CN111088430A - Recovery processing method of waste slurry of lithium battery positive electrode - Google Patents
Recovery processing method of waste slurry of lithium battery positive electrode Download PDFInfo
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- CN111088430A CN111088430A CN201911371198.3A CN201911371198A CN111088430A CN 111088430 A CN111088430 A CN 111088430A CN 201911371198 A CN201911371198 A CN 201911371198A CN 111088430 A CN111088430 A CN 111088430A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering and treating waste slurry of a lithium battery anode, which belongs to the technical field of recovery and treatment of lithium battery anode materials, and adopts a method of solid-liquid separation by a centrifuge, recovering NMP by normal pressure distillation, calcining solid phase at high temperature, crushing by a crusher, and finally leaching and recovering metal.
Description
Technical Field
The invention belongs to the technical field of lithium battery anode material recovery and treatment, and particularly relates to a recovery and treatment method of lithium battery anode waste slurry.
Background
Lithium ion batteries are widely used in the fields of mobile communication, notebook computers, electric bicycles, electric automobiles and the like due to their advantages of high energy density, light weight, long service life, low self-discharge rate, no memory effect and the like. The main part of the lithium ion battery is a positive plate and a negative plate, the positive plate is usually prepared by uniformly mixing a positive active material, a conductive agent and a binder into slurry and coating the slurry on a current collector aluminum foil, wherein the positive active material is generally a lithium compound, such as lithium cobaltate, lithium manganate, lithium iron phosphate and the like, and the positive active material accounts for about 30-40% of the total cost of the battery. The positive active material is made into slurry and coated on a current collector, and waste slurry is inevitably generated in the links of unqualified slurry generated due to incorrect proportioning, waste liquid generated by cleaning a storage tank, a pipeline or the ground and the like when the positive active material of the lithium battery is manufactured, so that not only is resource waste caused, but also environmental pollution is easily caused due to improper treatment. Therefore, in order to save costs and protect the environment, it is necessary to recover the waste cathode slurry. The components of the lithium battery anode slurry comprise an anode material, carbon powder, NMP (solvent) for short, N-methyl pyrrolidone, PVDF (adhesive) for short, polyvinylidene fluoride and other impurities. Some systems and methods for recycling waste slurry of positive electrodes of lithium batteries appear in the market at present, for example, chinese patent document 201610662341.4 discloses a system and a method for recycling waste slurry of positive electrodes of lithium ion batteries, the disclosed recycling system realizes continuous and efficient recycling of waste slurry of positive electrodes in lithium ion battery production, can ensure the purity of recycled materials, has high efficiency and little pollution, but the technical scheme lacks an NMP recycling method, and the recycling process is complicated; the same chinese patent document 201610157841.9 discloses a method for recovering waste slurry of positive electrode material of lithium ion battery, which adopts NMP as a solvent for preparing slurry in production to mix with the waste slurry of positive electrode material of lithium ion battery, then the NMP is distilled to remove water, no new component is introduced in the treatment process, the waste slurry can be directly used for battery pole piece slurry drawing after treatment, the operation is simple and the implementation is easy, but the technical scheme prepares a solid-liquid mixture by introducing NMP as a solvent for preparing slurry, and the method for directly using the prepared solid-liquid mixture for pole piece slurry drawing can realize the recovery and reuse of the waste slurry, but the metal elements in the waste slurry are still not separated, and the method is not matched with the actual production process. Therefore, the provided process method which can effectively separate the metal elements in the waste slurry of the positive electrode of the lithium battery and can realize the NMP recovery treatment has important significance for environmental protection, cost reduction and matching with the existing actual production process.
Disclosure of Invention
The invention aims to: the method for recovering and treating the waste slurry of the positive electrode of the lithium battery adopts a centrifuge to separate solid from liquid, distills and recovers NMP at normal pressure, calcines solid phase at high temperature, crushes the solid phase by a crusher, and finally leaches and recovers metal.
The technical scheme adopted by the invention is as follows:
a method for recycling waste slurry of a lithium battery positive electrode comprises the following steps:
the method comprises the following steps: filtering and separating: filtering and separating the positive electrode slurry to obtain an NMP liquid phase and a positive electrode material solid phase;
step two: and (3) distillation and recovery: distilling the NMP liquid phase obtained in the step one, and purifying to obtain pure NMP liquid;
step three: and (3) calcining: calcining the solid phase of the cathode material obtained in the step one at a high temperature in a calcining furnace;
step four: crushing: processing the calcined anode material by a pulverizer to obtain anode material powder;
step five: leaching: and carrying out acid leaching recovery process on the positive electrode material powder to recover each metal element.
The filtration mode in the first step is centrifugal filtration, and the aperture of the filter cloth is 200-800 meshes.
The distillation process in the second step is normal pressure distillation, and the distillation temperature is 80-100 ℃.
The calcining temperature in the calcining furnace in the third step is 300-600 ℃.
And a tail gas absorption device is fixedly connected to the calcining furnace in the third step.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1) the method adopts the solid-liquid separation of a centrifuge, the normal pressure distillation to recover the NMP, the high temperature calcination of the solid phase, the crushing of a crusher and the final leaching to recover the metal, has simple process and easy implementation, can recover the recyclable NMP, contributes to saving resources and reducing the cost;
2) the method provided by the invention has the advantages that the NMP and the metal elements in the waste slurry are separated and recovered, the recovery efficiency is high, the pollution is low, the treatment cost of the traditional waste slurry can be effectively reduced, and the method has market competitiveness compared with the prior art, and is matched with the conventional battery anode material recovery process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to various embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for recycling waste slurry of a lithium battery positive electrode comprises the following steps:
the method comprises the following steps: filtering and separating: filtering and separating the anode slurry by adopting a centrifugal filtration mode, wherein the aperture of filter cloth is 200-400 meshes to obtain an NMP liquid phase and an anode material solid phase, and the centrifugal filtration mode is convenient for the anode material solid phase to be coagulated and separated out and can also be carried out by adopting a stirring filtration mode;
step two: and (3) distillation and recovery: distilling the NMP liquid phase obtained in the step one at normal pressure and at the distillation temperature of 80-85 ℃, and purifying to obtain pure NMP liquid;
step three: and (3) calcining: calcining the solid phase of the anode material obtained in the step one in a calcining furnace at the temperature of 300-;
step four: crushing: processing the calcined anode material by a pulverizer to obtain anode material powder;
step five: leaching: and carrying out acid leaching recovery process on the positive electrode material powder to recover each metal element.
Example 2
A method for recycling waste slurry of a lithium battery positive electrode comprises the following steps:
the method comprises the following steps: filtering and separating: filtering and separating the positive slurry in a centrifugal filtering mode, wherein the aperture of filter cloth is 400-600 meshes to obtain an NMP liquid phase and a positive material solid phase;
step two: and (3) distillation and recovery: distilling the NMP liquid phase obtained in the step one at normal pressure and at the distillation temperature of 85-95 ℃, and purifying to obtain pure NMP liquid;
step three: and (3) calcining: calcining the solid phase of the anode material obtained in the step one in a calcining furnace at the temperature of 400-;
step four: crushing: processing the calcined anode material by a pulverizer to obtain anode material powder;
step five: leaching: and carrying out acid leaching recovery process on the positive electrode material powder to recover each metal element.
Example 3
A method for recycling waste slurry of a lithium battery positive electrode comprises the following steps:
the method comprises the following steps: filtering and separating: filtering and separating the positive slurry in a centrifugal filtering mode, wherein the aperture of filter cloth is 600-800 meshes to obtain an NMP liquid phase and a positive material solid phase;
step two: and (3) distillation and recovery: distilling the NMP liquid phase obtained in the step one at normal pressure and at the distillation temperature of 95-100 ℃, and purifying to obtain pure NMP liquid;
step three: and (3) calcining: calcining the solid phase of the anode material obtained in the step one in a calcining furnace at the temperature of 500-;
step four: crushing: processing the calcined anode material by a pulverizer to obtain anode material powder;
step five: leaching: and carrying out acid leaching recovery process on the positive electrode material powder to recover each metal element.
Experiments show that in the ranges of the aperture of the filter cloth of 200-800 meshes, the distillation temperature of 80-100 ℃ and the calcination temperature of 300-600 ℃, the standard reaching rate of the waste slurry can be improved along with the increase of the aperture number of the filter cloth, the distillation temperature and the distillation temperature, but if the aperture number of the filter cloth and the distillation temperature are too high, the requirements on the filter cloth, a distillation tower and a calciner are more strict, the treatment cost is increased, and further, in order to ensure the effective treatment and recovery of the waste slurry, the aperture of the filter cloth is preferably 800 meshes, the distillation temperature of 95 ℃ and the calcination temperature of about 500 ℃.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A method for recycling waste slurry of a lithium battery anode is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: filtering and separating: filtering and separating the positive electrode slurry to obtain an NMP liquid phase and a positive electrode material solid phase;
step two: and (3) distillation and recovery: distilling the NMP liquid phase obtained in the step one, and purifying to obtain pure NMP liquid;
step three: and (3) calcining: calcining the solid phase of the cathode material obtained in the step one at a high temperature in a calcining furnace;
step four: crushing: processing the calcined anode material by a pulverizer to obtain anode material powder;
step five: leaching: and carrying out acid leaching recovery process on the positive electrode material powder to recover each metal element.
2. The method for recycling the waste slurry of the positive electrode of the lithium battery as claimed in claim 1, wherein: the filtration mode in the first step is centrifugal filtration, and the aperture of the filter cloth is 200-800 meshes.
3. The method for recycling the waste slurry of the positive electrode of the lithium battery as claimed in claim 1, wherein: the distillation process in the second step is normal pressure distillation, and the distillation temperature is 80-100 ℃.
4. The method for recycling the waste slurry of the positive electrode of the lithium battery as claimed in claim 1, wherein: the calcining temperature in the calcining furnace in the third step is 300-600 ℃.
5. The method for recycling the waste slurry of the positive electrode of the lithium battery as claimed in claim 4, wherein: and a tail gas absorption device is fixedly connected to the calcining furnace in the third step.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112652832A (en) * | 2020-12-22 | 2021-04-13 | 东莞市和鸿升新材料科技有限公司 | Method for preparing negative electrode material by recycling negative electrode slurry |
| CN113173875A (en) * | 2021-05-12 | 2021-07-27 | 南京长江江宇环保科技有限公司 | Method for recycling N-methyl pyrrolidone from waste anode electrode slurry in lithium battery production |
| CN113540602A (en) * | 2021-06-22 | 2021-10-22 | 广东邦普循环科技有限公司 | Processing method and application of scrapped positive electrode slurry |
| CN113690502A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Method for recycling waste battery slurry |
| CN113764759A (en) * | 2021-07-28 | 2021-12-07 | 广东邦普循环科技有限公司 | Recovery method of waste lithium battery slurry |
| CN114583310A (en) * | 2022-03-08 | 2022-06-03 | 荆门亿纬创能锂电池有限公司 | Method for recycling lithium ion battery cathode slurry |
| WO2024045515A1 (en) * | 2022-08-31 | 2024-03-07 | 广东邦普循环科技有限公司 | Recovery method and production line for lithium iron phosphate positive electrode waste slurry |
| WO2024055550A1 (en) * | 2022-09-16 | 2024-03-21 | 广东邦普循环科技有限公司 | Recycling method for positive electrode paste of spent lithium-ion batteries and use thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112652832A (en) * | 2020-12-22 | 2021-04-13 | 东莞市和鸿升新材料科技有限公司 | Method for preparing negative electrode material by recycling negative electrode slurry |
| CN113173875A (en) * | 2021-05-12 | 2021-07-27 | 南京长江江宇环保科技有限公司 | Method for recycling N-methyl pyrrolidone from waste anode electrode slurry in lithium battery production |
| CN113540602A (en) * | 2021-06-22 | 2021-10-22 | 广东邦普循环科技有限公司 | Processing method and application of scrapped positive electrode slurry |
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| WO2022267421A1 (en) * | 2021-06-22 | 2022-12-29 | 广东邦普循环科技有限公司 | Method for treating scrapped positive electrode slurry, and application |
| CN113540602B (en) * | 2021-06-22 | 2023-02-14 | 广东邦普循环科技有限公司 | Processing method and application of scrapped positive electrode slurry |
| US20240039069A1 (en) * | 2021-06-22 | 2024-02-01 | Guangdong Brunp Recycling Technology Co., Ltd. | Method for treating scrapped positive electrode slurry, and application |
| GB2621934A (en) * | 2021-06-22 | 2024-02-28 | Guangdong Brunp Recycling Technology Co Ltd | Method for treating scrapped positive electrode slurry, and application |
| CN113690502B (en) * | 2021-07-23 | 2024-03-08 | 广东邦普循环科技有限公司 | Method for recycling waste battery slurry |
| CN113690502A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Method for recycling waste battery slurry |
| CN113764759A (en) * | 2021-07-28 | 2021-12-07 | 广东邦普循环科技有限公司 | Recovery method of waste lithium battery slurry |
| CN113764759B (en) * | 2021-07-28 | 2024-05-10 | 广东邦普循环科技有限公司 | Recovery method of waste lithium battery slurry |
| CN114583310B (en) * | 2022-03-08 | 2024-03-15 | 荆门亿纬创能锂电池有限公司 | Method for recycling lithium ion battery negative electrode slurry |
| CN114583310A (en) * | 2022-03-08 | 2022-06-03 | 荆门亿纬创能锂电池有限公司 | Method for recycling lithium ion battery cathode slurry |
| WO2024045515A1 (en) * | 2022-08-31 | 2024-03-07 | 广东邦普循环科技有限公司 | Recovery method and production line for lithium iron phosphate positive electrode waste slurry |
| WO2024055550A1 (en) * | 2022-09-16 | 2024-03-21 | 广东邦普循环科技有限公司 | Recycling method for positive electrode paste of spent lithium-ion batteries and use thereof |
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