CN113200541A - Method for recycling graphite negative electrode of waste battery - Google Patents

Method for recycling graphite negative electrode of waste battery Download PDF

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Publication number
CN113200541A
CN113200541A CN202110330381.XA CN202110330381A CN113200541A CN 113200541 A CN113200541 A CN 113200541A CN 202110330381 A CN202110330381 A CN 202110330381A CN 113200541 A CN113200541 A CN 113200541A
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China
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graphite
negative plate
waste
lithium ion
recycling
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CN202110330381.XA
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Chinese (zh)
Inventor
欧星
萧厚桂
龚海强
张佳峰
张宝
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Central South University
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Central South University
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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
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/21—After-treatment
    • C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M2004/027—Negative 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • 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

A method for recycling a graphite cathode of a waste battery. The invention comprises the following steps: (1) discharging, disassembling, manually cutting or mechanically crushing the waste lithium ion battery to obtain a negative plate; (2) mixing the negative plate obtained in the step (1) with salt which is hydrolyzed to be acidic and has strong oxidizing property, and soaking until copper in the negative plate is completely dissolved; (3) filtering the solution containing graphite, washing the obtained filter residue with deionized water, and drying to obtain regenerated graphite; according to the method provided by the invention, the pollution generated by the waste lithium ion battery is effectively reduced, and the waste graphite material of the negative electrode can be recycled to be the graphite negative electrode material. The regenerated material has excellent mechanical strength and toughness, good cycle performance, large reversible capacity and high capacity retention rate.

Description

Method for recycling graphite negative electrode of waste battery
Technical Field
The invention relates to the field of lithium ion battery recovery, in particular to a method for recovering a graphite cathode of a waste battery
Background
The decommissioning wave of the first wave power battery is about to come in 2018, and the decommissioned lithium ion battery reaches over 60 gigawatts in 2020. By 2030, the population using electric cars worldwide will reach 2.28 billion. With the rapid growth of electric automobiles, the annual demand of lithium ion batteries is also rapidly growing, which means that more and more lithium ion batteries are going to be retired in the future. Because the waste lithium ion battery contains heavy metals, organic solvents and harmful electrolytes, the waste lithium ion battery has great harm to the environment if not recycled. Meanwhile, the value of nickel, cobalt, manganese, lithium, iron and aluminum extracted from waste lithium ion battery cells reaches 101 million yuan by 2020. From this point of view, it is a valuable secondary resource. Recycling of used lithium ion batteries should be considered. The sustainability of lithium ion batteries should be of more interest, and recycling plays an important role. Since most of the valuable metals are present in the positive electrode, recycling of graphite of the negative electrode is receiving little attention from the industry and academia.
The recovery of negative electrode graphite in the following can be mainly classified into a pyrogenic process and a wet process. The pyrogenic process recovery process has the defects of high energy consumption, harmful gas emission, damaged structure of recovered graphite and entrainment of part of metal impurities; the wet recovery process mainly comprises acid pickling, and the acid pickling process has the problems of equipment corrosion, low acid utilization rate and difficulty in separation of copper foil and graphite. For example, the patent publication No. CN 105304967B discloses a method for recycling a graphite negative electrode sheet of a scrapped lithium ion battery, which comprises the following steps: a. crushing, namely crushing the raw materials by using a superfine crusher, wherein the particle size of the crushed materials is less than 20 microns; b. separating, namely passing the crushed powder through a cyclone separator on a crusher to obtain coarse copper powder and coarse stone ink powder with different densities; c. treating coarse copper powder, namely performing cyclone separation on the copper powder containing 2% of graphite powder impurities for 2-8 times to obtain 99.9% copper powder; d. and (3) treating the coarse graphite powder, namely dissolving the coarse graphite powder in a solution containing acid, passing through a centrifuge to obtain a wet graphite material, and drying through a drying oven to obtain the negative graphite powder of the lithium battery. The method is complex to operate and long in process, and the obtained collapsed structure of the graphite is not well repaired. Also, for example, patent publication No. CN107317048A discloses a method for recovering copper foil and graphite from negative electrode materials of waste lithium ion batteries. The method comprises the steps of soaking a negative plate in 1.0-3.0 mol/L sulfuric acid solution at the temperature of 30-60 ℃ for 1-3 min to completely separate copper foil from graphite; taking out the copper foil, washing with water, and drying to obtain a copper foil product; and filtering the graphite-containing solution by using a Buchner funnel, washing filter residues, drying and screening to obtain graphite. The graphite prepared by the method contains partial metal impurities, is easy to generate waste liquid, and has no repair measures for the collapsed structure of the waste lithium ion battery. In conclusion, the means for recovering the graphite cathode of the lithium ion battery by the acid washing process are not suitable.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for recycling the graphite cathode of the waste battery, which has the characteristics of simple preparation process, effective utilization of waste graphite materials, good restoration of the structure of the regenerated materials, large reversible capacity, designable capacity, good cycle performance and large-current discharge capacity and high tap density.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for recycling a graphite cathode of a waste battery comprises the following steps:
(1) discharging, disassembling, manually cutting or mechanically crushing the waste lithium ion battery to obtain a negative plate;
(2) mixing the obtained negative plate with salt which is hydrolyzed to be acidic and has strong oxidizing property, and soaking until copper in the negative plate is completely dissolved;
(3) and filtering the solution containing graphite, washing the obtained filter residue with deionized water, and drying to obtain the regenerated graphite.
Preferably, the solution used in the lithium ion discharge process in the step (1) is 0.2-6% sodium chloride solution, and the soaking time is 18-48 h, more preferably, the solution used is 3% sodium chloride, and the soaking time is 20 h.
Preferably, the width of the negative plate obtained in the step (1) through manual cutting and mechanical crushing is 3-5 cm, and the length of the negative plate is 3-8 cm.
Preferably, in the step (2), the solid-to-liquid ratio of the negative electrode plate to the salt is 1-100: 1g/L, and more preferably, the solid-to-liquid ratio of the negative electrode plate to the salt is 60 g/L.
Preferably, in the step (2), the salt molar concentration in the salt soaking process is 0-5 mol/L, the water bath heating temperature is 30-80 ℃, the soaking time is 10-80 min, more preferably, the water bath heating temperature is 60 ℃, the salt molar concentration of the soaking salt is 2mol/L, and the soaking time is 60 min.
Preferably, in step (2), the salt is selected from one or more of ammonium persulfate, sodium persulfate, potassium permanganate, sodium permanganate and potassium dichromate.
The invention has the beneficial effects that:
(1) the problem of in the recovery of old and useless lithium ion battery negative electrode material, copper foil and graphite can't thoroughly separate with high efficiency is solved, the battery level graphite that obtains, metallic impurity-free to utilize strong oxidizing salt to restore the damaged structure of graphite after thousands of charge-discharge cycles.
(3) No secondary pollution is generated in the recovery process, and the method is environment-friendly.
(4) The method has the advantages of simple process flow, high efficiency and environment-friendly recovery process, and the prepared high-purity graphite material is suitable for large-scale industrial recovery and reuse.
Drawings
FIG. 1 is an abstract drawing of the present invention;
FIG. 2 is an SEM image of a regenerated graphite material produced in example 1 of the present invention;
FIG. 3 is an XRD pattern of a regenerated graphite material produced in example 2 of the present invention;
FIG. 4 is an electrochemical cycle diagram of the regenerated graphite material obtained in example 1 of the present invention.
FIG. 5 is an electrochemical magnification chart of the regenerated graphite material obtained in example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
Example 1
The embodiment comprises the following steps:
(1) soaking a graphite cathode of a waste lithium ion battery in a 2% sodium chloride solution for 20h, then drying and disassembling to obtain 50g of cathode material, and then manually shearing a cathode piece with the length of 3cm and the width of 5 cm;
(2) placing the obtained regenerated graphite negative plate in 2mol/L ammonium persulfate solution according to the solid-to-liquid ratio of 50g/L, heating in water bath to 60 ℃, and soaking for 40min to completely dissolve the copper foil;
(3) after the reaction is finished, carrying out suction filtration on the solution containing the graphite, washing the solution for 3 times by using deionized water until the solution is neutral, and drying the solution to obtain the regenerated graphite.
The regenerated graphite material prepared in this example was subjected to electron microscope scanning, and the result is shown in fig. 2 (SEM), where it can be seen that the regeneration had a clear layered structure, the surface was smooth, no significant impurities were present, and the interlayer spacing was increased; the feasibility of preparing the regenerated graphite material by the experimental scheme is proved. In addition, the regenerated graphite material was subjected to electrochemical cycling test, and the result is shown in fig. 3, and the specific discharge capacity was maintained at 364mAh/g or more after 100 cycles of charging and discharging at a rate of 0.1C.
Example 2
(1) Soaking a graphite cathode of a waste lithium ion battery in a 6% sodium chloride solution for 18h, then drying and disassembling to obtain 100g of cathode material, and then manually shearing a cathode piece with the length of 3cm and the width of 8 cm;
(2) placing the obtained regenerated graphite negative plate in a sodium persulfate solution of 4mol/L according to a solid-to-liquid ratio of 30g/L, heating in a water bath to 80 ℃, and soaking for 40min to completely dissolve the copper foil;
(3) after the reaction is finished, carrying out suction filtration on the solution containing the graphite, washing the solution for 3 times by using deionized water until the solution is neutral, and drying the solution to obtain the regenerated graphite.
XRD test of the regenerated graphite material prepared in this example was carried out, and the results are shown in FIG. 4, and similar to FIG. 2(XRD pattern), it can be seen that the regenerated graphite retains the SP typical of graphite2The structure and the slight left shift of the characteristic peak of the carbon illustrate that the interlayer spacing of the regenerated graphite is enlarged, and the feasibility of preparing the regenerated graphite material by the experimental scheme is proved. And para-expanded graphite/silicon carbonElectrochemical performance tests of the composite material under different multiplying powers are carried out, as shown in fig. 5, the composite material is respectively charged and discharged for 10 circles under multiplying powers of 0.1C, 0.2C, 0.5C, 1C, 2C, 5C and 0.1C, the specific discharge capacity is respectively kept at 379.6mAh/g, 370.5mAh/g, 374.2mAh/g, 342.7mAh/g, 284.2mAh/g and more than 150.5mAh/g, particularly, the multiplying power is recycled to 0.1C for charging and discharging, and the specific discharge capacity can be recovered to more than 372.1 mAh/g.
Example 3
(1) Soaking a graphite cathode of a waste lithium ion battery in a 4% sodium chloride solution for discharging for 24h, then drying and disassembling to obtain 80g of a cathode material, and then manually shearing a cathode piece with the length of 3cm and the width of 7 cm;
(2) placing the obtained regenerated graphite negative plate in 5mol/L potassium dichromate solution according to the solid-to-liquid ratio of 80g/L, heating in water bath to 80 ℃, and soaking for 60min to completely dissolve the copper foil;
(3) after the reaction is finished, carrying out suction filtration on the solution containing the graphite, washing the solution for 5 times by using deionized water until the solution is neutral, and drying the solution to obtain the regenerated graphite.
The above description is only a basic description of the present invention, and any equivalent changes made according to the technical solution of the present invention should fall within the protection scope of the present invention.

Claims (3)

1. A method for recycling a graphite cathode of a waste battery is characterized by comprising the following steps:
(1) discharging, disassembling, manually cutting or mechanically crushing the waste lithium ion battery to obtain a negative plate;
(2) mixing the obtained negative plate with salt which is hydrolyzed to be acidic and has strong oxidizing property, and then heating in a water bath to soak the negative plate until copper in the negative plate is completely dissolved;
(3) and filtering the solution containing graphite, washing the obtained filter residue with deionized water, and drying to obtain the regenerated graphite.
2. The method for recycling the graphite cathode of the waste battery according to claim 1, wherein in the step (1), the discharging process is to soak the waste lithium ion battery in 0.2-6% sodium chloride solution for 18-48 h, and the width of the cathode piece obtained through the manual cutting and mechanical crushing processes is 3-5 cm, and the length of the cathode piece is 3-8 cm.
3. The method for recycling the graphite cathode of the waste battery is characterized in that the salt solution used in the step (2) is one or more of ammonium persulfate, sodium persulfate, potassium permanganate, sodium permanganate and potassium dichromate according to the following claims 1 and 2; the solid-to-liquid ratio of the negative plate to the salt is 1-100: 1g/L, preferably 60 g/L; the concentration of the salt solution is 0-5 mol/L, preferably 2mol/L, and the soaking time is 10-80 min, preferably 60 min; the water bath heating temperature is 30-80 ℃, and preferably 60 ℃.
CN202110330381.XA 2021-03-29 2021-03-29 Method for recycling graphite negative electrode of waste battery Pending CN113200541A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113860351A (en) * 2021-08-23 2021-12-31 中南大学 Preparation method and application of CuO-graphite composite material prepared from waste graphite
CN116443872A (en) * 2023-05-08 2023-07-18 贺州学院 Method for preparing high-performance expanded graphite from waste lithium ion battery negative electrode graphite

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113860351A (en) * 2021-08-23 2021-12-31 中南大学 Preparation method and application of CuO-graphite composite material prepared from waste graphite
CN116443872A (en) * 2023-05-08 2023-07-18 贺州学院 Method for preparing high-performance expanded graphite from waste lithium ion battery negative electrode graphite

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Application publication date: 20210803