CN112786989A - Method for separating active material layer and current collector of battery electrode plate - Google Patents
Method for separating active material layer and current collector of battery electrode plate Download PDFInfo
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- CN112786989A CN112786989A CN202110286216.9A CN202110286216A CN112786989A CN 112786989 A CN112786989 A CN 112786989A CN 202110286216 A CN202110286216 A CN 202110286216A CN 112786989 A CN112786989 A CN 112786989A
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- active material
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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
Abstract
The invention relates to the field of recovery of key materials of lithium ion batteries, in particular to a method for separating an active material layer and a current collector of a battery electrode plate. The method comprises the following steps: dissolving CO2 or/and SO2 gas in weak acid salt solution by a pressurization method to obtain solution A; mixing the battery pole piece with the solution A, reducing the pressure and/or raising the temperature to enable the gas to escape, and stirring and oscillating to obtain a mixture A; sieving the mixture A to separate and recover a current collector and a mixture B; and filtering and recovering the mixture B to obtain an active material layer. The method has the advantages of simple process, short flow, environmental protection, separation rate of the active material layer and the current collector of more than 98 percent, high purity of the recovered active material layer and the recovered current collector, expansion of the application field of the method and improvement of economic value.
Description
Technical Field
The invention relates to the field of recovery of key materials of lithium ion batteries, in particular to a method for separating an active material layer and a current collector of a battery electrode plate.
Background
Through the development of the last 30 years, the manufacturing and assembling of each component in the lithium ion battery and the use and maintenance technology of the battery are quite mature. With the increase of the usage amount of the lithium ion battery, the retirement amount of the lithium ion battery is increased. The cumulative amount of decommissioning of lithium ion power batteries, a member of lithium ion batteries, is about 8.4 to 12.4 ten thousand tons in 2019 nationwide, and is expected to exceed 73 ten thousand tons by 2025 years. Therefore, the amount of retirement of the lithium ion battery will increase greatly as the service life increases.
In the retired lithium ion battery, the comprehensive ratio of a current collector and an active material layer is the largest, the economic value is the highest, and the recovery of the current collector and the active material layer is very important. It is important to grasp the manufacturing process of the electrode sheet of the battery in order to separately recover the high-purity current collector and the high-purity active material layer. The manufacturing steps of the battery electrode plate are as follows: first, an active material, conductive carbon black, an additive, a binder, and the like (the above mixed materials are collectively referred to as an active material layer) are uniformly mixed to make a slurry. And then coating the slurry on a current collector and drying to obtain the battery electrode plate. And the current collector and the active material layer are bonded through an adhesive to realize interface bonding. After the pole piece is rolled, the pores among the particles in the active material layer are reduced, the compaction density is increased, and the interface bonding force between the active material layer and the current collector is increased, so that the difficulty degree of the separation of the active material layer and the current collector is increased, and the current collector and the active material layer are difficult to be separated cleanly and thoroughly by common water. In the prior art, CN106654437A, CN110534834A, CN110661055A and CN109216822A adopt a heat treatment method to separate the negative electrode active material layer from the copper foil. CN109216819A, CN111384462A, CN111430831A and CN104241723A adopt a solvent soaking mode to separate the active material layer from the current collector. CN107069078A extrudes and sieves the powder obtained by crushing the negative plate to obtain cake-shaped current collector particles (i.e. copper particles) on the sieve and electrode material powder (i.e. negative active material layer) under the sieve. CN111987380A uses ultrasonic means to separate the active material layer from the current collector.
In the above separation technique, there are the following disadvantages: (1) first, the heat treatment decomposes the binder to generate exhaust gas. Secondly, if the heat treatment is carried out in an aerobic environment, the copper foil of the current collector is easy to oxidize to generate copper oxide, and the aluminum foil of the current collector is also further oxidized to generate aluminum oxide, so that the purity of the current collector is reduced. If the heat treatment is carried out in an oxygen-free environment, the adhesive on the contact interface of the current collector and the active material layer can be decomposed to generate carbon which is connected between the current collector and the active material layer, so that the separation difficulty of the current collector and the active material layer is increased. (2) Single solvent soaking and sonication cannot separate all types of electrode pads; (3) the purity of the active material layer and the collector powder obtained by mechanical pulverization is low; (4) acid and/or alkali solution soaking is effective in separating the active material layer and the current collector, but is liable to generate waste liquid.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for separating an active material layer from a current collector by mixing a solution dissolved with gas with a battery electrode plate, regulating and controlling pressure and/or temperature to enable the gas in the solution to escape, and utilizing the gas to arch a solid-solid combined interface of the active material layer and the current collector to reduce the interface bonding force. The method can separate different types of battery electrode plates, and has strong applicability; the current collector and the active material layer obtained by separation have high purity, and the active material layer can be directly repaired and recycled; the treatment method is simple and the process flow is short.
In order to achieve the above object, the present invention provides a method for separating an active material layer from a current collector of a battery electrode sheet, the method comprising the steps of:
s1, dissolving CO2 or/and SO2 gas in weak acid salt solution by a pressurization method to obtain solution A;
s2, mixing the battery pole piece with the solution A, reducing pressure and/or raising temperature to enable the gas to escape, and stirring and vibrating to obtain a mixture A;
s3, screening the mixture A to separate and recover a current collector and a mixture B;
and S4, filtering and recovering the mixture B to obtain an active material layer.
Further, the weak acid salt solution is one or more of potassium carbonate, sodium carbonate, lithium carbonate, potassium bicarbonate, lithium bicarbonate, sodium bicarbonate, potassium acetate, sodium acetate, lithium acetate, sodium oxalate, potassium oxalate and lithium oxalate solution.
Further, the mass ratio of the battery pole piece to the solution A in the step S2 is 1:5-50, preferably 1: 10-30.
Further, in the step of gas escape, a pressure reduction method is adopted, wherein the pressure is-0.1-0.1 MPa.
Further, in the step of allowing the gas to escape by using a temperature raising method, the temperature is 5 to 90 ℃, preferably 10 to 30 ℃.
Further, in step S2, the stirring and oscillating process parameters are as follows:
the stirring speed is 5-300rpm, preferably 50-200rpm, and the stirring time is 0.5-24h, preferably 1-10 h.
Has the advantages that:
(1) the invention adjusts the solubility of gas in water by adopting the matching of pressure and/or temperature, utilizes the gas to escape to arch the interface of the current collector and the active material layer, reduces the interface binding force, realizes the separation of the active material layer and the current collector, overcomes the problem that the separation method in the prior art is limited by the type of the electrode plate of the battery to generate waste gas and waste liquid, has simple process, short flow, high product purity, saves resources and protects ecological environment. After the electrode plate and the gas-containing solution are mixed, gas is enriched on a contact interface of the current collector and the active material layer, the gas is separated from the solution in an escape process, new stress is generated on the contact surface of the current collector and the active material layer, an interface bonding layer of the active material layer and the current collector is damaged, and the active material is separated from the current collector.
(2) According to the separation method disclosed by the invention, the escaped gas can be recycled, the solution for dissolving the gas is prepared by re-pressurizing, the solvent can be recycled, no waste liquid or waste gas is generated in the whole process, the method can be used for a positive plate and a negative plate of a battery, different types of electrode plates can be separated, the adaptability is strong, the purity of the active material obtained by separation is high, the active material can be directly recycled, the purity of the current collector obtained by separation is high, the economic value is high, and the development trend of green and economic industries is compounded.
(3) According to the invention, by optimizing the process parameters such as the mass ratio, the pressure intensity range and the temperature range of the gas-containing solution and the electrode plate, the separation effect of the active material and the current collector is further improved, the separation rate can reach more than 98%, the separation efficiency is high, the resource utilization rate is high, the flexibility of equipment operation is improved, and the service life of the equipment is prolonged.
Drawings
Fig. 1 is a process flow chart of a method for separating an active material layer from a current collector of a battery electrode plate according to an embodiment of the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
As shown in fig. 1, an embodiment of the present invention provides a process flow diagram of a method for separating an active material layer from a current collector of a battery electrode plate, wherein a solution in which gas is dissolved is mixed with the electrode plate, the gas escapes by reducing pressure or controlling temperature to obtain a mixed solution, and finally, a current collector material and an electrode active material are obtained by sieving and filtering, respectively.
The following examples are further illustrative.
Example 1
The embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a negative active material layer from a copper foil in a negative electrode plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the electrode plate of the battery according to the proportion of 5:1, reducing the pressure to 0.1Mpa, and controlling the temperature of the mixture A to be 5 ℃; stirring was carried out for 0.5h at a rotation speed of 300rpm to obtain a mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
Example 2:
the embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a negative active material layer from a copper foil in a negative electrode plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the electrode plate of the battery according to the proportion of 10:1, reducing the pressure to 0.05Mpa, and controlling the temperature of the mixture A to be 10 ℃; stirring is carried out for 1h at the rotation speed of 200rpm, thus obtaining a mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
Example 3
The embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a positive active material layer from an aluminum foil in a positive plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the battery electrode plate according to the proportion of 25:1, reducing the pressure to 0Mpa, and controlling the temperature of the mixture A to be 25 ℃; stirring was carried out for 10 hours at a rotation speed of 200rpm to obtain a mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
Example 4
The embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a positive active material layer from an aluminum foil in a positive plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the electrode plate of the battery according to the proportion of 30:1, reducing the pressure to-0.02 Mpa, and controlling the temperature of the mixture A to be 65 ℃; stirring was carried out for 18 hours at 50rpm to obtain mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
Example 5
The embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a negative active material layer from a copper foil in a negative electrode plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the electrode plate of the battery according to the proportion of 50:1, reducing the pressure to-0.01 Mpa, and controlling the temperature of the mixture A to be 90 ℃; stirring was carried out for 24 hours at 5rpm to obtain a mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
Example 6
The embodiment provides a method for separating an active material layer from a current collector in a battery electrode plate, which is mainly used for separating a negative active material layer from a copper foil in a negative electrode plate, and comprises the following steps:
dissolving CO2 gas in water in a pressurizing mode to form a solution A in which CO2 gas is dissolved; mixing the solution A and the electrode plate of the battery according to the proportion of 30:1, reducing the pressure to 0.01Mpa, and controlling the temperature of the mixture A to be 25 ℃; stirring was carried out for 1 hour at 50rpm to obtain a mixture A. Sieving the mixture A, separating and recovering a current collector to obtain a mixture B; and filtering and separating the mixture B to recover the active material layer.
The mass M of the electrode sheet in the embodiments 1 to 6 of the present invention was measured respectively1Mass M of separated active material layer2And measuring the thickness of the electrode plate current collector after separation, and taking the quality of the current collector with the thickness in the industry as the original quality M0And (3) calculating the separation rate by adopting a formula (1), and meanwhile, calculating the content of the current collector active material layer.
Separation rate [ M ═ M2/(M1-M0)]*100％ (1)
The separation effect of examples 1 to 6 is shown in Table 1.
TABLE 1 separation Rate and active Material layer content of the examples
| Examples | Separation rate/%) | Content of active material layer in current collector% |
| Example 1 | 98.2 | 1.8 |
| Example 2 | 98.5 | 1.5 |
| Example 3 | 98.9 | 1.1 |
| Example 4 | 99.2 | 0.8 |
| Example 5 | 98.7 | 1.3 |
| Example 6 | 99.4 | 0.6 |
According to the result, the separation effect of the active material layer and the current collector is good, the separation rate can reach more than 98%, and the mass ratio of the gas-containing solution to the electrode plate is optimized, so that the use amount of the solution can be effectively reduced, the energy consumption is reduced, the utilization rate of resources is improved, and the separation efficiency of the active material layer and the current collector is effectively improved. Within a specific pressure range, the separation efficiency of the active material layer and the current collector can be ensured, the flexibility of equipment operation is improved, and the service life of the equipment is prolonged. In the optimized temperature range, the interfacial force provided by the carbon dioxide and the sulfur dioxide during the gathering and arching can be effectively kept still.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.
Claims (6)
1. A method for separating an active material layer from a current collector of a battery electrode plate is characterized by comprising the following steps:
s1, mixing CO2Or/and SO2Dissolving gas in weak acid salt solution by a pressurization method to obtain solution A;
s2, mixing the battery pole piece with the solution A, reducing pressure and/or raising temperature to enable the gas to escape, and stirring and vibrating to obtain a mixture A;
s3, screening the mixture A to separate and recover a current collector and a mixture B;
and S4, filtering and recovering the mixture B to obtain an active material layer.
2. The method for separating the active material layer from the current collector of the battery electrode plate according to claim 1, wherein the weak acid salt solution is one or more of potassium carbonate, sodium carbonate, lithium carbonate, potassium bicarbonate, lithium bicarbonate, sodium bicarbonate, potassium acetate, sodium acetate, lithium acetate, sodium oxalate, potassium oxalate, and lithium oxalate solutions.
3. The method for separating an active material layer from a current collector of a battery electrode sheet according to claim 1, wherein the mass ratio of the battery electrode sheet to the solution A in the step S2 is 1: 5-50.
4. The method for separating an active material layer from a current collector of a battery electrode sheet according to claim 1, wherein the pressure in the step of releasing the gas by using a pressure reduction method is-0.1 to 0.1 MPa.
5. The method for separating an active material layer from a current collector of a battery electrode sheet according to claim 1, wherein the step of escaping the gas by using an elevated temperature method is performed at a temperature of 5 to 90 ℃.
6. The method for separating an active material layer from a current collector of a battery electrode sheet according to claim 1, wherein in the step S2, the stirring and shaking process parameters are as follows:
the stirring speed is 5-300rpm, and the stirring time is 0.5-24 h.
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