CN114639887A - Method for separating anode powder and current collector in lithium ion battery pole piece - Google Patents
Method for separating anode powder and current collector in lithium ion battery pole piece Download PDFInfo
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- CN114639887A CN114639887A CN202210252705.7A CN202210252705A CN114639887A CN 114639887 A CN114639887 A CN 114639887A CN 202210252705 A CN202210252705 A CN 202210252705A CN 114639887 A CN114639887 A CN 114639887A
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000004642 Polyimide Substances 0.000 claims description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 2
- 229910002993 LiMnO2 Inorganic materials 0.000 claims description 2
- 229910000668 LiMnPO4 Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 229910013100 LiNix Inorganic materials 0.000 claims 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims 1
- 239000006182 cathode active material Substances 0.000 claims 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- OTYYBJNSLLBAGE-UHFFFAOYSA-N CN1C(CCC1)=O.[N] Chemical compound CN1C(CCC1)=O.[N] OTYYBJNSLLBAGE-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 2
- 238000004904 shortening Methods 0.000 abstract 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000006258 conductive agent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for separating pole powder and current collectors in a lithium ion battery pole piece, which comprises the following steps: mixing water and N-methyl pyrrolidone to prepare a stripping agent; step two: heating the stripping agent in the first step to 55-140 ℃; step three: and (3) immersing the battery pole piece into a stripping agent, and carrying out ultrasonic or mechanical stirring to obtain a pole powder layer and a current collector. The separating method of the invention adopts the mixture of water or water and a small part of nitrogen methyl pyrrolidone as the stripping agent, which is used for softening the pole powder layer on the surface of the pole piece to ensure that the pole piece has certain toughness, and then the pole powder is completely fallen off by slight stirring, and the main purpose is to separate the pole powder from the current collector, thus avoiding the mixing of different recovered substances, ensuring that the classified recovered substances have higher purity, being easy to realize industrially, having low cost and relatively small pollution to the environment, shortening the working procedure of recovering the battery materials and improving the quality of the recovered battery materials.
Description
Technical Field
The invention relates to the technical field of lithium ion battery recovery, in particular to a method for separating anode powder and current collectors in a lithium ion battery pole piece.
Background
With global intellectualization and unmanned commercialization, under the background of a large trend of carbon peak reaching and carbon neutralization, green traffic represented by new energy vehicles and clean energy represented by wind energy and photovoltaic energy show huge industrial prospects, the new energy becomes a global tuyere, and the new energy vehicles cannot be blocked in development momentum. The power battery spans from GWH to the TWh era, shows thousands of times of growth space, and the battery material resource is more and more in shortage. Therefore, it is important to clean and recycle the waste battery materials with high efficiency. The method really realizes the closed loop cyclic utilization of the energy from green to green, and can enable the continuous development of the new energy industry in the future to become possible.
Generally, for recycling lithium ion battery pole pieces, pole powder and a metal current collector are separated, and then pole powder copper foil and aluminum foil are respectively recycled. Because the purity requirements of the battery pole piece on copper foil, aluminum foil and positive and negative active materials are very high, the battery pole piece is usually incinerated by a fire method at present, and then pole powder is stripped by a mechanical treatment method, the incineration has serious pollution to the atmosphere, a large amount of dust pollution can be generated by mechanical stripping, copper powder and aluminum powder are easy to mix into the positive material, so that the impurity content of a recovered material is higher, the subsequent impurity removal process is multiple, and the recovery cost is high.
Disclosure of Invention
The invention aims to provide a method for separating pole powder and current collectors in a lithium ion battery pole piece, which is environment-friendly, convenient, rapid and large-batch to realize that a pole powder layer is completely separated from positive and negative current collectors, so that metal foils of the current collectors cannot be mixed into the pole powder, and the pole powder remained in the current collectors is reduced, thereby improving the purity of the recovered copper, aluminum and battery pole powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating pole powder and current collectors in a lithium ion battery pole piece comprises the following steps:
step one, mixing water and N-methyl pyrrolidone to prepare a stripping agent;
step two, heating the stripping agent in the step one to a temperature which is enough to dissolve the adhesive in the pole piece and not to volatilize the stripping agent, wherein the temperature range is 55-140 ℃;
immersing the battery pole piece into a stripping agent, and carrying out ultrasonic or mechanical stirring to accelerate the dissolution of the binder, shorten the time for separating the pole powder from the current collector, simultaneously not damaging the current collector of the pole piece, and introducing impurities to finally obtain a pole powder layer and a current collector;
preferably, in the first step, the content of the azomethidone in the stripping agent is 0-40wt% in terms of mass percentage, that is, the stripping agent is water or a mixture of water and a small part of azomethidone.
Further, in the second step, the heating temperature of the stripping agent is preferably 55-105 ℃, and more preferably 90-105 ℃.
Further, in the third step, the frequency of ultrasonic stirring is 28-100khz, the rotating speed of mechanical stirring is 5-100 r/min, and the stirring time is 0.5-24 h.
Further, in the third step, when the lithium ion battery pole piece is a positive pole piece, the positive active material on the positive pole piece comprises at least one of LiNixCoyMnzOE, LiNixCoyAlzOE, LiFePO4, LiMnPO4 and LiMnO2, the used binder comprises one or more of Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), Polyimide (PI), polyacrylic acid and Polyacrylonitrile (PAN), and the content of the binder in the positive pole piece is 0.2-10 wt%; when the lithium ion battery pole piece is a negative pole piece, the negative active material on the negative pole piece is graphite, a composite negative pole of silicon and graphite or lithium titanate, the used binder comprises one or more of Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), Polyimide (PI), polyacrylic acid (PAA) and Polyacrylonitrile (PAN), carboxymethyl cellulose (CMC-Na), LA133 type water-based binder and Styrene Butadiene Rubber (SBR), and the content of the binder in the negative pole piece is 0.2-10 wt%.
Compared with the prior separation method of the anode powder and the current collector in the lithium ion battery pole piece, the invention has the following beneficial effects:
1. the method can conveniently, quickly and massively realize that the pole powder layers of the positive and negative pole pieces are completely separated from the positive and negative current collectors, in the process, the residual pole powder on the current collectors can be reduced, and metal impurities such as copper, aluminum and the like can not be mixed in the pole powder, so that the subsequent purification and recycling are facilitated.
2. The stripping agent is water or a mixture of water and a small part of N-methyl pyrrolidone, is used for softening a pole powder layer on the surface of a pole piece, enables the pole piece to have certain toughness, and then enables the pole powder to fall off completely through slight stirring.
3. The stripping agent can be repeatedly used, so that the separation cost is further reduced, and the recovery process of the waste lithium ion battery is more environment-friendly.
Drawings
Fig. 1 is a graph showing the peeling effect of the pole powder layer of the battery pole piece in example 1: the figure is a graph of peeling effects at 45, 60, 75, 90 and 105 ℃ from left to right in sequence;
fig. 2 is a graph showing the peeling effect of the pole powder layer of the battery pole piece in example 2: the figure shows the peeling effect under 28, 33, 40, 80 and 100khz in sequence from left to right;
fig. 3 is a graph showing the peeling effect of the pole powder layer of the battery pole piece using pure water as the peeling agent in example 3: the figure shows the peeling effect at 45, 55, 65, 75 and 85 ℃ from left to right.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the method of the present invention is described in detail below with reference to the specific embodiments and the accompanying drawings.
Example 1
Step one, respectively mixing water (60 wt%) and nitrogen methyl pyrrolidone (40 wt%) to obtain a stripping agent;
step two, taking 5 parts of the stripping agent in the step one, and respectively heating the stripping agent to 45 ℃, 60 ℃, 75 ℃, 90 ℃ and 105 ℃;
and step three, selecting a positive pole piece containing NCM523 (nickel-cobalt-manganese ternary lithium)), PVDF (polyvinylidene fluoride) and a conductive agent SP with the mass ratio of 96:2:2, immersing the pole piece in the stripping agents with different temperatures, and stirring for 3 hours at the frequency of 80 Khz. And (3) stripping the pole piece pole powder layer to obtain a relatively complete current collector, wherein the experimental result is shown in table 1 and figure 1.
TABLE 1 NMP and H2Peeling experiment result of O mixed peeling agent on pole piece
Example 2
Step one, respectively mixing water (80 wt%) and nitrogen methyl pyrrolidone (20 wt%) to obtain a stripping agent;
step two, taking 5 parts of the stripping agent in the step one, heating to 70 ℃, selecting a positive pole piece containing NCM523 (nickel-cobalt-manganese ternary lithium)), PVDF (polyvinylidene fluoride) and a conductive agent SP in a mass ratio of 96:2:2, and immersing the pole piece in the stripping agent;
and step three, ultrasonically stirring for 3 hours at frequencies of 28KhZ, 33KhZ, 40KhZ, 80KhZ and 100KhZ respectively, observing the peeling condition of the pole piece pole powder layer, and obtaining the experimental result shown in table 2 and fig. 2.
TABLE 2 peeling test results of pole pieces by ultrasonic agitation
Example 3
Selecting pure water as a stripping agent;
step two, taking 5 parts of the stripping agent in the step one, and respectively heating to 45 ℃, 55 ℃, 65 ℃, 75 ℃ and 85 ℃;
and step three, selecting a negative pole piece containing graphite C, CMC-Na, SBR and a conductive agent SP with the mass ratio of 96:1:2:1, respectively immersing the negative pole piece into the stripping agents with different temperatures in the step two, mechanically stirring for 3 hours at the rotating speed of 50r/min, and observing the stripping condition of the pole piece pole powder layer, wherein the experimental results are shown in table 3 and fig. 3.
TABLE 3 peeling test results of mechanical stirring on pole pieces
The results in the figures and tables show that the pole powder layer can be completely separated from the battery pole piece by adopting the separation method, and the pole powder layer and the current collector obtained by the method can be used for screening and separating valuable metals in the lithium ion battery, detecting components, analyzing structures, analyzing failures and the like, and have obvious application value in the recycling, research, preparation and development of the lithium ion battery.
In summary, compared with the prior art, the method for separating the anode powder and the current collector in the lithium ion battery pole piece provided by the invention can conveniently, quickly, controllably and massively separate the anode powder layer and the cathode powder layer from the anode current collector and the cathode current collector, so that relatively complete current collectors and anode powder can be obtained, copper and aluminum materials in the battery pole piece can be quickly separated, the impurity content of a battery recovery material can be reduced, the purification process of the battery recovery material can be reduced, and the method has great practical significance.
The foregoing is directed to the preferred embodiment of the present invention and, accordingly, it is understood that all changes and modifications that come within the spirit of the invention are desired to be protected by the following claims.
Claims (9)
1. A method for separating pole powder and current collectors in a lithium ion battery pole piece is characterized by comprising the following steps:
step one, mixing water and N-methyl pyrrolidone to prepare a stripping agent;
step two, heating the stripping agent in the step one to 55-140 ℃;
and step three, immersing the battery pole piece into a stripping agent, and carrying out ultrasonic or mechanical stirring to obtain a pole powder layer and a current collector.
2. The method for separating the anode powder and the current collector in the lithium ion battery pole piece according to claim 1, wherein in the first step, the content of the azomethidone in the stripping agent is 0 to 40 wt%.
3. The method for separating the pole powder and the current collector in the lithium ion battery pole piece according to claim 1, wherein in the second step, the heating temperature of the stripping agent is 55-105 ℃.
4. The method for separating the electrode powder and the current collector in the lithium ion battery electrode plate according to claim 3, wherein the heating temperature of the stripping agent is 90-105 ℃.
5. The method for separating the pole powder and the current collector in the pole piece of the lithium ion battery as claimed in claim 1, wherein in the third step, the frequency of the ultrasonic agitation is 28-100 khz.
6. The method for separating the pole powder and the current collector in the pole piece of the lithium ion battery as claimed in claim 1, wherein in the third step, the rotation speed of the mechanical stirring is 5-100 r/min.
7. The method for separating the pole powder and the current collector in the lithium ion battery pole piece according to claim 5 or 6, wherein the stirring time is 0.5-24 h.
8. The method for separating the cathode powder and the current collector in the lithium ion battery pole piece according to any one of claims 1 to 6, wherein in the third step, when the lithium ion battery pole piece is a cathode pole piece, the cathode active material on the cathode pole piece comprises LiNixCoyMnzOE、LiNixCoyAlzOE、LiFePO4、LiMnPO4And LiMnO2The used binder comprises one or more of polytetrafluoroethylene, polyvinylidene fluoride, polyimide, polyacrylic acid and polyacrylonitrile, and the content of the binder in the positive pole piece is 0.2-10 wt%.
9. The method for separating the anode powder and the current collector in the lithium ion battery pole piece according to any one of claims 1 to 6, wherein in the third step, when the lithium ion battery pole piece is a negative pole piece, the negative active material on the negative pole piece is graphite, a composite negative pole of silicon and graphite or lithium titanate, the used binder comprises one or more of polytetrafluoroethylene, polyvinylidene fluoride, polyimide, polyacrylic acid and polyacrylonitrile, sodium carboxymethyl cellulose, LA133 type aqueous binder and styrene butadiene rubber, and the content of the binder in the negative pole piece is 0.2 to 10 wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210252705.7A CN114639887A (en) | 2022-03-15 | 2022-03-15 | Method for separating anode powder and current collector in lithium ion battery pole piece |
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| CN202210252705.7A CN114639887A (en) | 2022-03-15 | 2022-03-15 | Method for separating anode powder and current collector in lithium ion battery pole piece |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115513549A (en) * | 2022-09-15 | 2022-12-23 | 厦门海辰储能科技股份有限公司 | Electrode piece recycling method |
| WO2024093096A1 (en) * | 2022-11-02 | 2024-05-10 | 广东邦普循环科技有限公司 | Method for circularly stripping waste positive electrode sheet current collector and positive electrode material by using nmp |
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| CN115513549B (en) * | 2022-09-15 | 2024-01-26 | 厦门海辰储能科技股份有限公司 | Recovery method of electrode plate |
| WO2024093096A1 (en) * | 2022-11-02 | 2024-05-10 | 广东邦普循环科技有限公司 | Method for circularly stripping waste positive electrode sheet current collector and positive electrode material by using nmp |
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