CN116140073A - Method for carrying out flotation separation on anode and cathode mixed materials of waste lithium iron phosphate battery - Google Patents
Method for carrying out flotation separation on anode and cathode mixed materials of waste lithium iron phosphate battery Download PDFInfo
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- CN116140073A CN116140073A CN202310157309.0A CN202310157309A CN116140073A CN 116140073 A CN116140073 A CN 116140073A CN 202310157309 A CN202310157309 A CN 202310157309A CN 116140073 A CN116140073 A CN 116140073A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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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
- 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 separating positive and negative electrode mixed materials of a waste lithium iron phosphate battery by floatation, which belongs to the technical field of waste battery recycling. The invention has the advantages of simple flow, convenient operation, high production efficiency and the like.
Description
Technical Field
The invention belongs to the technical field of recycling of waste lithium batteries, and particularly relates to a method for separating positive and negative mixed materials of a waste lithium iron phosphate battery by floatation.
Background
In the 21 st century, with continuous consumption of traditional energy sources such as coal, petroleum and natural gas and increasingly outstanding environmental problems, development of sustainable energy sources has become an important way to solve the energy problems. With the development of technology and social progress, lithium batteries are gradually paid attention to and widely applied to the fields of information technology, electric automobiles, digital products, energy storage and the like due to the advantages of high energy density, high working voltage, environmental friendliness in use and production processes, small self-discharge, no memory effect, good cycle performance, long service life and the like. With the rapid development of new energy industry and the wide application of lithium batteries, the price of energy metal is continuously increased, so that the production cost of downstream industries is pressure-bearing, and the further development of the new energy industry is limited to a certain extent. Meanwhile, the treatment of the waste lithium batteries is also a great technical problem at present, and if the waste lithium batteries cannot be properly treated, the waste lithium batteries not only harm the environment, but also cause resource waste. Therefore, research on the aspect of efficient recycling of waste lithium batteries is carried out, so that the recycling of energy metal and the development of new energy industries can be promoted, the environment can be protected, and important economic and social significance is achieved.
As a main power battery, a lithium iron phosphate battery is generally composed of a positive electrode, a negative electrode, an electrolyte, a separator, and the like. In general, the waste lithium battery needs to be recycled by carrying out pretreatment operations such as disassembly, discharge, crushing, screening, color selection, reselection and the like to recycle valuable components such as copper foil, aluminum foil, anode and cathode mixed materials, and then separating and recycling the anode and cathode mixed materials by adopting a physical, chemical or physical-chemical combination method. Among the separation and recovery means, flotation is an important means for separating anode and cathode mixed materials because of the advantages of cleanliness, high efficiency, environmental protection, low production cost and the like, and is also receiving attention of people.
Under natural conditions, the positive and negative electrode materials are easy to separate through flotation due to the fact that the natural hydrophobicity of the positive and negative electrode materials is greatly different, however, as the positive and negative electrode mixture materials still contain the adhesive PVDF, lithium hexafluorophosphate and other harmful components, the harmful components can further cover the surface of the positive electrode material lithium iron phosphate, the hydrophobicity of the positive and negative electrode mixture materials is increased, and the flotation separation efficiency of the positive and negative electrode mixture materials is affected. Therefore, aiming at the problems, the development of a clean and efficient lithium iron phosphate battery anode and cathode mixture material recovery and separation method has important significance.
Disclosure of Invention
The invention aims to provide a method for separating positive and negative electrode mixed materials of a waste lithium iron phosphate battery by floatation, which solves the problems of difficult activation and separation of positive electrode materials in the current waste battery material recovery process.
In order to achieve the purpose, the invention provides a method for separating positive and negative mixed materials of a waste lithium iron phosphate battery by floatation, which comprises the following steps:
(1) And carrying out ultrasonic washing treatment on the mixed material by adopting an organic solvent.
(2) And (3) carrying out water stirring washing operation on the organic solvent washing material.
(3) And (3) mixing the washing materials with water, placing the mixture in a flotation tank, stirring, sequentially adding a dispersing agent, an inhibitor, a collector and a foaming agent in the stirring process, and performing roughing operation, wherein roughing sediment is a lithium iron phosphate concentrate product.
(4) Carrying out twice carefully choosing operation on the roughing foam product, returning sediment sequentially, and adding an inhibitor and a foaming agent in one carefully choosing stage; the second stage of fine selection is blank fine selection, and the final foam product is a graphite concentrate product.
Preferably, in the step (1), the organic detergent is one or more of acetic acid, methanol and ethanol.
Preferably, in step (1), the washing time is 5 to 40 minutes.
Preferably, in step (1), the washing is carried out in an ultrasonic cleaner having a frequency of 30KHz and 50KHz and a power of 100 to 500W.
Preferably, in the step (2), an electromechanical stirrer is adopted for the water washing, and the stirring speed is 300-2000 r/min.
Preferably, in step (2), the concentration of the washing slurry is 5% -20%.
Preferably, in step (2), the washing time is 3 to 30 minutes.
Preferably, in the step (3), a 1L self-sucking mechanical stirring flotation machine is adopted for the flotation operation, the rotation speed of the flotation machine is 2000r/min, and the flotation time is 5min.
Preferably, in the step (3), the concentration of the flotation slurry is 8% -40%.
Preferably, in the step (3), the dispersing agent is one or more of sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate, and the dosage is 50-400 g/t.
In the steps (3) and (4), the inhibitor is one or more of phytic acid, citric acid and polyaspartic acid, and the dosage is 30-300 g/t.
In the step (3), the collecting agent is one or two of kerosene and diesel oil, and the dosage is 30-250 g/t.
In the steps (3) and (4), the foaming agent is No. 2, and the dosage is 10-100 g/t.
Compared with the prior art, the invention has the following beneficial effects: (1) The invention adopts the organic solvent to carry out ultrasonic washing on the mixed electrode material, can fully remove organic solvent on the surface of the electrode material, and enlarges the difference of hydrophobicity on the surface of the electrode material; (2) The invention can further remove organic matters and organic solvent residues on the surface of the electrode material by stirring and washing, thereby being beneficial to the subsequent flotation separation; (3) The invention carries out multistage floatation operation on the foam product (graphite) to obtain the high-purity electrode material product.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings and preferred embodiments in order to facilitate an understanding of the invention, but the scope of the invention is not limited to the following specific embodiments.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
(1) Mixing 500g of waste lithium iron phosphate battery powder with 1500g of methanol, and placing the mixture in an ultrasonic cleaning agent for ultrasonic cleaning, wherein the ultrasonic frequency and power are respectively set to be 30KHZ and 300W, and the cleaning time is 20min.
(2) And filtering the material subjected to ultrasonic cleaning by using the organic solvent to obtain battery powder, mixing the battery powder with 3L of water to obtain mixed slurry, stirring and washing, wherein the stirring speed is 1000r/min, and the stirring time is 20min.
(3) And filtering the materials subjected to stirring and washing to obtain battery powder, placing the battery powder into a 1.5L flotation tank, mixing the battery powder with water, stirring and pulping at a stirring rotation speed of 2000rpm, sequentially adding 200g/t sodium tripolyphosphate, 150g/t citric acid, 100g/t kerosene and 30g/t No. 2 during stirring, and carrying out roughing operation after stirring for 5min, wherein roughing sediment is a lithium iron phosphate positive electrode concentrate product.
(4) Placing the flotation foam product obtained by flotation into a 1L flotation tank, further mixing with water, stirring and pulping at a stirring speed of 2000rpm, sequentially adding 100g/t citric acid and 20g/t No. 2 in the stirring process, carrying out a period of fine selection operation after stirring, carrying out flotation for 5min, and returning a period of fine selection sediment to carry out rough selection.
(5) And (3) placing the first-stage carefully-selected foam product into a 1L flotation tank for size mixing, wherein the stirring rotating speed in the size mixing process is 2000rpm, performing blank second-stage carefully-selected operation after size mixing is finished, combining the second-stage carefully-selected sediment and roughing concentrate for first-stage carefully-selected, taking the second-stage carefully-selected foam product as a graphite concentrate product, and repeatedly performing 8 times of experiments, wherein the test indexes reach an equilibrium state.
And finally, the cathode graphite powder with the recovery rate and the grade of 98.54 percent and 97.66 percent respectively can be obtained through detection.
Example 2
(1) Mixing 500g of waste lithium iron phosphate battery powder with 1500g of ethanol, and placing the mixture in an ultrasonic cleaning agent for ultrasonic cleaning, wherein the ultrasonic frequency and power are respectively set to be 30KHZ and 350W, and the cleaning time is 18min.
(2) And filtering the material subjected to ultrasonic cleaning by using the organic solvent to obtain battery powder, mixing the battery powder with 3L of water to obtain mixed slurry, stirring and washing, wherein the stirring speed is 1500r/min, and the stirring time is 15min.
(3) And filtering the materials subjected to stirring and washing to obtain battery powder, placing the battery powder into a 1.5L flotation tank, mixing the battery powder with water, stirring and pulping at a stirring rotation speed of 2000rpm, sequentially adding 150g/t sodium hexametaphosphate, 180g/t phytic acid, 80g/t diesel oil and 30g/t No. 2 during stirring, carrying out roughing operation after stirring, wherein the flotation time is 5min, and roughing sediment is a lithium iron phosphate positive electrode concentrate product.
(4) Placing the flotation foam product obtained by flotation into a 1L flotation tank, further mixing with water, stirring and pulping at a stirring speed of 2000rpm, sequentially adding 90g/t phytic acid and 20g/t No. 2 in the stirring process, carrying out a period of fine selection operation after stirring, carrying out flotation for 5min, and returning a period of fine selection sediment to carry out rough selection.
(5) And (3) placing the first-stage carefully-selected foam product into a 1L flotation tank for size mixing, wherein the stirring rotating speed in the size mixing process is 2000rpm, performing blank second-stage carefully-selected operation after size mixing is finished, combining the second-stage carefully-selected sediment and roughing concentrate for first-stage carefully-selected, taking the second-stage carefully-selected foam product as a graphite concentrate product, and repeatedly performing 8 times of experiments, wherein the test indexes reach an equilibrium state.
And finally, detecting to obtain the cathode graphite powder with the recovery rate and grade of 98.58% and 97.71% respectively and 99.86% and 98.66% respectively.
Example 3
(1) Mixing 500g of waste lithium iron phosphate battery powder with 1500g of ethanol, and placing the mixture in an ultrasonic cleaning agent for ultrasonic cleaning, wherein the ultrasonic frequency and power are respectively set to be 50KHZ and 400W, and the cleaning time is 18min.
(2) And filtering the material subjected to ultrasonic cleaning by using the organic solvent to obtain battery powder, mixing the battery powder with 3L of water to obtain mixed slurry, stirring and washing, wherein the stirring speed is 1500r/min, and the stirring time is 15min.
(3) And filtering the materials subjected to stirring and washing to obtain battery powder, placing the battery powder into a 1.5L flotation tank, mixing the battery powder with water, stirring and pulping at a stirring rotation speed of 2000rpm, sequentially adding 180g/t sodium pyrophosphate, 200g/t tannic acid, 80g/t diesel oil and 30g/t No. 2 in the stirring process, carrying out roughing operation after stirring and knotting, wherein the flotation time is 5min, and roughing sediment is a lithium iron phosphate positive electrode concentrate product.
(4) Placing the flotation foam product obtained by flotation into a 1L flotation tank, further mixing with water, stirring and pulping at a stirring speed of 2000rpm, sequentially adding 95g/t tannic acid and 20g/t No. 2 in the stirring process, carrying out a period of fine selection operation after stirring, carrying out flotation for 5min, and returning a period of fine selection sediment to carry out rough selection.
(5) And (3) placing the first-stage carefully-selected foam product into a 1L flotation tank for size mixing, wherein the stirring rotating speed in the size mixing process is 2000rpm, performing blank second-stage carefully-selected operation after size mixing is finished, combining the second-stage carefully-selected sediment and roughing concentrate for first-stage carefully-selected, taking the second-stage carefully-selected foam product as a graphite concentrate product, and repeatedly performing 8 times of experiments, wherein the test indexes reach an equilibrium state.
And finally, the cathode graphite powder with the recovery rate and the grade of 98.55 percent and 97.69 percent respectively can be obtained through detection.
Example 4
(1) Mixing 500g of waste lithium iron phosphate battery powder with 1500g of ethanol, and placing the mixture in an ultrasonic cleaning agent for ultrasonic cleaning, wherein the ultrasonic frequency and power are respectively set to be 50KHZ and 500W, and the cleaning time is 185min.
(2) And filtering the material subjected to ultrasonic cleaning by using an organic solvent to obtain battery powder, mixing the battery powder with 3.5L of water to obtain mixed slurry, stirring and washing, wherein the stirring speed is 2000r/min, and the stirring time is 13min.
(3) And filtering the materials subjected to stirring and washing to obtain battery powder, placing the battery powder into a 1.5L flotation tank, mixing the battery powder with water, stirring and pulping at a stirring rotation speed of 2000rpm, sequentially adding 200g/t sodium hexametaphosphate, 180g/t tannic acid, 110g/t kerosene and 35g/t No. 2 in the stirring process, carrying out roughing operation after stirring and forming, wherein the flotation time is 5min, and roughing sediment is a lithium iron phosphate positive electrode concentrate product.
(4) Placing the flotation foam product obtained by flotation into a 1L flotation tank, further mixing with water, stirring and pulping at a stirring speed of 2000rpm, sequentially adding 110g/t tannic acid and 30g/t No. 2 in the stirring process, carrying out a period of fine selection operation after stirring, carrying out flotation for 5min, and returning a period of fine selection sediment to carry out rough selection.
(5) And (3) placing the first-stage carefully-selected foam product into a 1L flotation tank for size mixing, wherein the stirring rotating speed in the size mixing process is 2000rpm, performing blank second-stage carefully-selected operation after size mixing is finished, combining the second-stage carefully-selected sediment and roughing concentrate for first-stage carefully-selected, taking the second-stage carefully-selected foam product as a graphite concentrate product, and repeatedly performing 8 times of experiments, wherein the test indexes reach an equilibrium state.
And finally, the cathode graphite powder with the recovery rate and the grade of 98.79 percent and 97.25 percent respectively can be obtained through detection, and the recovery rate and the grade of 99.89 percent and 98.55 percent respectively.
Claims (10)
1. A method for separating anode and cathode mixed materials of a waste lithium iron phosphate battery by floatation is characterized by comprising the following steps:
(1) Ultrasonic washing is carried out on the mixed material by adopting an organic solvent;
(2) Carrying out water stirring washing operation on the organic solvent washing material;
(3) Mixing the washing materials with water, placing the mixture in a flotation tank, stirring, sequentially adding a dispersing agent, an inhibitor, a collector and a foaming agent in the stirring process, and performing roughing operation, wherein roughing sediment is a lithium iron phosphate concentrate product;
(4) Carrying out twice carefully choosing operation on the roughing foam product, returning sediment sequentially, and adding an inhibitor and a foaming agent in one carefully choosing stage; the second stage of fine selection is blank fine selection, and the final foam product is a graphite concentrate product.
2. The method for separating the anode and cathode mixture materials of the waste lithium iron phosphate battery by floatation, which is disclosed in claim 1, is characterized in that in the step (1), the organic detergent is one or more of acetic acid, methanol and ethanol.
3. The method for separating the anode and cathode mixture materials of the waste lithium iron phosphate battery by floatation according to claim 1, wherein in the step (1), the washing time is 5-40 min.
4. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by floatation according to claim 1, wherein in the step (1), washing is performed in an ultrasonic cleaner with the frequency of 30KHZ and 50KHZ and the power of 100-500W.
5. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by floatation, which is disclosed in claim 1, is characterized in that in the step (2), an electromechanical stirrer is adopted for washing, and the stirring speed is 300-2000 r/min.
6. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by floatation, which is disclosed in claim 1, is characterized in that in the step (2), the concentration of the washing slurry is 5% -20%.
7. The method for separating the anode and cathode mixture materials of the waste lithium iron phosphate battery by floatation according to claim 1, wherein in the step (2), the washing time is 3-30 min.
8. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by flotation according to claim 1, wherein in the step (3), a 1L self-suction mechanical stirring flotation machine is adopted for the flotation operation, the rotation speed of the flotation machine is 2000r/min, and the flotation time is 5min.
9. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by floatation, which is disclosed in claim 1, is characterized in that in the step (3), the concentration of the floatation slurry is 8% -40%.
10. The method for separating the anode and cathode mixed materials of the waste lithium iron phosphate battery by floatation, which is characterized in that in the step (3), the dispersant is one or more of sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate, and the dosage is 50-400 g/t;
in the step (3) and the step (4), the inhibitor is one or more of phytic acid, citric acid and polyaspartic acid, and the dosage is 30-300 g/t;
in the step (3), the collecting agent is one or two of kerosene and diesel oil, and the dosage is 30-250 g/t;
in the steps (3) and (4), the foaming agent is No. 2 oil, and the dosage is 10-100 g/t.
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| CN202310157309.0A CN116140073A (en) | 2023-02-23 | 2023-02-23 | Method for carrying out flotation separation on anode and cathode mixed materials of waste lithium iron phosphate battery |
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| CN202310157309.0A CN116140073A (en) | 2023-02-23 | 2023-02-23 | Method for carrying out flotation separation on anode and cathode mixed materials of waste lithium iron phosphate battery |
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Citations (5)
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| CN112756104A (en) * | 2020-12-28 | 2021-05-07 | 湖南邦普循环科技有限公司 | Wet sorting process for waste lithium batteries and application thereof |
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| CN115213023A (en) * | 2022-08-17 | 2022-10-21 | 湖南五创循环科技有限公司 | A method for improving the flotation separation efficiency of positive and negative electrode materials of waste lithium batteries |
| CN115672560A (en) * | 2022-08-23 | 2023-02-03 | 中南大学 | A method for separation and recovery of waste lithium iron phosphate positive and negative electrode materials |
| US20230038978A1 (en) * | 2021-08-02 | 2023-02-09 | Ascend Elements, Inc. | Lithium Iron Phosphate (LFP) battery recycling |
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2023
- 2023-02-23 CN CN202310157309.0A patent/CN116140073A/en active Pending
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| CN112756104A (en) * | 2020-12-28 | 2021-05-07 | 湖南邦普循环科技有限公司 | Wet sorting process for waste lithium batteries and application thereof |
| US20230038978A1 (en) * | 2021-08-02 | 2023-02-09 | Ascend Elements, Inc. | Lithium Iron Phosphate (LFP) battery recycling |
| CN115213023A (en) * | 2022-08-17 | 2022-10-21 | 湖南五创循环科技有限公司 | A method for improving the flotation separation efficiency of positive and negative electrode materials of waste lithium batteries |
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