CN113955812B - Recovery processing method for ternary positive electrode material crushed dust collection material - Google Patents

Recovery processing method for ternary positive electrode material crushed dust collection material Download PDF

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CN113955812B
CN113955812B CN202111159046.4A CN202111159046A CN113955812B CN 113955812 B CN113955812 B CN 113955812B CN 202111159046 A CN202111159046 A CN 202111159046A CN 113955812 B CN113955812 B CN 113955812B
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ternary
positive electrode
dust collection
electrode material
crushed dust
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CN113955812A (en
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徐成
孙杰
林硕
梅京
何雅
周宇
赵亚清
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Hubei Rongtong High Tech Advanced Materials Group Co ltd
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    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C01P2006/40—Electric properties
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to the technical field of recovery of dust collection materials of ternary nickel cobalt lithium manganate materials, and discloses a recovery treatment method of crushed dust collection materials of ternary positive electrode materials, which comprises the following steps: (1) Mixing the ternary positive electrode material crushed dust collection material with a lithium source to obtain a mixture; (2) Sintering the mixture obtained in the step (1) under an oxygen-containing atmosphere to obtain a sintered material, and sequentially crushing, grading and sieving the sintered material to obtain a ternary positive electrode material crushed dust collection material treatment material; (3) And (3) mixing the ternary cathode material crushed dust collection material treatment material obtained in the step (2) with the monocrystal ternary cathode material. According to the invention, the ternary positive electrode material crushed dust collection material is recycled, so that the production cost is reduced, and the discharge capacity and other performances of the obtained ternary positive electrode material are basically consistent with those of the normal ternary positive electrode material.

Description

Recovery processing method for ternary positive electrode material crushed dust collection material
Technical Field
The invention relates to the technical field of recovery of a dust collection material of a ternary nickel cobalt lithium manganate material, in particular to a recovery treatment method of a crushed dust collection material of a ternary positive electrode material.
Background
The lithium ion battery has the advantages of high voltage, large specific energy, long cycle life, stable working voltage, small self-discharge and the like, and is considered as one of batteries with development potential. The positive electrode material is an important component of the lithium ion battery, and the cost of the positive electrode material accounts for 40% -50% of the cost of the whole battery.
The cost reduction of the cathode material factory is not started from the cost reduction of raw materials and the process optimization. The final purpose of process optimization is to improve the product yield. The generation of dust collection materials is unavoidable in the anode material factories, and the yield of the dust collection materials is 0.5% -2% different in each factory due to different production processes. The dust collection material is always a troublesome problem for each positive electrode material factory due to the problems of small particle size, poor electrical property and the like.
In order to improve the product yield and recycle the dust-collecting material, a new dust-collecting material recycling method is urgently needed.
Disclosure of Invention
The invention aims to solve the problems of high production cost and difficult treatment of generated dust collection materials in the production process of ternary positive electrode materials in the prior art, and provides a recovery treatment method for the crushed dust collection materials of the ternary positive electrode materials.
In order to achieve the above object, the present invention provides a recovery processing method of a ternary positive electrode material crushed dust collection material, the method comprising the steps of:
(1) Mixing the ternary positive electrode material crushed dust collection material with a lithium source to obtain a mixture;
(2) Sintering the mixture obtained in the step (1) under an oxygen-containing atmosphere to obtain a sintered material, and sequentially crushing, grading and sieving the sintered material to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi x Co y Mn z O 2 Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x+y+z=1;
(3) Mixing the ternary cathode material crushed dust collection material treatment material obtained in the step (2) with ternary monocrystal cathode material;
wherein, the chemical formula of the ternary positive electrode material smashing dust collection material is as follows: liNi x Co y Mn z O 2 ，0≤x≤1，0≤y≤1，0≤z≤1，x+y+z＝1；
In the step (1), the ratio of the amount of the lithium element in the lithium source to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is (0.5-1): 1, a step of;
in the step (2), the specific sintering process is as follows: heating to 400-550 ℃ at a heating rate of 2-7 ℃/min for calcination for 4-8h, and continuously heating to 700-900 ℃ at a heating rate of 1-3 ℃/min for calcination for 8-14h; the flow rate of the sintering gas is 1-5m 3 /h。
Preferably, in the step (1), the ternary positive electrode material crushed dust collection material is ternary polycrystalline positive electrode material crushed dust collection material and/or ternary single crystal positive electrode material crushed dust collection material.
Preferably, in step (1), the lithium source is at least one of lithium phosphate, lithium hydroxide, and lithium carbonate.
Further preferably, the lithium source is lithium carbonate.
Preferably, in step (1), the lithium source has a D50 of 3-8 μm.
Preferably, in the step (1), dmin of the ternary positive electrode material crushed dust collection material is 0.1-2 μm, D50 is 1-7 μm, and Dmax is 5-30 μm.
Preferably, in step (2), the oxygen-containing atmosphere is oxygen and/or air.
Further preferably, the oxygen-containing atmosphere is air.
Preferably, in step (2), the frequency of comminution is 5-15Hz.
Preferably, in step (2), the frequency of the classification is 2-8Hz.
Preferably, in the step (2), the particle size of the crushed dust collection material treated material of the ternary positive electrode material obtained after sieving is less than 5 mu m.
Preferably, in the step (3), the molar ratio of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material treatment material is the same as the molar ratio of nickel, cobalt and manganese in the ternary single crystal positive electrode material;
further preferably, the weight ratio of the ternary positive electrode material crushed dust collection material treatment material to the ternary single crystal positive electrode material is (0.01-0.1): 1.
according to the method disclosed by the invention, the crushed dust collection material of the ternary positive electrode material is recycled, so that the ternary positive electrode material is obtained again, the production cost is reduced, and the discharge capacity and the circulation capacity retention rate of the obtained ternary positive electrode material are basically consistent with those of a normal ternary positive electrode material, and the shape of an electron microscope is good.
Drawings
FIG. 1 is a conventional ternary single crystal positive electrode material LiNi used in step (3) of example 1 0.5 Co 0.2 Mn 0.3 O 2 Scanning electron microscope images of (2);
FIG. 2 is a scanning electron microscope image of the product A1 obtained in example 1.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a recovery processing method of ternary positive electrode material crushed dust collection materials, which comprises the following steps:
(1) Mixing the ternary positive electrode material crushed dust collection material with a lithium source to obtain a mixture;
(2) Sintering the mixture obtained in the step (1) under an oxygen-containing atmosphere to obtain a sintered material, and sequentially crushing, grading and sieving the sintered material to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi x Co y Mn z O 2 Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x+y+z=1;
(3) Mixing the ternary cathode material crushed dust collection material treatment material obtained in the step (2) with ternary monocrystal cathode material;
wherein, the chemical formula of the ternary positive electrode material smashing dust collection material is as follows: liNi x Co y Mn z O 2 ，0≤x≤1，0≤y≤1，0≤z≤1，x+y+z＝1；
In the step (1), the ratio of the amount of the lithium element in the lithium source to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is (0.5-1): 1, a step of;
in the step (2), the specific sintering process is as follows: heating to 400-550 ℃ at a heating rate of 2-7 ℃/min for calcination for 4-8h, and continuously heating to 700-900 ℃ at a heating rate of 1-3 ℃/min for calcination for 8-14h; the flow rate of the sintering gas is 1-5m 3 /h。
In the invention, after the ternary positive electrode material is crushed, qualified materials with granularity and fine dust are generated, wherein the fine dust is the crushed dust collection material of the ternary positive electrode material.
In the invention, the ternary positive electrode material crushing dust collection material is obtained by collecting dust collection systems by equipment such as a mechanical mill, an air flow mill, a pair roller machine, a jaw crusher, a rotary wheel mill and the like.
In the invention, in the step (1), the ternary positive electrode material crushed dust collection material is ternary polycrystalline positive electrode material crushed dust collection material and/or ternary single crystal positive electrode material crushed dust collection material.
In the invention, the chemical formula of the ternary positive electrode material crushed dust collection material can be LiNi 0.83 Co 0.12 Mn 0.05 O 2 、LiNi 0.8 Co 0.1 Mn 0.1 O 2 、LiNi 0.6 Co 0.2 Mn 0.2 O 2 、LiNi 0.55 Co 0.15 Mn 0.3 O 2 Or LiNi 0.5 Co 0.2 Mn 0.3 O 2 Etc.
In the present invention, in step (1), the lithium source may be a conventional choice in the art, and preferably, the lithium source is at least one of lithium phosphate, lithium hydroxide, and lithium carbonate.
In order to save raw material costs, in a preferred embodiment, in step (1), the lithium source is lithium carbonate.
In a preferred embodiment, in step (1), the lithium source has a D50 of 3-8 μm. Specifically, in step (1), the D50 of the lithium source may be 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm or 8 μm. Further preferably, the lithium source has a D50 of 5 μm.
In a preferred embodiment, in step (1), dmin of the ternary positive electrode material crushed dust collection material is 0.1-2 μm, D50 is 1-7 μm, and Dmax is 5-30 μm. Specifically, in the step (1), dmin of the ternary positive electrode material pulverized dust collection material may be 0.1 μm, 0.3 μm, 0.5 μm, 0.7 μm, 1 μm, 1.1 μm, 1.3 μm, 1.5 μm, 1.7 μm or 2 μm, D50 may be 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, 5.5 μm, 6 μm, 6.5 μm or 7 μm, dmax may be 5 μm, 7 μm, 9 μm, 11 μm, 13 μm, 15 μm, 17 μm, 19 μm, 20 μm, 23 μm, 25 μm, 27 μm, 29 μm or 30 μm.
In order to effectively treat the ternary material dust collection material, the proportion between the ternary positive electrode material crushing dust collection material and the lithium source in the step (1) needs to be reasonably controlled. In a specific embodiment, in the step (1), the ratio of the amount of the substance of the lithium element in the lithium source to the total amount of the three elements of nickel, cobalt and manganese in the crushed dust collection material of the ternary cathode material may be 0.5:1. 0.55: 1. 0.6: 1. 0.65: 1. 0.7: 1. 0.75: 1. 0.8: 1. 0.85: 1. 0.9: 1. 0.95:1 or 1:1. preferably, the ratio of the amount of the substance of the lithium element in the lithium source to the total amount of the three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.5:1.
in the present invention, in step (1), the equipment used for the mixing operation may be a conventional choice in the art. Preferably, in step (1), the mixing operation is performed in a high-speed mixer.
In the present invention, in step (2), the oxygen-containing atmosphere is oxygen and/or air. In order to improve the sintering effect, preferably, the oxygen-containing atmosphere is air.
In order to control the uniformity of the oxygen-containing atmosphere during sintering, in step (2), the flow rate of the sintering gas is controlled to be 1-5m 3 And/h. In particular, the sintering gas flow rate may be 1m 3 /h、1.5m 3 /h、2m 3 /h、2.5m 3 /h、3m 3 /h、3.5m 3 /h、4m 3 /h、4.5m 3 /h or 5m 3 And/h. Preferably, the sintering gas flow is 2-4m 3 /h。
In the invention, in the step (2), in order to ensure the electrochemical performance of the material after the ternary positive electrode material is recovered and the dust collection material is crushed, a two-step gradient sintering process is adopted, and the specific process of sintering is as follows: calcining for 4-8h at a temperature rising rate of 2-7deg.C/min to 400-550deg.C, specifically, the temperature rising rate may be 2deg.C/min, 2.5deg.C/min, 3 deg.C/min, 3.5deg.C/min, 4 deg.C/min, 4.5deg.C/min, 5 deg.C/min, 5.5 deg.C/min, 6 deg.C/min, 6.5 deg.C/min or 7 deg.C/min, the calcining temperature may be 400deg.C, 410 deg.C, 420 deg.C, 430 deg.C, 440 deg.C, 450 deg.C, 470 deg.C, 480 deg.C, 490 deg.C, 500 deg.C, 510 deg.C, 520 deg.C, 530 deg.C or 550deg.C, the calcination time may be 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours or 8 hours, the calcination is continued to be performed at a temperature rising speed of 1-3 ℃/min to 700-900 ℃ for 8-14 hours, specifically, the temperature rising speed may be 1 ℃/min, 1.5 ℃/min, 2 ℃/min, 2.5 ℃/min or 3 ℃/min, the calcination temperature may be 700 ℃, 725 ℃, 750 ℃, 775 ℃, 800 ℃, 825 ℃, 850 ℃, 875 ℃, or 900 ℃, and the calcination time may be 8 hours, 8.5 hours, 9 hours, 9.5 hours, 10 hours, 10.5 hours, 11 hours, 11.5 hours, 12 hours, 12.5 hours, 13.5 hours or 14 hours.
In the present invention, the equipment used for the sintering operation may be a conventional choice in the art, preferably the sintering operation is performed in a sintering furnace.
In the present invention, in the step (2), the pulverization may be mechanical pulverization or jet pulverization. Preferably, the comminution is mechanical comminution.
In a preferred embodiment, in step (2), the frequency of comminution is in the range of 5-15Hz. In particular, the frequency of comminution may be 5Hz, 6Hz, 7Hz, 8Hz, 9Hz, 10Hz, 11Hz, 12Hz, 13Hz, 14Hz or 15Hz.
In a preferred embodiment, in step (2), the frequency of the fractionation is 2-8Hz. In particular, the frequency of the classification may be 2Hz, 3Hz, 4Hz, 5Hz, 6Hz, 7Hz or 8Hz.
In the invention, in the step (2), the sintered product is crushed and graded and then is screened by sieving to obtain a product with proper particle size, and preferably, the particle size of the crushed dust collection material treated material of the ternary positive electrode material obtained after sieving is less than 5 mu m.
In the present invention, in the step (3), the chemical formula of the ternary single crystal positive electrode material is: liNi x Co y Mn z O 2 ，0≤x≤1，0≤y≤1，0≤z≤1，x+y+z＝1。
In the invention, in the step (3), the molar ratio of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material treatment material is the same as the molar ratio of nickel, cobalt and manganese in the ternary single crystal positive electrode material.
In the preferred case, in the step (3), the weight ratio of the ternary positive electrode material pulverized dust collection material treated material to the ternary single crystal positive electrode material is (0.01-0.1): 1. specifically, the weight ratio of the ternary positive electrode material crushed dust collection material treatment material to the monocrystal ternary positive electrode material can be 0.01: 1. 0.015: 1. 0.02: 1. 0.025: 1. 0.03: 1. 0.035: 1. 0.04: 1. 0.045: 1. 0.05: 1. 0.055: 1. 0.06: 1. 0.065: 1. 0.07: 1. 0.075: 1. 0.08: 1. 0.085: 1. 0.09: 1. 0.095:1 or 0.1:1.
according to the invention, conventional dry mixing is adopted, the ternary positive material dust collection material and the lithium source are mixed, the requirement on ternary material recovery material is reduced, lithium carbonate with lower price can be adopted for the lithium source to obtain uniform materials, in addition, the materials can be uniformly mixed by the dry mixing, the lithium source is uniformly coated or permeated into the dust collection material to reach the uniformity of an atomic level, then the obtained uniformly mixed materials are placed into a sintering furnace for sintering by a two-step gradient sintering process, the temperature and the oxygen-containing atmosphere uniformity are controlled in the sintering process, and meanwhile, the primary particle regrowth of the dust collection material is facilitated by sintering, so that the original electrical property of the dust collection material is maintained; and then mechanically crushing, classifying and screening the material obtained by sintering to obtain a ternary material subjected to primary treatment, and finally mixing the ternary material with a conventional monocrystal ternary positive electrode material to achieve the aim of recycling treatment.
The present invention will be described in detail by way of examples, but the method of the present invention is not limited thereto.
Examples 1-10, and comparative examples 1-3 all used ternary positive electrode material crushed dust collection materials were ternary 523 positive electrode material crushed dust collection materials. Examples and comparative examples conventional ternary monocrystalline cathode material LiNi used in step (3) 0.5 Co 0.2 Mn 0.3 O 2 All of the materials are from self-production, the product number is SC60, and the crushed dust collection materials of the ternary monocrystal anode materials used in the examples are the same.
Example 1
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.5 Co 0.2 Mn 0.3 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 30.2kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.5:1, obtaining a mixture;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 10 Hz), then grading (the grading frequency is 6 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The particle size of the crushed dust collection material treatment material of the ternary positive electrode material is less than 5 mu m;
(3) 20kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, ternary positive electrode materialThe weight ratio of the crushed dust collection material treatment material to the ternary monocrystal anode material is 0.01:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A1；
In the step (2), the specific sintering process is as follows: heating to 400 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 880 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3m 3 /h。
Example 2
In contrast to the method of example 1, in step (3), 40kg of the ternary cathode material pulverized dust collection material treatment material was mixed with 2000kg of ternary single crystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.02:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A2。
Example 3
In contrast to the method of example 1, in step (3), 60kg of the ternary cathode material pulverized dust-collecting material treated material and 2000kg of the ternary single-crystal cathode material LiNi were subjected to the method of example 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.03:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A3。
Example 4
In contrast to the method of example 1, in step (3), 100kg of the ternary cathode material pulverized dust-collecting material treated material and 2000kg of ternary single-crystal cathode material LiNi were subjected to the method of example 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A4。
Example 5
In contrast to the method of example 1, in step (3), 120kg of the ternary cathode material pulverized dust-collecting material treated material and 2000kg of ternary single-crystal cathode material LiNi were subjected to the method of example 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary monocrystal positive electrode material is 0.06:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A5。
Example 6
In contrast to the method of example 1, in step (3), 140kg of the ternary cathode material pulverized dust-collecting material treated material and 2000kg of the ternary single-crystal cathode material LiNi were subjected to the method of example 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.07:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A6。
Example 7
The process was carried out as in example 1, except that 36.5kg of lithium carbonate and 160kg of ternary single crystal positive electrode material were pulverized to collect dust material LiNi in step (1) 0.5 Co 0.2 Mn 0.3 O 2 Mixing, namely, the ratio of the amount of lithium element substances in lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.6:1, and recovering to obtain a ternary single crystal positive electrode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A7。
Example 8
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.5 Co 0.2 Mn 0.3 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 36.5kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the crushed dust collecting material of the ternary positive electrode material is 0.6:1, obtain a mixtureMixing materials;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 10 Hz), then grading (the grading frequency is 6 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The particle size of the crushed dust collection material treatment material of the ternary positive electrode material is less than 5 mu m;
(3) 100kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A8；
In the step (2), the specific sintering process is as follows: heating to 400 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 880 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3m 3 /h。
Example 9
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.5 Co 0.2 Mn 0.3 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 42.5kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the crushed dust collection material of the ternary positive electrode material is 0.7:1, obtaining a mixture;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 10 Hz), then grading (the grading frequency is 6 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Crushing ternary positive electrode materialThe particle size of the dust collection material treatment material is less than 5 mu m;
(3) 100kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A9；
In the step (2), the specific sintering process is as follows: heating to 400 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 880 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3m 3 /h。
Example 10
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.5 Co 0.2 Mn 0.3 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 48.5kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.8:1, obtaining a mixture;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 10 Hz), then grading (the grading frequency is 6 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The particle size of the crushed dust collection material treatment material of the ternary positive electrode material is less than 5 mu m;
(3) 100kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）A10；
In the step (2), the specific sintering process is as follows: heating to 400 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 880 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3m 3 /h。
Comparative example 1
The process was carried out as in example 1, except that in step (1), 160kg of ternary single crystal positive electrode material pulverized dust collection material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing with 18.1kg of lithium carbonate, namely, the ratio of the mass of lithium element in the lithium carbonate to the total mass of three elements of nickel, cobalt and manganese in the crushed dust collection material of the ternary positive electrode material is 0.3:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）D1。
Comparative example 2
The process was carried out as in example 1, except that in step (1), 160kg of ternary single crystal positive electrode material pulverized dust collection material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing with 90.9kg of lithium carbonate, namely, the ratio of the mass of lithium element in the lithium carbonate to the total mass of three elements of nickel, cobalt and manganese in the crushed dust collection material of the ternary positive electrode material is 1.5:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）D2。
Comparative example 3
The process was carried out as in example 1, except that in step (3), 400kg of the ternary cathode material dust collecting material treated material was mixed with 2000kg of the ternary single crystal cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.2:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.5 Co 0.2 Mn 0.3 O 2 ）D3。
Test example 1
Using a scanning electron microscope pair A1 and the method used in step (3) of example 1Conventional ternary monocrystalline cathode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The detection is carried out, a scanning electron microscope image of the conventional ternary single crystal positive electrode material is shown in fig. 1, an A1 scanning electron microscope image is shown in fig. 2, and the situation that the morphology of the A1 material particles obtained after the conventional ternary single crystal positive electrode material is mixed with the ternary positive electrode material dust collecting material is not changed obviously can be seen from fig. 1 and 2.
Test example 2
Pulverizing the ternary monocrystal positive electrode material in the steps A1-A10, D1-D3 and the step (1) of the embodiment 1 to obtain dust collection material LiNi 0.5 Co 0.2 Mn 0.3 O 2 And conventional ternary single crystal cathode material LiNi used in step (3) of example 1 0.5 Co 0.2 Mn 0.3 O 2 As the positive electrode, a CR2025 type coin cell was prepared using a lithium sheet as the negative electrode, and tested for a 0.1C first discharge capacity in a voltage range of 3.0 to 4.3V, and also tested for a capacity retention rate after 100 cycles at a 1C discharge rate and a 1C first discharge capacity, and test results are shown in table 1.
TABLE 1
From table 1, the effect of the primary discharge capacity of 0.1C is not great, and the primary discharge capacity of 1C tends to decrease, as the ratio of the amount of lithium element in the lithium source to the total amount of nickel, cobalt and manganese elements in the crushed dust collection material of the ternary cathode material increases gradually within a certain range; with the increase of the weight ratio of the ternary positive electrode material crushed dust collection material treatment material to the conventional ternary single crystal positive electrode material, the initial discharge capacity of 0.1C, the initial discharge capacity of 1C and the capacity retention rate of 100 circles of 1C are obviously reduced, the ratio of the amount of lithium element substances in a lithium source to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.5:1, and when the weight ratio of the ternary positive electrode material crushed dust collection material treatment material to the conventional ternary single crystal positive electrode material is 0.05:1, the ternary positive electrode material crushed dust collection material treatment material can be furthest utilized on the premise of ensuring the electrochemical performance of a product, and the comprehensive treatment benefit and the product performance are optimal;
the primary discharge capacity of the product obtained by the method is more than 172mA/h at 0.1C, more than 152.5mA/h at 1C, and the capacity retention rate of the product in 100 circles of 1C circulation is more than 93 percent.
The ternary positive electrode material crushed dust collection materials used in examples 11-13 are ternary 622 positive electrode material crushed dust collection materials. Examples 11-13 conventional ternary monocrystalline cathode material LiNi used in step (3) 0.6 Co 0.2 Mn 0.2 O 2 All of the materials are from self-production, the product number is SC70, and the crushed dust collection materials of the ternary monocrystal anode materials used in the examples are the same.
Example 11
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.6 Co 0.2 Mn 0.2 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 30.4kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.5:1, obtaining a mixture;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 8 Hz), then grading (the grading frequency is 5 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.6 Co 0.2 Mn 0.2 O 2 The particle size of the crushed dust collection material treatment material of the ternary positive electrode material is less than 5 mu m;
(3) 20kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.6 Co 0.2 Mn 0.2 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary monocrystal positive electrode material is 0.01:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.6 Co 0.2 Mn 0.2 O 2 ）A11；
In the step (2), the specific sintering process is as follows: heating to 500 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 900 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3.5m 3 /h。
Example 12
The process was carried out in accordance with example 11, except that in step (3), 100kg of the ternary positive electrode material dust collecting material treated material was mixed with 2000kg of the ternary single crystal positive electrode material LiNi 0.6 Co 0.2 Mn 0.2 O 2 Mixing, wherein the weight ratio of the ternary positive electrode material grinding dust collection material treatment material to the ternary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.6 Co 0.2 Mn 0.2 O 2 ）A12。
Example 13
(1) 160kg of ternary monocrystal anode material is crushed to collect dust material LiNi 0.6 Co 0.2 Mn 0.2 O 2 (D50 is 3 μm, dmin is 0.2 μm, dmax is 15 μm) and 48.9kg of lithium carbonate (D50 is 5 μm) are mixed in a high-speed mixer, and the ratio of the amount of lithium element in the lithium carbonate to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is 0.8:1, obtaining a mixture;
(2) Placing the mixture obtained in the step (1) in a sintering furnace, sintering in air to obtain a sintered material, placing the sintered material in a mechanical mill for mechanical crushing (the crushing frequency is 8 Hz), then grading (the grading frequency is 5 Hz), and then sieving with a 325-mesh sieve to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi 0.6 Co 0.2 Mn 0.2 O 2 The particle size of the crushed dust collection material treatment material of the ternary positive electrode material is less than 5 mu m;
(3) 100kg of the ternary cathode material crushed dust collection material treatment material obtained in the step (2) and 2000kg of ternary monocrystal cathode material LiNi 0.6 Co 0.2 Mn 0.2 O 2 Mixing, crushing ternary positive electrode material, dust collecting material treatment material and ternary positive electrode materialThe weight ratio of the primary single crystal positive electrode material is 0.05:1, recovering to obtain ternary monocrystalline cathode material (LiNi 0.6 Co 0.2 Mn 0.2 O 2 ）A13；
In the step (2), the specific sintering process is as follows: heating to 500 ℃ at a heating rate of 5 ℃/min for calcination for 5 hours, and continuously heating to 900 ℃ at a heating rate of 2 ℃/min for calcination for 10 hours; sintering gas (air) flow rate of 3.5m 3 /h。
Test example 3
Pulverizing the ternary monocrystal positive electrode material in the steps (1) of A11-A13 and example 11 respectively to obtain dust collection material LiNi 0.6 Co 0.2 Mn 0.2 O 2 And conventional ternary single crystal cathode material LiNi used in step (3) of example 11 0.6 Co 0.2 Mn 0.2 O 2 As the positive electrode, a CR2025 type coin cell was prepared using a lithium sheet as the negative electrode, and tested for a 0.1C first discharge capacity in a voltage range of 3.0 to 4.3V, and also tested for a capacity retention rate after 100 cycles at a 1C discharge rate and a 1C first discharge capacity, and test results are shown in table 2.
TABLE 2
As can be seen from the results of table 2, the electrochemical performance of the ternary positive electrode material obtained by crushing the ternary positive electrode material and recycling the dust collecting material by adopting the method of the invention is basically consistent with that of the conventional ternary positive electrode material.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (11)

1. The recovery processing method of the ternary positive electrode material crushed dust collection material is characterized by comprising the following steps of:
(1) Mixing the ternary positive electrode material crushed dust collection material with a lithium source to obtain a mixture;
(2) Sintering the mixture obtained in the step (1) under an oxygen-containing atmosphere to obtain a sintered material, and sequentially crushing, grading and sieving the sintered material to obtain a ternary positive electrode material crushed dust collection material treatment material LiNi x Co y Mn z O 2 Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x+y+z=1;
(3) Mixing the ternary cathode material crushed dust collection material treatment material obtained in the step (2) with ternary monocrystal cathode material;
wherein, the chemical formula of the ternary positive electrode material smashing dust collection material is as follows: liNi x Co y Mn z O 2 ，0≤x≤1，0≤y≤1，0≤z≤1，x+y+z＝1；
In the step (1), the ratio of the amount of the lithium element in the lithium source to the total amount of three elements of nickel, cobalt and manganese in the ternary positive electrode material crushed dust collection material is (0.5-1): 1, a step of;
in the step (2), the specific sintering process is as follows: heating to 400-550 ℃ at a heating rate of 2-7 ℃/min for calcination for 4-8h, and continuously heating to 700-900 ℃ at a heating rate of 1-3 ℃/min for calcination for 8-14h; the flow rate of the sintering gas is 1-5m 3 /h；
In the step (3), the weight ratio of the ternary positive electrode material crushed dust collection material treatment material to the ternary single crystal positive electrode material is (0.01-0.1): 1, a step of;
in the step (3), the molar ratio of nickel, cobalt and manganese in the ternary positive electrode material crushing and dust collecting material treatment material is the same as the molar ratio of nickel, cobalt and manganese in the ternary single crystal positive electrode material.
2. The method of claim 1, wherein in step (1), the ternary positive electrode material crushed dust collection material is ternary polycrystalline positive electrode material crushed dust collection material and/or ternary monocrystalline positive electrode material crushed dust collection material.
3. The method of claim 1, wherein in step (1), the lithium source is at least one of lithium phosphate, lithium hydroxide, and lithium carbonate.
4. A method according to claim 3, wherein in step (1) the lithium source is lithium carbonate.
5. A method according to claim 1 or 3, wherein in step (1) the D50 of the lithium source is 3-8 μm.
6. The method according to claim 1 or 2, wherein in step (1), dmin of the ternary positive electrode material crushed dust collection material is 0.1 to 2 μm, D50 is 1 to 7 μm, dmax is 5 to 30 μm.
7. The method according to claim 1, wherein in step (2), the oxygen-containing atmosphere is oxygen and/or air.
8. The method of claim 7, wherein in step (2), the oxygen-containing atmosphere is air.
9. The method according to claim 1, wherein in step (2), the frequency of pulverization is 5-15Hz.
10. The method of claim 1, wherein in step (2), the frequency of the classification is 2-8Hz.
11. The method according to claim 1, wherein in the step (2), the particle size of the crushed dust collecting material treated material of the ternary cathode material obtained after sieving is less than 5 μm.
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