CN111342163A - Method for recovering positive active material of waste lithium battery - Google Patents
Method for recovering positive active material of waste lithium battery Download PDFInfo
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- CN111342163A CN111342163A CN202010268776.7A CN202010268776A CN111342163A CN 111342163 A CN111342163 A CN 111342163A CN 202010268776 A CN202010268776 A CN 202010268776A CN 111342163 A CN111342163 A CN 111342163A
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- lithium battery
- positive plate
- active material
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- waste lithium
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
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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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A method for recovering a positive active material of a waste lithium battery. The invention adopts the plasma technology to process the positive plate, and the process steps comprise deep discharge of the lithium battery, positive plate acquisition and positive plate processing. The invention utilizes the advantages of lower processing temperature and larger cooling rate of the plasma technology, the lower processing temperature avoids the aluminum foil current collector from softening and crushing, and the larger cooling rate is beneficial to the separation of the anode active material and the aluminum foil current collector. The invention has short time for processing the positive plate and high processing efficiency, and the generated harmful gas can be absorbed to avoid polluting the environment. The experimental result shows that after the positive plate is treated by adopting the plasma technology, the aluminum foil current collector is not broken, and the positive active material and the aluminum foil current collector are better separated.
Description
Technical Field
The invention relates to a method for recovering a positive active material of a waste lithium battery, belonging to the technical field of lithium battery recovery.
Background
The electric automobile has no tail gas emission and no pollution to the environment. The development of the electric automobile industry increases the demand of lithium batteries, and the production of lithium battery cathode materials is increased. This increases the demand for lithium resources and cobalt resources. During the use of the electric automobile, the battery capacity is continuously reduced, and when the battery capacity is reduced to 80% of the initial capacity, the battery is retired and is no longer used as a power battery. The retired lithium battery contains high-value lithium elements and cobalt elements, the direct abandonment of the retired lithium battery can cause resource waste and environmental pollution, and the recycling of the waste lithium battery is beneficial to resource saving and environmental protection.
The lithium battery positive electrode comprises an aluminum foil current collector, a conductive agent carbon black, a binder polyvinylidene fluoride and a positive electrode active material, and high-value lithium resources and cobalt resources exist in the positive electrode active material. In order to recycle the lithium resource and the cobalt resource, it is necessary to first recover the active material in the positive electrode. Current methods for recovering the positive electrode active material include a dissolution-heating method and a direct heating method. The dissolving-heating method comprises the steps of deeply discharging the waste lithium battery, removing a lithium battery shell, taking out the positive plate, dissolving polyvinylidene fluoride serving as a binder in the positive electrode by using an organic solvent, filtering and drying, and removing carbon black serving as a conductive agent in the positive electrode by using a high-temperature heating process to obtain the positive active material. The direct heating method comprises the steps of deeply discharging the lithium battery, removing a shell of the lithium battery, taking out the positive plate, heating the positive plate, and decomposing a binder polyvinylidene fluoride and an oxidation conductive agent carbon black by using high temperature to obtain the positive active material. The dissolution-heating method has more steps and longer treatment time. The temperature in the direct heating method is generally around 600 ℃, and the high-temperature heating easily causes the softening and crushing of the aluminum foil current collector, so that the aluminum foil is difficult to separate from the positive active material.
A method having fewer steps and better effects is required for recovering the positive active material.
Disclosure of Invention
The invention aims to overcome the defect of high-temperature heating in the conventional lithium battery positive active material recovery technology, and designs a method for recovering a waste lithium battery positive active material.
According to the technical scheme, the method for recycling the positive active material of the waste lithium battery comprises the steps of processing a positive plate of the lithium battery by adopting a microwave plasma technology, decomposing a binder polyvinylidene fluoride and a conductive agent carbon black at a lower temperature, and promoting the separation of the positive active material and an aluminum foil current collector by utilizing the large cooling rate of the microwave plasma.
A method for recycling positive active materials of waste lithium batteries comprises the following steps:
(1) deeply discharging the waste lithium battery, preparing a sodium chloride solution with the concentration of 15g/L, and soaking the waste lithium battery in the sodium chloride solution for 10 hours to deeply discharge the waste lithium battery; the lithium cell was then dried at 80 ℃ for 4 h.
(2) The method comprises the steps of obtaining a lithium battery positive plate, removing a waste lithium battery shell, taking out the positive plate, soaking the positive plate in absolute ethyl alcohol for 1 hour, and then drying at 60 ℃ for 2 hours.
(3) Processing a lithium battery positive plate, namely processing the positive plate by adopting a plasma method, putting the positive plate into a plasma device, and vacuumizing to 10Pa by utilizing a mechanical vacuum pump; introducing oxygen into the plasma device, and treating the positive plate for 25-35min under proper microwave power condition, proper oxygen flow condition and proper internal air pressure condition of the plasma device; the gas pumped by the mechanical pump is absorbed by 0.5mol/L sodium hydroxide solution, so that the hydrogen fluoride gas generated in the reaction chamber is prevented from polluting the air; and (4) after the reaction is finished, closing the microwave power supply, cooling the positive plate to room temperature, and recovering the positive active material.
The suitable power in step (3) is 350-450W.
The suitable gas flow rate in the step (3) is 60-80 mL/min.
The suitable air pressure in the step (3) is 7-9 kPa.
The temperature of the positive plate processed in the step (3) is 420-480 ℃.
The invention has the advantages of lower treatment temperature and higher cooling rate. The microwave plasma method generates oxygen plasma, can oxidize and decompose the adhesive polyvinylidene fluoride and the conductive agent acetylene black at a lower temperature, and avoids softening and crushing of the aluminum foil current collector caused by high temperature. The microwave plasma method inputs energy into the reaction chamber through microwaves, after the reaction is finished, the microwaves stop inputting, the positive plate is rapidly cooled, and the separation of the positive active material and the aluminum foil current collector is promoted at a high cooling rate. In addition, when the positive electrode plate is treated by the microwave plasma method, the generated hydrogen fluoride gas can be absorbed, and the air pollution is prevented.
Detailed Description
Example 1:
in the embodiment, a sodium chloride solution with the concentration of 15g/L is prepared, and the waste lithium battery is placed into the sodium chloride solution to be soaked for 10 hours; the lithium cell was then dried at 80 ℃ for 4 h.
Removing the shell of the waste lithium battery, taking out the positive plate, and soaking the positive plate in absolute ethyl alcohol for 1 hour; then dried at 60 ℃ for 2 h.
And (3) putting the positive plate into a microwave plasma device, vacuumizing to 10Pa by using a mechanical vacuum pump, introducing oxygen into the device, adjusting the oxygen flow to 70mL/min, controlling the internal air pressure of the plasma device to be 8kPa, and inputting microwaves into the reaction chamber, wherein the microwave power is 400W. And (3) treating the positive plate for 30min by using microwave plasma, wherein the temperature of the positive plate is near 450 ℃, and gas pumped out by a mechanical pump is absorbed by 0.5mol/L sodium hydroxide solution. And (4) after the reaction is finished, closing the microwave power supply, and cooling the positive plate to room temperature to obtain the positive active material.
The experimental result of the embodiment shows that the aluminum foil current collector is not broken, and the positive active material and the aluminum foil current collector are well separated.
Example 2:
in the embodiment, a sodium chloride solution with a concentration of 15g/L is prepared, a waste lithium battery is placed into the sodium chloride solution to be soaked for 10 hours, and then the lithium battery is dried for 4 hours at a temperature of 80 ℃.
Removing the shell of the waste lithium battery, taking out the positive plate, soaking the positive plate in absolute ethyl alcohol for 1h, and then drying at 60 ℃ for 2 h.
And (3) putting the positive plate into a microwave plasma device, vacuumizing to 10Pa by using a mechanical vacuum pump, introducing oxygen into the device, adjusting the oxygen flow to be 60mL/min, controlling the internal air pressure of the plasma device to be 7kPa, and inputting microwaves into the reaction chamber, wherein the microwave power is 350W. And (3) treating the positive plate for 35min by using microwave plasma, wherein the temperature of the positive plate is about 420 ℃, and gas pumped out by a mechanical pump is absorbed by 0.5mol/L sodium hydroxide solution. And (4) after the reaction is finished, closing the microwave power supply, and cooling the positive plate to room temperature to obtain the positive active material.
The experimental result of the embodiment shows that the aluminum foil current collector is not broken, and the positive active material and the aluminum foil current collector are well separated.
Example 3:
in the embodiment, a sodium chloride solution with a concentration of 15g/L is prepared, a waste lithium battery is placed into the sodium chloride solution to be soaked for 10 hours, and then the lithium battery is dried for 4 hours at a temperature of 80 ℃.
Removing the shell of the waste lithium battery, taking out the positive plate, soaking the positive plate in absolute ethyl alcohol for 1h, and then drying at 60 ℃ for 2 h.
And putting the positive plate into a microwave plasma device, vacuumizing to 10Pa by using a mechanical vacuum pump, introducing oxygen into the device, adjusting the oxygen flow to 80mL/min, controlling the internal air pressure of the plasma device to be 9kPa, and inputting microwaves into the reaction chamber, wherein the microwave power is 450W. And (3) treating the positive plate for 25min by using microwave plasma, wherein the temperature of the positive plate is near 480 ℃, and gas pumped out by a mechanical pump is absorbed by 0.5mol/L sodium hydroxide solution. And (4) after the reaction is finished, closing the microwave power supply, and cooling the positive plate to room temperature to obtain the positive active material.
The experimental result of the embodiment shows that the aluminum foil current collector is not broken, and the positive active material and the aluminum foil current collector are well separated.
Claims (5)
1. A method for recovering a positive active material of a waste lithium battery is characterized in that a microwave plasma method is adopted to treat a positive plate and recover the positive active material; the method comprises the following steps:
(1) preparing a sodium chloride solution with the concentration of 15g/L, and soaking the waste lithium battery in the sodium chloride solution for 10 hours to deeply discharge the waste lithium battery; then drying the lithium battery for 4h at 80 ℃;
(2) removing the shell of the waste lithium battery, taking out the positive plate, soaking the positive plate in absolute ethyl alcohol for 1h, and then drying at 60 ℃ for 2 h;
(3) processing the positive plate by adopting a plasma method, putting the positive plate into a plasma device, and vacuumizing to 10Pa by utilizing a mechanical vacuum pump; introducing oxygen into the plasma device, and treating the positive plate for 25-35min under proper microwave power condition, proper oxygen flow condition and proper internal air pressure condition of the plasma device; the gas pumped by the mechanical pump is absorbed by 0.5mol/L sodium hydroxide solution, so that the hydrogen fluoride gas generated in the reaction chamber is prevented from polluting the air; and (4) after the reaction is finished, closing the microwave power supply, cooling the positive plate to room temperature, and recovering the positive active material.
2. The method as claimed in claim 1, wherein the suitable microwave power is 350-450W.
3. The method for recycling the positive active material of the waste lithium battery as claimed in claim 1, wherein the suitable oxygen flow rate is 60-80 mL/min.
4. The method for recycling the positive active material of the waste lithium battery as claimed in claim 1, wherein the internal pressure of the suitable plasma device is 7-9 kPa.
5. The method for recycling the positive active material of the waste lithium battery as claimed in claim 1, wherein the temperature of the positive plate is 420-480 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010268776.7A CN111342163A (en) | 2020-04-08 | 2020-04-08 | Method for recovering positive active material of waste lithium battery |
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| CN202010268776.7A CN111342163A (en) | 2020-04-08 | 2020-04-08 | Method for recovering positive active material of waste lithium battery |
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| CN202010268776.7A Pending CN111342163A (en) | 2020-04-08 | 2020-04-08 | Method for recovering positive active material of waste lithium battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11590568B2 (en) | 2019-12-19 | 2023-02-28 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
| US11633785B2 (en) | 2019-04-30 | 2023-04-25 | 6K Inc. | Mechanically alloyed powder feedstock |
| US11717886B2 (en) | 2019-11-18 | 2023-08-08 | 6K Inc. | Unique feedstocks for spherical powders and methods of manufacturing |
| US11839919B2 (en) | 2015-12-16 | 2023-12-12 | 6K Inc. | Spheroidal dehydrogenated metals and metal alloy particles |
| US11855278B2 (en) | 2020-06-25 | 2023-12-26 | 6K, Inc. | Microcomposite alloy structure |
| US11919071B2 (en) | 2020-10-30 | 2024-03-05 | 6K Inc. | Systems and methods for synthesis of spheroidized metal powders |
| US11963287B2 (en) | 2020-09-24 | 2024-04-16 | 6K Inc. | Systems, devices, and methods for starting plasma |
| CN118213656A (en) * | 2024-03-28 | 2024-06-18 | 广东华菁新能源科技有限公司 | Positive plate recycling method suitable for retired lithium ion power battery |
| US12040162B2 (en) | 2022-06-09 | 2024-07-16 | 6K Inc. | Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows |
| US12042861B2 (en) | 2021-03-31 | 2024-07-23 | 6K Inc. | Systems and methods for additive manufacturing of metal nitride ceramics |
| US12094688B2 (en) | 2022-08-25 | 2024-09-17 | 6K Inc. | Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (PIP) |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11839919B2 (en) | 2015-12-16 | 2023-12-12 | 6K Inc. | Spheroidal dehydrogenated metals and metal alloy particles |
| US11633785B2 (en) | 2019-04-30 | 2023-04-25 | 6K Inc. | Mechanically alloyed powder feedstock |
| US11717886B2 (en) | 2019-11-18 | 2023-08-08 | 6K Inc. | Unique feedstocks for spherical powders and methods of manufacturing |
| US11590568B2 (en) | 2019-12-19 | 2023-02-28 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
| US11855278B2 (en) | 2020-06-25 | 2023-12-26 | 6K, Inc. | Microcomposite alloy structure |
| US11963287B2 (en) | 2020-09-24 | 2024-04-16 | 6K Inc. | Systems, devices, and methods for starting plasma |
| US11919071B2 (en) | 2020-10-30 | 2024-03-05 | 6K Inc. | Systems and methods for synthesis of spheroidized metal powders |
| US12042861B2 (en) | 2021-03-31 | 2024-07-23 | 6K Inc. | Systems and methods for additive manufacturing of metal nitride ceramics |
| US12040162B2 (en) | 2022-06-09 | 2024-07-16 | 6K Inc. | Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows |
| US12094688B2 (en) | 2022-08-25 | 2024-09-17 | 6K Inc. | Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (PIP) |
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Application publication date: 20200626 |
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