CN110885072A - Method for efficiently purifying and recovering lithium ion battery anode powder material - Google Patents
Method for efficiently purifying and recovering lithium ion battery anode powder material Download PDFInfo
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- CN110885072A CN110885072A CN201911196784.9A CN201911196784A CN110885072A CN 110885072 A CN110885072 A CN 110885072A CN 201911196784 A CN201911196784 A CN 201911196784A CN 110885072 A CN110885072 A CN 110885072A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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 provides a method for efficiently purifying and recovering a lithium ion battery anode powder material, which comprises the following steps: taking a lithium ion battery positive plate and adding an organic solvent; heating and stirring to separate the dressing from the Al foil; sieving to remove Al foil and aluminum scraps; filtering and drying to obtain powder; and (3) carrying out chemical element analysis test on the powder, and when the weight content of the Al element is more than or equal to 0.3%, sieving the powder by using a higher-mesh sieve and carrying out chemical analysis test again until the weight content of the Al element is less than 0.3%, thus obtaining the high-efficiency purified and recycled lithium ion battery anode powder material. Wherein the positive plate is layered LiMeO2Wherein Me is one or more of Ni, Co and Mn; or the positive plate of the lithium ion battery is LiMePO4Wherein Me is one or more of Fe and Mn. The heating and stirring temperature is 20-200 ℃, and the speed is 10-2000 r/min; the drying temperature is 50-300 ℃, and the drying time is more than or equal to 10 min. The method is favorable for improving the regeneration efficiency of the recycled material, has good repeatability of performance indexes and high resource utilization rate, and has very high social and economic values.
Description
Technical Field
The invention relates to a method for efficiently purifying and recovering a lithium ion battery anode powder material, belonging to the field of waste lithium ion battery recovery and resource recycling.
Background
In recent years, the demand for lithium ion batteries has proliferated in the rapidly growing consumer electronics, electric automobiles, and energy storage markets. According to statistics, the cumulative waste lithium battery in China in 2018 has the GWH of 12.08, and the cumulative scrap amount reaches about 17.25 ten thousand tons. If a common garbage disposal method is adopted, metals such as cobalt, nickel, lithium, manganese and the like, inorganic compounds and organic compounds in the garbage disposal method can cause serious pollution. And the high-price rare metals such as lithium, cobalt, nickel and the like can avoid environmental pollution through effective recovery treatment, can be about a large amount of production cost for battery manufacturers, and has very high economic value.
In addition to the discarded lithium batteries, a large amount of electrode waste generated during the production process cannot be ignored. The electrode waste has its own characteristics compared to used battery materials. For example, the scrap was not assembled into a battery, was not contacted with an electrolyte, and was not subjected to a charge and discharge test. Thus, the active material in the electrode remains intact. The method can be used for recovering the anode powder by considering a simple and green method, can save the complicated traditional recovery process and purification step of acid leaching, and realizes the closed-loop recovery of the waste.
In view of the above-discussed waste batteries and electrode wastes in the production process, the separation and recovery of the cathode powder is the primary step.
The existing separation technology mainly comprises three types:
firstly, crushing and sorting, the method has high efficiency and simple equipment, but has two problems: 1, broken Al scraps are extremely difficult to completely remove through sorting, and 2, the agglomerate cathode material can have the problems of particle cracking, particle size reduction and the like caused by excessive breakage.
Second, acid/base dissolves the Al current collector, which is complete with Al removal, but has two problems: 1, acid/alkali solution is a hazardous chemical substance and causes environmental pollution, 2 Al element dissolved in the solution is extremely difficult to remove, and waste liquid causes secondary pollution.
Thirdly, the method has high efficiency but has three problems: 1, sintering energy loss and time loss, 2, fluoride generated by sintering can damage the material structure, and 3, environmental pollution is caused by using acid-base solution.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for efficiently purifying and recovering the lithium ion battery anode powder material, which is environment-friendly, does not damage the material structure, has simple process, high purity and low energy consumption, and is commercially feasible.
In order to achieve the above technical object, the present invention adopts the following technical means.
A method for efficiently purifying and recovering a lithium ion battery anode powder material comprises the following steps,
s1, taking a lithium ion battery positive plate, and adding an organic solvent into the lithium ion battery positive plate;
s2, heating and stirring to separate the dressing from the Al foil; wherein, the dressing refers to the material on the front sheet except the Al foil.
S3, sieving the mixture by using a 10-30-mesh sieve to remove Al foil, and removing Al scraps by using a 200-400-mesh sieve;
s4, filtering and drying the material/solvent mixture after the Al foil and the Al scraps are removed to obtain powder;
s5, performing chemical analysis test (ICP-AES) on the powder, when the weight content of the Al element is more than or equal to 0.3%, sieving the powder by using a 500-1000-mesh sieve to remove aluminum scraps again, and then performing chemical analysis test (ICP-AES) again until the weight content of the Al element is less than 0.3% to obtain the high-efficiency purified and recycled lithium ion battery anode powder material.
Further, the method for efficiently purifying and recovering the lithium ion battery anode powder material further comprises the step of shearing the lithium ion battery anode plate before adding the organic solvent. Furthermore, the anode material of the lithium ion battery is cut into pieces of 2cm multiplied by 2cm to 10cm multiplied by 10 cm.
Further, in the method for efficiently purifying and recovering the lithium ion battery anode powder material, the lithium ion battery anode plate of S1 is layered LiMeO2Wherein Me is one or more of Ni, Co and Mn; or the positive plate of the lithium ion battery is LiMePO4Wherein Me is one or more of Fe and Mn.
Further, in the method for efficiently purifying and recovering the lithium ion battery cathode powder material, in S1, the organic solvent is one or more of NMP, DMAc, DMF, TEP and DMSO, and preferably NMP.
Further, in the method for efficiently purifying and recovering the lithium ion battery positive electrode powder material, in S1, the dosage of the organic solvent is the amount of completely soaking the ion battery positive electrode sheet.
Further, in the method for efficiently purifying and recovering the lithium ion battery anode powder material of the invention, in S2, the heating temperature is 20-200 ℃, preferably 120-150 ℃, the stirring speed is 10-2000 r/min, preferably 800-1500r/min, and the corresponding separation time is 10-30 min.
Furthermore, the method for efficiently purifying and recovering the lithium ion battery anode powder material has the drying temperature of 50-300 ℃, preferably 180-200 ℃, and the drying time of not less than 10min, preferably 30-120 min.
By adopting the technical scheme, the invention has the following technical effects.
1. The invention provides a purification method of a lithium ion battery anode recycled material, which is beneficial to improving the regeneration efficiency and performance index of the recycled material. The method has the characteristics of good repeatability, high resource utilization rate, simple process, high efficiency and the like, and has very high social and economic values.
2. The method uses a chemical element analysis method (ICP-AES) to measure and strictly control the Al content to achieve the effect of complete separation, thereby avoiding the phenomenon that the content of Al impurities exceeds the standard, and the self-discharge or safety risk is caused by the micro short circuit in the battery when the battery is reused.
Drawings
FIG. 1 is a diagram of a heated stirred separator according to an embodiment of the invention;
FIG. 2 is a graph comparing ICP contents of Al element in materials before and after the high-efficiency purification and recovery of example 1;
FIG. 3 is a comparison of XRD structures of materials before and after efficient purification and recovery in example 2;
FIG. 4 is a comparison graph of ICP content of Al element in the material before and after the material is efficiently purified and recovered in example 3.
Detailed Description
The following further describes the technical solutions of the present invention with reference to specific embodiments, so that those skilled in the art can better understand the present invention and can implement the present invention.
Example 1
A method for efficiently purifying and recovering a lithium ion battery anode powder material comprises the following steps,
s1, taking a lithium ion battery positive plate, and adding an organic solvent into the lithium ion battery positive plate;
500g of LiCoO was weighed using an electronic balance2Shearing the positive plate into a size of 10cm multiplied by 10cm, placing the positive plate in a 5L stirrer, and adding 2000ml of NMP organic solvent to enable the organic solvent to completely soak the positive plate;
s2, heating and stirring to separate the dressing from the Al foil;
in this step, the heating temperature is 120 ℃, the stirring speed is 1000r/min, the separation time is 15min, and the heating stirring separator is shown in FIG. 1.
S3 sieving to remove Al foil and Al filings;
in the step, a 30-mesh screen is used for sieving to remove Al foil, and a 300-mesh screen is used for removing Al scraps;
s4, sieving the material/solvent mixture with the Al foil and Al scraps removed, and drying to obtain powder;
specifically, the mixture is placed in a forced air drying oven, the drying temperature is 180 ℃, and the drying time is 2 hours;
s5, carrying out chemical analysis test (ICP-AES) on the powder, when the weight content of the Al element is more than or equal to 0.3%, sieving the powder by using a 500-mesh sieve, and carrying out chemical analysis test (ICP-AES) again until the weight content of the Al element is less than 0.3%, thus obtaining the lithium ion battery anode powder material which is efficiently purified and recovered.
The results of chemical analysis tests (ICP-AES) performed on the lithium ion battery positive plate and the lithium ion battery positive powder material recovered by efficient purification are shown in fig. 2, and it can be seen that the weight content of Al element in the material is reduced from 21.02% to 0.23% before and after purification recovery, and it can be considered that Al removal is complete.
Example 2
A method for efficiently purifying and recovering a lithium ion battery anode powder material comprises the following steps,
s1, taking a lithium ion battery positive plate, and adding an organic solvent into the lithium ion battery positive plate;
50g of LiNi was weighed with an electronic balance0.5Co0.2Mn0.3O2Shearing the positive plate into 2cm multiplied by 2cm in size, placing the positive plate in a 5L stirrer, and adding 400ml of DMAc organic solvent to enable the organic solvent to completely soak the positive plate;
s2, heating and stirring to separate the dressing from the Al foil;
in this step, the heating temperature is 150 ℃, the stirring speed is 800r/min, the separation time is 10min, and the heating stirring separator is shown in FIG. 1.
S3 sieving to remove Al foil and Al filings;
in the step, a 10-mesh screen is used for sieving to remove Al foil, and a 200-mesh screen is used for removing Al scraps;
s4, filtering and drying the material/solvent mixture after the Al foil and the Al scraps are removed to obtain powder;
specifically, filtering with quick filter paper, and placing in an air-blast drying oven at a drying temperature of 200 ℃ for 0.5 h;
s5, carrying out chemical analysis test (ICP-AES) on the powder, when the weight content of the Al element is more than or equal to 0.3%, sieving the powder by using a 800-mesh sieve, and carrying out chemical analysis test (ICP-AES) again until the weight content of the Al element is less than 0.3%, thus obtaining the lithium ion battery anode powder material which is efficiently purified and recovered.
And performing chemical element analysis test (ICP-AES) on the obtained high-efficiency purified and recycled lithium ion battery anode powder material, wherein the weight content of Al element is 0.15%. The positive plate of the lithium ion battery and the high-efficiency purified and recycled positive powder material of the lithium ion battery are analyzed by an X-ray diffractometer, and the obtained result is shown in figure 3, so that the crystal phase of the material is not changed before and after purification and recycling.
Example 3
A method for efficiently purifying and recovering a lithium ion battery anode powder material comprises the following steps,
s1, taking a lithium ion battery positive plate, and adding an organic solvent into the lithium ion battery positive plate;
2000g LiFePO were weighed out with an electronic balance4Shearing the positive plate into a size of 10cm multiplied by 10cm, placing the positive plate in a 5L stirrer, and adding 3000ml of DMF organic solvent to enable the organic solvent to completely soak the positive plate;
s2, heating and stirring to separate the dressing from the Al foil;
in the step, the heating temperature is 80 ℃, the stirring speed is 1500r/min, the separation time is 15min, and the heating stirring separator is shown in figure 1.
S3 sieving to remove Al foil and Al filings;
in the step, a 30-mesh screen is screened to remove Al foil, and a 400-mesh screen is used to remove Al scraps;
s4, filtering and drying the material/solvent mixture after the Al foil and the Al scraps are removed to obtain powder;
specifically, filtering with quick filter paper, and placing in an air-blast drying oven at a drying temperature of 200 ℃ for 0.5 h;
and (3) carrying out chemical analysis test (ICP-AES) on the powder, sieving the powder by using a 1000-mesh sieve when the weight content of the Al element is more than or equal to 0.3%, and carrying out chemical analysis test (ICP-AES) again until the weight content of the Al element is less than 0.3%, thus obtaining the lithium ion battery anode powder material which is efficiently purified and recycled.
The results of chemical analysis tests (ICP-AES) performed on the lithium ion battery positive plate and the lithium ion battery positive powder material recovered by efficient purification are shown in fig. 4, and it can be seen that the weight content of Al element in the material is reduced from 14.30% to 0.12% before and after purification recovery, and it can be considered that Al removal is complete.
The technical solution provided by the present invention is not limited by the above embodiments, and all technical solutions formed by utilizing the structure and the mode of the present invention through conversion and substitution are within the protection scope of the present invention.
Claims (10)
1. A method for efficiently purifying and recovering a lithium ion battery anode powder material is characterized by comprising the following steps:
s1, taking a lithium ion battery positive plate, and adding an organic solvent into the lithium ion battery positive plate;
s2, heating and stirring to separate the dressing from the Al foil;
s3 sieving to remove aluminum foil and aluminum scraps;
s4, filtering and drying the material/solvent mixture after the Al foil and the Al scraps are removed to obtain powder;
and S5, carrying out chemical analysis test on the powder, when the weight content of the Al element is more than or equal to 0.3%, sieving the powder by using a sieve with a mesh number larger than that of S3 to remove aluminum skimmings again, and then carrying out chemical analysis test again (until the weight content of the Al element is less than 0.3%), thus obtaining the high-efficiency purified and recycled lithium ion battery anode powder material.
2. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: s1, before adding the organic solvent, the method also comprises the process of shearing the lithium ion battery positive plate.
3. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 2, characterized in that: s1 cutting the anode material of the lithium ion battery into pieces of 2cm multiplied by 2cm to 10cm multiplied by 10cm before adding the organic solvent.
4. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: the lithium ion battery positive plate of S1 is a layered LiMeO2Wherein Me is one or more of Ni, Co and Mn;
or the positive plate of the lithium ion battery is LiMePO4Wherein Me is one or more of Fe and Mn.
5. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: in S1, the organic solvent is one or more of NMP, DMAc, DMF, TEP and DMSO.
6. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: in S1, the dosage of the organic solvent is to completely soak the positive plate of the ion battery.
7. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: in S2, the heating temperature is 20-200 ℃, the stirring speed is 10-2000 r/min, and the corresponding separation time is 10-30 min.
8. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: the drying temperature in S4 is 50-300 ℃, and the drying time is more than or equal to 10 min.
9. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: in S3, Al foil is removed by sieving with a 10-30 mesh sieve, and Al scrap is removed by sieving with a 200-400 mesh sieve.
10. The method for efficiently purifying and recycling the lithium ion battery cathode powder material according to claim 1, characterized in that: the mesh number in S5 is larger than that in S3, and the mesh number is 500-1000 meshes.
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Cited By (3)
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| CN112467241A (en) * | 2020-11-12 | 2021-03-09 | 郑州中科新兴产业技术研究院 | Short-process recycling method for ternary cathode material, recycled material and application |
| US20220200074A1 (en) * | 2020-12-17 | 2022-06-23 | Ut-Battelle, Llc | Recovery of materials from electrode scraps and spent lithium-ion batteries via a green solvent-based separation process |
| US20230033430A1 (en) * | 2021-07-28 | 2023-02-02 | Ut-Battelle, Llc | Direct recycling of lithium-ion battery scraps for manufacturing a new anode |
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Application publication date: 20200317 |