18 | 广东邦普循环科技有限公司 | Method for removing fluorine in waste lithium battery |
| WO2023024593A1 (en) * | 2021-08-25 | 2023-03-02 | 广东邦普循环科技有限公司 | Method for recovering mixed waste of lithium nickel cobalt manganate and lithium iron phosphate |
| CN115747521A (en) * | 2022-12-29 | 2023-03-07 | 江苏电科环保有限公司 | Method for recovering and preparing lithium carbonate from waste lithium ion battery positive electrode material |
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