CN111129635A - Method and device for separating anode material and cathode material of waste lithium battery - Google Patents
Method and device for separating anode material and cathode material of waste lithium battery Download PDFInfo
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- CN111129635A CN111129635A CN201911301731.9A CN201911301731A CN111129635A CN 111129635 A CN111129635 A CN 111129635A CN 201911301731 A CN201911301731 A CN 201911301731A CN 111129635 A CN111129635 A CN 111129635A
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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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- 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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/30—Combinations with other devices, not otherwise provided for
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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 provides a method for separating anode and cathode materials of waste lithium batteries, which comprises the following steps: carrying out reductive roasting on the anode and cathode materials of the waste lithium battery; crushing and grinding the anode and cathode materials subjected to reductive roasting; carrying out filter pressing on the crushed and ground positive and negative electrode materials to remove impurities so as to obtain a positive and negative electrode mixed material; and carrying out magnetic separation twice on the positive and negative electrode mixed materials, and separating and purifying to obtain a cobalt-nickel-manganese product and a graphite product. The invention also provides a device corresponding to the method. The method and the device have the advantages of high recovery rate of the anode material and graphite, high purification degree, simple and convenient process path, low energy consumption, no secondary pollution and high anode and cathode separation rate of more than 98 percent.
Description
Technical Field
The invention belongs to the technical field of waste lithium battery recovery, and particularly relates to a method for separating positive and negative electrode materials of a waste lithium battery.
Background
At present, methods such as flotation, acid leaching, chemical precipitation, solvent extraction and the like are mostly adopted to separate and recycle positive and negative electrode materials of a lithium battery, the invention patent of China (a comprehensive recycling method of the positive and negative electrodes of a scrapped lithium battery) (He Jun Wei et al, patent number 201810768128.0) discloses that insoluble nickel, cobalt, manganese and carbon enter a solid phase, a beneficiation reagent is added into the solid phase in an environment containing carbonate radicals for flotation after washing, carbon is separated from nickel, cobalt and manganese, the negative electrode material is obtained through washing, activating, drying and sorting, and the separated nickel, cobalt and manganese are directly used as raw materials of nickel, cobalt and manganese multielement precursor materials after being washed by pure water. The methods use a large amount of medicaments, particularly organic heteropolar substances such as foaming agents and collecting agents, water glass, hydrochloric acid, flake caustic soda and other medicaments, bring secondary pollution to the environment, simultaneously have low recovery rate and low purification degree of the anode material, and have high requirements on corrosion resistance of equipment and process pipelines by strong acid and strong alkali, and large industrial application investment.
Therefore, it is necessary to provide a method for separating the anode and cathode materials of the waste lithium battery, which has the advantages of simple process flow, low energy consumption, no secondary pollution, high recovery rate of cobalt, nickel, manganese and graphite products and high purification degree.
Disclosure of Invention
The invention aims to provide a method for separating positive and negative electrode materials of waste lithium batteries, and aims to solve the technical problems that in the prior art, the positive electrode and the negative electrode cannot be effectively separated, the acid consumption in the leaching process is high, and graphite cannot be well recycled.
The invention provides a method for separating anode and cathode materials of waste lithium batteries, which comprises the following steps:
carrying out reductive roasting on the anode and cathode materials of the waste lithium battery;
crushing and grinding the anode and cathode materials subjected to reductive roasting;
carrying out filter pressing on the crushed and ground positive and negative electrode materials to remove impurities so as to obtain a positive and negative electrode mixed material;
and carrying out magnetic separation twice on the positive and negative electrode mixed materials, and separating and purifying to obtain a cobalt-nickel-manganese product and a graphite product.
Furthermore, the magnetic field intensity of the first magnetic separation is 2000-5000 Oe, and the magnetic induction intensity of the second magnetic separation is 10000 Gs-15000 Gs.
Furthermore, the temperature of the reductive roasting is 850-1000 ℃, and the time is 2-5 h.
Further, adding an ecological activating agent during reductive roasting, wherein the ecological activating agent is one or a combination of more of nano-scale graphite, particle laminar graphite, biological rice hull carbon, refined charcoal, high-purity bamboo charcoal and high-fineness activated carbon.
Further, during the reductive roasting, a stabilizing gas is filled at the tail of the roasting furnace.
Further, the stabilizing gas is nitrogen.
Further, crushing and grinding the reducibly roasted anode and cathode materials in a wet grinding mode; the concentration of the anode and cathode materials during wet grinding is 45-67%.
Further, the concentration of the anode and cathode mixed material is 8% -20%.
A device for realizing the method for separating the anode material and the cathode material of the waste lithium battery is characterized by comprising a roasting furnace, a horizontal ball mill, a filter-pressing impurity removal device and a magnetic separation device which are sequentially connected; the magnetic separation device comprises a CTN counter-flow type permanent magnet machine and a pulse type high-gradient magnetic separator, one end of the CTN counter-flow type permanent magnet machine is connected with the filter-pressing impurity removal device, and the other end of the CTN counter-flow type permanent magnet machine is connected with the pulse type high-gradient magnetic separator.
Furthermore, the filling balls adopted by the horizontal ball mill are corundum balls or stainless steel balls, and the diameter of the filling balls is one or a combination of more than one of phi 20cm, phi 30cm, phi 40cm and phi 50 cm.
The method for separating the anode and cathode materials of the waste lithium battery has the beneficial effects that: the method comprises the steps of reducing and roasting the anode and cathode materials of the waste lithium batteries to convert metals in the anode materials into forms with stronger magnetism, then dissociating the anode and cathode materials through horizontal wet grinding, removing impurities through filter pressing, preparing to obtain anode and cathode mixed materials, and finally separating and purifying to obtain the cobalt-nickel-manganese composite material and the graphite product with high added values through a two-stage magnetic separation physical separation process. The method has the advantages of high separation rate of the anode and cathode materials, high recovery rate of graphite, high purification degree, simple and convenient process path, low energy consumption and no secondary pollution.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a process flow chart of the method for separating positive and negative electrode materials from waste lithium batteries provided in this embodiment.
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 the accompanying drawings and 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.
In order to explain the technical solution of the present invention, the following detailed description is made with reference to the specific drawings and examples.
The invention provides a method for separating anode and cathode materials of waste lithium batteries, which comprises the following steps:
(1) and (3) reductive roasting: and performing reductive roasting on the positive and negative electrode materials of the waste lithium battery at the temperature of 850-1000 ℃ for 2-5 hours to convert Co and Ni metals in the positive electrode material of the lithium battery into magnetic forms. When the anode and cathode materials are roasted, an ecological activator is added, wherein the ecological activator comprises nano-scale graphite, particle laminar graphite, biological rice hull carbon, refined charcoal, high-purity bamboo charcoal, high-fineness activated carbon and the like, the material granularity is-100 meshes to about 98 percent, and the material granularity is-200 meshes to about 87 percent, the ecological activator can promote the magnetic conversion of the anode materials, meanwhile, the hearth temperature of the roasting furnace can be effectively ensured, the electric energy can be greatly reduced after the temperature in the hearth is stable, and the operation cost is saved. Meanwhile, in order to ensure the reducing atmosphere in the hearth, stable gas is filled at the tail of the furnace, and the stable gas is nitrogen, so that micro-positive pressure is formed in the hearth.
(2) Crushing and grinding: and crushing and grinding the anode and cathode materials subjected to reductive roasting. Adopting a ball mill to carry out horizontal wet grinding, wherein the filling balls of the ball mill are corundum balls or stainless steel balls, and the diameter ranges of the filling balls are phi 20cm, phi 30cm, phi 40cm and phi 50 cm. The horizontal wet grinding of the ball mill can improve the dissociation degree of the anode and cathode materials, and pollution components such as dust and the like are not generated. The discharge concentration of the wet-grinding anode and cathode mixed material is 45-67%, and the grinding ore discharge granularity is 69-86% of-325 mesh.
(3) Filter pressing and impurity removal: filter-pressing and removing impurities from the crushed and ground positive and negative electrode materials, and adding circulating water to prepare a positive and negative electrode mixed material; the concentration of the anode and cathode mixed materials is controlled to be 8% -20%, and the materials in the ore pulp can be well dispersed by adopting high-speed double-paddle stirring.
(4) Magnetic separation: and carrying out magnetic separation twice on the positive and negative electrode mixed materials, and separating and purifying to obtain a cobalt-nickel-manganese product and a graphite product.
The first magnetic separation adopts a CTN counter-flow type permanent magnet machine, the permanent magnet system is an open type magnetic system formed by magnetic materials and a magnetic yoke, the falling of the magnetic materials in the operation process can be effectively prevented, the magnetic field intensity is 2000-5000 Oe, and a part of cobalt-nickel-manganese products are obtained; and conveying the tailings to high-gradient magnetic separation equipment by using a pump for secondary magnetic separation, wherein the magnetic induction intensity of the secondary magnetic separation is 10000 Gs-15000 Gs, a rotating ring of the pulse type high-gradient magnetic separation equipment vertically rotates to recoil concentrate, a built-in pulse mechanism can obtain a high enrichment ratio and is not easy to block, the adaptability to the fluctuation of the feeding granularity, the concentration and the grade is high, a magnetic medium at the lower part of the rotating ring is immersed in the liquid level of the material and moves up and down through a separation chamber, and meanwhile, the pulse fluid force enables the ore particle group to be always kept in a loose state, so that the mechanical inclusion of nonmagnetic particles is eliminated. And the high-gradient strong-magnetic separation concentrate and the permanent-magnetic separation concentrate are combined and enter a concentrate filter pressing system to finally obtain a cobalt-nickel-manganese composite product as a positive electrode material, and the high-gradient strong-magnetic separation tailings enter a tailing filter pressing system to finally obtain a graphite product as a negative electrode material. The separation rate can reach more than 98 percent after the two magnetic separation processes.
Example 1
The embodiment provides a method for separating anode and cathode materials of waste lithium batteries, which comprises the following specific operation steps:
enriching positive and negative electrode materials of waste lithium batteries, adding a certain amount of ecological activating agent, carrying out reduction roasting at the high temperature of 950 ℃ for 3 hours, and conveying the roasted materials into a lifter through automatic tipping equipment and conveying the materials to a high-level stock bin;
crushing and wet-grinding the roasted material, placing alumina corundum balls (wherein phi 40: phi 30: phi 20: 2:5:3) in an overflow cylindrical ball mill, adding an aqueous medium, controlling the concentration of wet-grinding ore pulp to be 35-40% and controlling the discharge particle size to be-325 meshes which is more than or equal to 75%;
after filter pressing and impurity removal, the materials are conveyed to an ore supply barrel by a pump, and filtrate of a filter pressing system is recycled and compounded to control the concentration of the anode and cathode mixed materials to be 8-15%;
and conveying the compounded material to a CTN counter-flow type permanent magnet machine, wherein the magnetic field intensity is 3000Oe, the magnetic material enters a concentrate material barrel, and the non-magnetic material overflows into a buffer tank through a counter-flow port. The flow of the materials in the buffer tank is controlled by a valve to be 4.5m3/h, and the materials enter a pulse type high gradient magnetic separator, and the magnetic induction intensity is 12000 Gs.
Example 2
The embodiment provides a method for separating anode and cathode materials of waste lithium batteries, which refers to the specific operation steps of embodiment 1, and is different from embodiment 1 in that the temperature of reductive roasting is 1000 ℃ and the time is 2 hours; the magnetic field intensity of the first magnetic separation is 2000 Oe; the magnetic induction intensity of the second magnetic separation is 10000 Gs.
Example 3
The embodiment provides a method for separating anode and cathode materials of waste lithium batteries, which refers to the specific operation steps of embodiment 1, and is different from embodiment 1 in that the temperature of reductive roasting is 850 ℃ and the time is 5 hours; the magnetic field intensity of the first magnetic separation is 5000 Oe; the magnetic induction intensity of the second magnetic separation is 15000 Gs.
Comparative example 1
The comparative example provides a method for separating positive and negative electrode materials of waste lithium batteries, which refers to the steps of separating the positive and negative electrode materials in the prior art.
The percent yields and recovery rates for examples 1-3 and comparative example 1 are shown in Table 1:
the results of the particle size analysis of the intermediate product discharged from the on-site ball mill of example 1 are shown in table 2:
TABLE 2 analysis of the particle size of the ball milled discharge intermediate product
| Particle size | Material ratio | Cumulative percentage of |
| +100 mesh | 1％ | 1％ |
| Minus 100 meshes to plus 200 meshes | 8％ | 9％ |
| Minus 200 meshes to plus 325 meshes | 13％ | 17％ |
| 325 mesh | 78％ | 100％ |
The method for separating the anode material and the cathode material of the waste lithium battery provided by the embodiment is implemented through reduction roasting, filter pressing impurity removal, primary permanent magnet and secondary high-gradient pulse strong magnetism, the separation rate of the anode material and the cathode material is not less than 98%, the recovery rate of the anode material is high, the purification degree is high, the process path is simple and convenient, the energy consumption is low, and no secondary pollution is generated.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. It should be noted that there are no specific structures but a few objective structures due to the limited character expressions, and that those skilled in the art may make various improvements, decorations or changes without departing from the principle of the invention or may combine the above technical features in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (10)
1. A method for separating positive and negative electrode materials of waste lithium batteries is characterized by comprising the following steps:
carrying out reductive roasting on the anode and cathode materials of the waste lithium battery;
crushing and grinding the anode and cathode materials subjected to reductive roasting;
carrying out filter pressing on the crushed and ground positive and negative electrode materials to remove impurities so as to obtain a positive and negative electrode mixed material;
and carrying out magnetic separation twice on the positive and negative electrode mixed materials, and separating and purifying to obtain a cobalt-nickel-manganese product and a graphite product.
2. The method for separating the anode and cathode materials of the waste lithium battery as claimed in claim 1, wherein the magnetic field intensity of the first magnetic separation is 2000-5000 Oe, and the magnetic induction intensity of the second magnetic separation is 10000 Gs-15000 Gs.
3. The method for separating the positive and negative electrode materials of the waste lithium battery as claimed in claim 1, wherein the temperature of the reductive calcination is 850-1000 ℃ and the time is 2-5 h.
4. The method for separating the positive and negative electrode materials of the waste lithium batteries as claimed in claim 1, wherein an ecological activator is added during reductive roasting, and the ecological activator is one or more of nano-scale graphite, particle layered graphite, biological rice hull carbon, refined charcoal, high-purity bamboo charcoal and high-fineness activated carbon.
5. The method for separating positive and negative electrode materials of waste lithium batteries according to claim 1, wherein a stabilizing gas is filled at a furnace tail of the roasting furnace during the reductive roasting process.
6. The method for separating positive and negative electrode materials of waste lithium batteries according to claim 5, wherein the stabilizing gas is nitrogen.
7. The method for separating the positive and negative electrode materials of the waste lithium batteries according to claim 1, wherein the positive and negative electrode materials subjected to reductive roasting are crushed and ground in a wet grinding mode; the concentration of the anode and cathode materials during wet grinding is 45-67%.
8. The method for separating positive and negative electrode materials of waste lithium batteries according to claim 1, wherein the concentration of the positive and negative electrode mixture is 8-20%.
9. The device for realizing the method for separating the anode and cathode materials of the waste lithium battery as claimed in any one of claims 1 to 8 is characterized by comprising a roasting furnace, a horizontal ball mill, a filter-pressing impurity removal device and a magnetic separation device which are sequentially connected; the magnetic separation device comprises a CTN counter-flow type permanent magnet machine and a pulse type high-gradient magnetic separator, one end of the CTN counter-flow type permanent magnet machine is connected with the filter-pressing impurity removal device, and the other end of the CTN counter-flow type permanent magnet machine is connected with the pulse type high-gradient magnetic separator.
10. The apparatus of claim 9, wherein the horizontal ball mill uses corundum balls or stainless steel balls with a diameter of 20cm, 30cm, 40cm or 50 cm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112635867A (en) * | 2020-12-29 | 2021-04-09 | 广东省科学院资源综合利用研究所 | Method for recovering waste lithium battery graphite material |
| CN112670614A (en) * | 2020-12-29 | 2021-04-16 | 广东省科学院资源综合利用研究所 | Physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries |
| CN114515651A (en) * | 2022-01-24 | 2022-05-20 | 宜昌邦普循环科技有限公司 | Compound inhibitor and preparation method and application thereof |
| CN115011790A (en) * | 2022-05-31 | 2022-09-06 | 湖南力合厚浦科技有限公司 | Method for recovering nickel, cobalt and manganese, material obtained by recovery and recovery system |
| CN116273445A (en) * | 2023-02-20 | 2023-06-23 | 湖南五创循环科技股份有限公司 | Method for improving separation efficiency of mixed materials of waste lithium manganate batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112635867A (en) * | 2020-12-29 | 2021-04-09 | 广东省科学院资源综合利用研究所 | Method for recovering waste lithium battery graphite material |
| CN112670614A (en) * | 2020-12-29 | 2021-04-16 | 广东省科学院资源综合利用研究所 | Physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries |
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| CN116273445A (en) * | 2023-02-20 | 2023-06-23 | 湖南五创循环科技股份有限公司 | Method for improving separation efficiency of mixed materials of waste lithium manganate batteries |
| CN116273445B (en) * | 2023-02-20 | 2024-02-02 | 湖南五创循环科技股份有限公司 | Method for improving separation efficiency of mixed materials of waste lithium manganate batteries |
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