CN111313120A - Method for recovering cobalt and lithium metals in waste lithium ion battery - Google Patents
Method for recovering cobalt and lithium metals in waste lithium ion battery Download PDFInfo
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- CN111313120A CN111313120A CN202010103559.2A CN202010103559A CN111313120A CN 111313120 A CN111313120 A CN 111313120A CN 202010103559 A CN202010103559 A CN 202010103559A CN 111313120 A CN111313120 A CN 111313120A
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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
- 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
- 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
- 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 discloses a method for recovering cobalt and lithium metals in waste lithium ion batteries, which comprises the following steps: disassembling the waste lithium ion battery to obtain a positive plate; cutting the positive plate into small pieces, soaking the small pieces into a separation liquid, placing the separation liquid soaked with the positive plate in an ultrasonic environment for a period of time, and taking out an aluminum foil to obtain a mixed liquid; carrying out rotary evaporation on the obtained mixed solution to obtain a solid substance, and drying the solid substance to obtain a lithium ion battery anode material; mixing the positive electrode material with a chelating agent and then carrying out mechanical activation treatment to obtain an activated mixture; and performing acid leaching treatment on the obtained activated mixture to obtain enrichment liquid containing cobalt and lithium. The method has the advantages of simple operation method, no secondary pollution in the recovery process, low cost and easy industrial production, and the recovery rate of cobalt and lithium metal of the anode material of the waste lithium ion battery can reach 100 percent.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery recovery, and particularly relates to a method for recovering cobalt and lithium metals in waste lithium ion batteries.
Background
With the development of technology, batteries have become an essential power source for electric appliances in daily life. Since the nineties of the last century, lithium batteries have replaced wired power supplies and fuel power supplies with the remarkable advantages of large capacity, small volume, high specific energy, high working voltage and the like, and have become energy and power guarantees for modern technological development. China is the biggest manufacturing base of lithium batteries in the world, and the scrappage of lithium ion batteries in China reaches 32.2GWh by 2020.
The lithium ion battery belongs to a consumable, and is scrapped due to the reduction of the discharge performance after the use reaches the age limit, and the number of scrapped lithium ion batteries is greatly increased. On one hand, the failed lithium battery contains heavy metals such as cobalt and copper and organic substances such as lithium hexafluorophosphate, and if the heavy metals are randomly discharged, the environment is polluted; on the other hand, metals such as cobalt, lithium, copper and the like contained in the lithium battery are valuable resources, wherein the metal cobalt with the highest content (up to 20 percent) is an internationally accepted strategic material.
Chinese patent (CN102956935A) discloses a method for recovering metal elements from waste power batteries step by step through precipitation. The method can realize all metal elements in the waste power battery, but the process is complex, the pH value of the solution needs to be adjusted in multiple steps, and a large amount of different chemical reagents are added. Chinese patent (CN104659438A) discloses a method for preparing a ternary precursor by using a waste lithium ion battery anode material, which comprises the steps of dissolving the anode material by using sulfuric acid, separating cobalt sulfate and nickel sulfate by using an extraction method, and finally preparing the ternary precursor by mixing the nickel sulfate and the cobalt sulfate and additionally supplementing manganese sulfate. Although the method can recover nickel and cobalt from waste lithium batteries, the operation is complex and secondary pollution cannot be eliminated. Chinese patent (CN104868190A) discloses a method for leaching metals in the anode material of waste lithium ion batteries by using a reducing agent and organic acid, which can improve the metal leaching rate by using organic acid such as formic acid and the like in combination with the reducing agent, but formic acid is expensive, causes secondary pollution to water, and hydrogen peroxide is unstable, and a large amount of potential safety hazards are stored. Chinese patent (CN102665912A) discloses a method for extracting and recovering cobalt and manganese in the anode material of waste lithium batteries and preparing a Co-Mn-Br liquid phase catalyst (CMB catalyst for short), which can recover cobalt and manganese, but has a complex process and needs to consume a large amount of organic solvent, and cannot realize the recycling of the organic solvent.
At present, most of the published patents and researches aim at that the recovery method of the anode material of the waste lithium ion battery is complex to operate or the used reagent causes secondary pollution.
Therefore, it is required to develop a method for recovering a positive electrode material for a lithium ion battery, which can be easily handled and has high recovery efficiency.
Disclosure of Invention
The purpose is as follows: in order to solve the defects of the prior art, the invention provides a method for recovering cobalt and lithium metals in a waste lithium ion battery.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for recovering cobalt and lithium metals in waste lithium ion batteries is characterized by comprising the following steps:
step (1), disassembling a waste lithium ion battery to obtain a positive plate;
cutting the positive plate into small pieces, soaking the small pieces into a separation liquid, placing the separation liquid soaked with the positive plate in an ultrasonic environment for a period of time, and taking out an aluminum foil to obtain a mixed liquid;
step (3), carrying out rotary evaporation on the mixed liquid obtained in the step (2) to obtain a solid substance, and drying the solid substance to obtain the lithium ion battery anode material;
step (4), mixing the positive electrode material obtained in the step (3) with a chelating agent, and then carrying out mechanical activation treatment to obtain an activated mixture;
and (5) carrying out acid leaching treatment on the activated mixture obtained in the step (4) to obtain enriched liquid containing cobalt and lithium.
The positive plate is as follows: the method comprises the following steps of preparing a positive plate, and optionally one or the combination of at least two of the production wastes of the positive plate or the manually disassembled waste positive plate of the lithium ion battery.
In the step (2), the separation liquid comprises an organic solvent; preferably, the organic solvent is Dimethylacetamide (DMAC);
and mixing the positive plate and the separation liquid according to a solid-liquid ratio of 100-500 g/L.
In the step (2), the ultrasonic time is 30-90 min, and the ultrasonic power is 100-300W; the temperature is 20-90 ℃.
In the step (3), the temperature of the rotary evaporation is 60-90 ℃.
In the step (4), the chelating agent is an organic chelating agent;
preferably, the chelating agent is any one or a combination of at least two of nitrilotriacetic acid, sodium aminotriacetate, sodium aminotrimethylphosphate, ethylene diamine tetraacetic acid, hydroxyethylidene diphosphonic acid, diethyl triaminepentaacetic acid, and N- β -hydroxyethyl ethylenediamine triacetic acid;
preferably, the chelating agent and the positive electrode material are mixed according to the weight ratio of 0.5-3 g/g;
preferably, the mechanical activation treatment mode is mechanical ball milling;
preferably, the rotation speed of the mechanical ball milling is 300-500 rpm, the ball milling time is 60-120 min, and the ball-to-material ratio is 3-10 g/g.
In the step (5), the leaching agent used in the acid leaching treatment is organic acid with reducibility;
preferably, the organic acid having reducibility is ascorbic acid;
preferably, the concentration of the leaching agent is 0.25-1 mol/L, the leaching temperature is 25-95 ℃, the leaching time is 10-90 min, the solid-liquid ratio is 20-100 g/L, and the stirring speed is 150-300 rpm.
And (3) recycling the separated liquid in the step (2) in a rotary evaporation mode.
In some embodiments, the method specifically comprises the following steps:
(1) manually disassembling or mechanically crushing the waste lithium ion battery to obtain a positive plate containing an aluminum foil and a positive material;
(2) cutting the positive plate into small pieces with the length of 5cm, soaking the small pieces into a separation liquid, adjusting the solid-to-liquid ratio to be 100-500 g/L, adjusting the temperature of the separation liquid soaked with the positive plate to 20-90 ℃, adjusting the ultrasonic power to 100-300W in an ultrasonic environment, and performing ultrasonic treatment for 30-90 min, and then taking out an aluminum foil to obtain a mixed liquid;
(3) carrying out rotary evaporation on the mixed liquid obtained in the step (2) at the temperature of 60-90 ℃ to obtain a solid substance, and drying the solid substance to obtain a lithium ion battery anode material;
(4) mixing the positive electrode material and the chelating agent in the step (3) according to a weight ratio of 0.5-3 g/g, and then performing mechanical ball milling treatment, wherein the ball milling rotation speed is 300-500 rpm, the ball milling time is 60-120 min, and the ball-to-material ratio is 3-10 g/g, so as to obtain an activated mixture;
(5) and (3) performing acid leaching treatment on the activated mixture obtained in the step (4) by using a leaching solid-liquid ratio of 20-100 g/L, a leaching agent concentration of 0.25-1 mol/L, a leaching temperature of 25-95 ℃, a leaching time of 10-90 min and a stirring speed of 150-300 rpm, and recovering cobalt and lithium metals in the waste lithium ion battery.
In some embodiments, the recovery rate of cobalt and lithium metal in the spent lithium ion battery can reach 100% by the recovery method.
Has the advantages that: the method for recovering cobalt and lithium metal in the waste lithium ion battery provided by the invention has the following advantages: (1) according to the invention, the waste lithium ion battery anode material can be rapidly obtained by means of ultrasonic, and the separation liquid can be recycled in a rotary evaporation manner, so that secondary pollution is avoided; (2) the chelating agent used in the method is a nontoxic or low-toxic organic chelating agent, and a mechanical activation mode is used, so that the energy consumption and the cost are reduced; (3) the selected leaching agent such as ascorbic acid does not cause secondary pollution to the environment, and the dosage of the leaching agent is less, and the cost is low; (4) the method for recovering cobalt and lithium metal in the waste lithium ion battery has simple process, easy industrial production and low cost, and avoids the pollution of waste acid and reducing agent to the environment.
Drawings
Fig. 1 is a flow chart of a process for recovering cobalt and lithium metals from a waste lithium ion battery according to an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1
(1) Taking a certain brand of waste lithium ion battery, and manually disassembling the brand of waste lithium ion battery to obtain 200g of a positive plate containing aluminum foil and a positive material;
(2) cutting 30g of positive plate into small pieces with the length of 5cm and the width of 6cm, soaking the small pieces into 100mL of DMAC (dimethylacetamide), placing a beaker filled with the positive plate and a separation solution in an ultrasonic environment, adjusting the temperature to 30 ℃, adjusting the ultrasonic power to 300W, performing ultrasonic treatment for 60min, and taking out an aluminum foil to obtain a mixed solution;
(3) carrying out rotary evaporation on the mixed solution containing the anode material at the temperature of 80 ℃ to obtain a solid substance, and drying the solid substance at the temperature of 105 ℃ to obtain 14.3g of the anode material of the lithium ion battery;
(4) mixing 10g of positive electrode material and 10g of nitrilotriacetic acid, and then carrying out mechanical ball milling treatment, wherein the ball milling rotation speed is 400rpm, the ball milling time is 90min, and the ball-to-material ratio is 3g/g, so that 19.2g of activated mixture is obtained;
(5) the activated mixture, 19.2g, was acid leached with 500mL of a lixiviant (0.25 mol/L ascorbic acid) in a mixed acid at 80 ℃ for 30min at a leach agitation rate of 200rpm, and filtered through 0.45 micron filter paper to yield 495mL of the enriched liquor. The leaching efficiency of cobalt and lithium was 100%.
Optionally, the separated liquid is reused by rotary evaporation.
Example 2
(1) Taking a certain brand of waste lithium ion battery, and manually disassembling the brand of waste lithium ion battery to obtain 300g of a positive plate containing aluminum foil and a positive material;
(2) cutting 40g of positive plate into small pieces with the length of 5cm and the width of 6cm, soaking the small pieces into 150mL of DMAC (dimethylacetamide), placing a beaker filled with the positive plate and a separation solution in an ultrasonic environment, adjusting the temperature to 50 ℃, adjusting the ultrasonic power to 300W, performing ultrasonic treatment for 60min, and taking out an aluminum foil to obtain a mixed solution;
(3) carrying out rotary evaporation on the mixed solution containing the anode material at the temperature of 80 ℃ to obtain a solid substance, and drying the solid substance at the temperature of 105 ℃ to obtain 25.6g of the anode material of the lithium ion battery;
(4) mixing 25.6g of the positive electrode material with 30g of sodium aminotriacetate, and then carrying out mechanical ball milling treatment, wherein the ball milling rotation speed is 500rpm, the ball milling time is 90min, and the ball-to-material ratio is 3g/g, so that 54.8g of an activation mixture is obtained;
(5) 54.8g of the activated mixture was acid-leached with 1L of a leaching agent (0.25 mol/L ascorbic acid) at 80 ℃ for 15min at a leaching agitation rate of 300rpm, and filtered through 0.45 micron filter paper to obtain 993mL of the enriched solution. The leaching efficiency of cobalt and lithium was 100%.
Optionally, the separated liquid is reused by rotary evaporation.
Example 3
(1) Taking a certain brand of waste lithium ion battery, and manually disassembling the brand of waste lithium ion battery to obtain 200g of a positive plate containing aluminum foil and a positive material;
(2) cutting 30g of positive plate into small pieces with the length of 5cm and the width of 6cm, soaking the small pieces into 100mL of DMAC (dimethylacetamide), placing a beaker filled with the positive plate and a separation solution in an ultrasonic environment, adjusting the temperature to 30 ℃, adjusting the ultrasonic power to 200W, performing ultrasonic treatment for 80min, and taking out an aluminum foil to obtain a mixed solution;
(3) carrying out rotary evaporation on the mixed solution containing the anode material at the temperature of 80 ℃ to obtain a solid substance, and drying the solid substance at the temperature of 105 ℃ to obtain 15.8g of the anode material of the lithium ion battery;
(4) mixing 15.8g of positive electrode material with 20g of disodium ethylene diamine tetraacetate, and then carrying out mechanical ball milling treatment, wherein the ball milling rotation speed is 500rpm, the ball milling time is 90min, and the ball-to-material ratio is 3g/g, so that 35.1g of an activated mixture is obtained;
(5) the activated mixture (35.1 g) was acid leached with 800mL of a lixiviant (0.25 mol/L ascorbic acid) in a mixed acid at 80 ℃ for 15min at a leach agitation rate of 150rpm, and filtered through 0.45 micron filter paper to obtain 795mL of the enriched solution. The leaching efficiency of cobalt and lithium was 100%.
Optionally, the separated liquid is reused by rotary evaporation.
The present invention has been disclosed in terms of the preferred embodiment, but it is not intended to be limited to the embodiment, and all technical solutions obtained by substituting or converting the equivalent embodiments fall within the scope of the present invention.
Claims (10)
1. A method for recovering cobalt and lithium metals in waste lithium ion batteries is characterized by comprising the following steps:
step (1), disassembling a waste lithium ion battery to obtain a positive plate;
cutting the positive plate into small pieces, soaking the small pieces into a separation liquid, placing the separation liquid soaked with the positive plate in an ultrasonic environment for a period of time, and taking out an aluminum foil to obtain a mixed liquid;
step (3), carrying out rotary evaporation on the mixed liquid obtained in the step (2) to obtain a solid substance, and drying the solid substance to obtain the lithium ion battery anode material;
step (4), mixing the positive electrode material obtained in the step (3) with a chelating agent, and then carrying out mechanical activation treatment to obtain an activated mixture;
and (5) carrying out acid leaching treatment on the activated mixture obtained in the step (4) to obtain enriched liquid containing cobalt and lithium.
2. The recycling method according to claim 1, wherein the positive electrode sheet is: the method comprises the following steps of preparing a positive plate, and optionally one or the combination of at least two of the production wastes of the positive plate or the manually disassembled waste positive plate of the lithium ion battery.
3. The recovery method according to claim 1, wherein in the step (2), the separation liquid comprises an organic solvent;
preferably, the organic solvent is dimethylacetamide;
and mixing the positive plate and the separation liquid according to a solid-liquid ratio of 100-500 g/L.
4. The recycling method according to claim 1, wherein in the step (2), the ultrasonic time is 30-90 min, and the ultrasonic power is 100-300W; the temperature is 20-90 ℃.
5. The recycling method according to claim 1, wherein the temperature of the rotary evaporation in the step (3) is 60 to 90 ℃.
6. The recovery method according to any one of claims 1 to 5, wherein in the step (4), the chelating agent is an organic chelating agent;
preferably, the chelating agent is any one of or a combination of at least two of nitrilotriacetic acid, sodium aminotriacetate, sodium aminotrimethosphate, ethylenediaminetetraacetic acid, hydroxyethylidene diphosphonic acid, diethyltriaminepentaacetic acid, and N- β -hydroxyethylethylenediaminetriacetic acid.
7. The recycling method according to any one of claims 1 to 5, wherein in the step (4), the chelating agent and the positive electrode material are mixed in a weight ratio of 0.5 to 3 g/g;
and/or the mechanical activation treatment mode is mechanical ball milling;
preferably, the rotation speed of the mechanical ball milling is 300-500 rpm, the ball milling time is 60-120 min, and the ball-to-material ratio is 3-10 g/g.
8. The recovery method according to any one of claims 1 to 5, wherein in the step (5), the leaching agent used in the acid leaching is an organic acid having a reducing property;
preferably, the leaching agent is ascorbic acid;
preferably, the concentration of the leaching agent is 0.25-1 mol/L, the leaching temperature is 25-95 ℃, the leaching time is 10-90 min, the solid-liquid ratio is 20-100 g/L, and the stirring speed is 150-300 rpm.
9. The recovery method according to claim 1, wherein 0.25mol/L ascorbic acid is used as the leaching agent.
10. The recovery method according to any one of claims 1 to 5, wherein the separated liquid is recovered by rotary evaporation.
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Cited By (2)
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| CN112575203A (en) * | 2020-12-07 | 2021-03-30 | 金川集团股份有限公司 | Method for recycling lithium in waste power lithium battery |
| CN117230312A (en) * | 2023-11-13 | 2023-12-15 | 帕瓦(长沙)新能源科技有限公司 | Alkaline leaching process of waste lithium ion battery anode material |
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| CN112575203A (en) * | 2020-12-07 | 2021-03-30 | 金川集团股份有限公司 | Method for recycling lithium in waste power lithium battery |
| CN117230312A (en) * | 2023-11-13 | 2023-12-15 | 帕瓦(长沙)新能源科技有限公司 | Alkaline leaching process of waste lithium ion battery anode material |
| CN117230312B (en) * | 2023-11-13 | 2024-03-19 | 帕瓦(长沙)新能源科技有限公司 | Alkaline leaching process of waste lithium ion battery anode material |
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Application publication date: 20200619 |