CN113802000A - Lithium ion battery positive electrode material recovery process - Google Patents
Lithium ion battery positive electrode material recovery process Download PDFInfo
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- CN113802000A CN113802000A CN202110928945.XA CN202110928945A CN113802000A CN 113802000 A CN113802000 A CN 113802000A CN 202110928945 A CN202110928945 A CN 202110928945A CN 113802000 A CN113802000 A CN 113802000A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/0007—Preliminary treatment of ores or scrap or any other metal source
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 process for recovering the positive electrode material of Li-ion battery includes such steps as crushing, specific gravity separation to remove Al from powder, dusting the rest powder to obtain the first remainder, high-temp heating to obtain the second remainder, putting the second remainder in the electrolyte solution of Co, stacking the second remainder around or adhering it to anode, and electrolyzing the anode and cathode until solid Co is obtained on cathode and coated on the surface of cathode. The design has the advantages of high utilization rate of raw materials, difficult generation of waste gas and waste liquid, low recovery cost and contribution to reducing energy consumption.
Description
Technical Field
The invention relates to a recovery process, belongs to the field of lithium ion battery recovery, and particularly relates to a recovery process of a lithium ion battery anode material.
Background
The lithium ion battery anode material contains relatively expensive cobalt element inside, has high recovery value, and in addition, the waste lithium ion battery has certain toxicity and difficult degradability, belongs to a serious pollution source, and poses great threat to the environment and human health, so that the recovery of the cobalt element from the waste battery is an excellent technology with economic value and environmental protection.
The invention patent application with the application number of CN201910085004.7 and the application date of 2019, 1 month and 29 days discloses a method for recycling cobalt and lithium in waste lithium cobalt oxide batteries through molten salt electrolysis, which comprises the following steps: pressing lithium cobaltate anode powder, sintering to serve as a cathode, graphite as an anode, eutectic mixed salt of carbonate as molten salt, inserting the graphite anode and a LiCoO2 cathode into the molten salt, applying constant voltage between the graphite anode and a LiCoO2 sheet cathode, and electrolyzing for 3-5 hours to obtain an electrolyzed cathode; and extracting fused salt from the cathode after electrolysis, cooling, cleaning and removing impurities to obtain Co or CoO powder. Although this method enables the recovery of CoO or Co powder, achieving recycling of resources, it still has the following drawbacks:
firstly, the design needs to grind the lithium cobaltate anode into powder and then remake the cathode, so that external element pollution is easily introduced;
secondly, in the process of electrolysis, the design is easy to generate waste liquid and waste gas, and pollutes the environment.
The information disclosed in this background section is only for enhancement of understanding of the general background of the patent application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects and problems of high recovery cost and easy generation of waste gas and waste liquid in the prior art, and provides a recovery process of a lithium ion battery anode material, which has low recovery cost and is difficult to generate waste gas and waste liquid.
In order to achieve the above purpose, the technical solution of the invention is as follows: a lithium ion battery positive electrode material recycling process, comprising the steps of:
specific gravity dealuminization: crushing the lithium ion battery anode material, then carrying out specific gravity sorting on the crushed powder to remove metal aluminum in the powder, and then carrying out dust removal on the residual powder to obtain a first residue;
high-temperature burning-out step: putting the first residue into a furnace for high-temperature heating to obtain a second residue;
and (3) electrolyzing to obtain cobalt: the second residue is firstly arranged in the cobalt electrolyte, after the arrangement, the second residue is stacked around the electrolytic anode or bonded on the electrolytic anode, and then the electrolytic anode and the electrolytic cathode which are inserted into the cobalt electrolyte are electrified for electrolysis until solid cobalt is obtained on the electrolytic cathode, and the solid cobalt is coated on the outer surface of the electrolytic cathode.
The solute of the obtained cobalt electrolyte is 0.01-5 mol/l of organic acid radical and 0.01-5 mol/l of inorganic acid radical, and the solvent of the electrolyte is ultrapure water; the PH value of the obtained cobalt electrolyte is between 0.5 and 1.5.
The organic acid radical is any one or any mixture of a sulfonic acid radical, a citrate radical, a formate radical and a sulfinate radical;
the inorganic acid radical is any one or any mixture of sulfate radical and nitrate radical.
In the specific gravity dealuminization step, the crushing of the lithium ion battery anode material refers to: and crushing the lithium ion battery anode material by using a multi-cutter crusher.
In the specific gravity dealuminization step, the specific gravity sorting of the crushed powder is as follows:
the crushed powder is firstly put into a specific gravity sorting machine and then is subjected to specific gravity sorting, at the moment, the crushed powder comprises powder with larger relative gravity and powder with smaller relative gravity, and then the powder with larger relative gravity is removed, so that the aim of removing the metal aluminum in the powder is fulfilled.
The powder with a large relative specific gravity refers to metallic aluminum or a powder containing metallic aluminum, and the powder with a small relative specific gravity refers to carbon or lithium cobalt powder.
In the high-temperature burning-out step, the parameters of high-temperature heating are as follows: the temperature is 180-600 ℃, and the time is 2-3H.
In the step of obtaining cobalt through electrolysis, the electrolysis anode is a graphite electrode or other inert electrodes, and the electrolysis cathode is a titanium plate or other inert electrodes.
In the step of obtaining cobalt by electrolysis, the current density of the electrolysis is 2-50A/square meter.
In the step of obtaining cobalt by electrolysis, after solid cobalt is obtained on an electrolysis cathode, the solid cobalt is taken down firstly, pure water is used for cleaning and removing the obtained cobalt electrolyte on the surface of the solid cobalt, and then the solid cobalt is dried to obtain the final cobalt with the purity of more than or equal to 99.9 percent.
Compared with the prior art, the invention has the beneficial effects that:
1. in the recovery process of the lithium ion battery anode material, the steps of specific gravity dealumination, high temperature burning-off and electrolysis to obtain cobalt are sequentially carried out, wherein in the initial specific gravity dealumination step, the lithium ion battery anode material only needs to directly participate in treatment and is directly crushed into powder without reworking a cathode, so that the pollution of external elements is avoided, and the normal operation of subsequent treatment is facilitated. Therefore, the recycling cost of the invention is lower.
2. In the lithium ion battery anode material recovery process, when the step of obtaining cobalt by electrolysis is carried out, the solute of the adopted cobalt electrolyte is organic acid radical and inorganic acid radical, the solvent of the electrolyte is ultrapure water, and the contents of the organic acid radical and the inorganic acid radical are limited. Therefore, the invention not only has higher utilization rate of raw materials, but also is not easy to generate waste gas and waste liquid.
3. In the high-temperature burning-out step, the parameters for limiting high-temperature heating are that the temperature is 180-600 ℃ and the time is 2-3H, the reason is that the removal target of the high-temperature burning-out step is mainly PVDF, while the melting point of PVDF is 177 ℃, researches show that burning-out for more than 2 hours at the temperature higher than the temperature can greatly facilitate the smooth proceeding of subsequent electrolysis (because PVDF is an organic matter, the conductivity is poor, the burning-out is beneficial to the next step of electrolysis), in addition, the voltage of the subsequent electrolysis can be reduced, and the power consumption is saved. Therefore, the invention not only has good high-temperature burning-off effect, but also is beneficial to reducing energy consumption.
4. In the recovery process of the lithium ion battery cathode material, solid cobalt is directly obtained at last, the purity of the solid cobalt is more than or equal to 99.9%, meanwhile, the recovery rate of the cobalt is 99% or more by comparing with the raw material, and the recovery process has higher recovery effect by considering the recovery purity and the recovery rate. Therefore, the invention has better recovery effect.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
A lithium ion battery positive electrode material recycling process, comprising the steps of:
specific gravity dealuminization: crushing the lithium ion battery anode material, then carrying out specific gravity sorting on the crushed powder to remove metal aluminum in the powder, and then carrying out dust removal on the residual powder to obtain a first residue;
high-temperature burning-out step: putting the first residue into a furnace for high-temperature heating to obtain a second residue;
and (3) electrolyzing to obtain cobalt: the second residue is firstly arranged in the cobalt electrolyte, after the arrangement, the second residue is stacked around the electrolytic anode or bonded on the electrolytic anode, and then the electrolytic anode and the electrolytic cathode which are inserted into the cobalt electrolyte are electrified for electrolysis until solid cobalt is obtained on the electrolytic cathode, and the solid cobalt is coated on the outer surface of the electrolytic cathode.
The solute of the obtained cobalt electrolyte is 0.01-5 mol/l of organic acid radical and 0.01-5 mol/l of inorganic acid radical, and the solvent of the electrolyte is ultrapure water; the PH value of the obtained cobalt electrolyte is between 0.5 and 1.5.
The organic acid radical is any one or any mixture of a sulfonic acid radical, a citrate radical, a formate radical and a sulfinate radical;
the inorganic acid radical is any one or any mixture of sulfate radical and nitrate radical.
In the specific gravity dealuminization step, the crushing of the lithium ion battery anode material refers to: and crushing the lithium ion battery anode material by using a multi-cutter crusher.
In the specific gravity dealuminization step, the specific gravity sorting of the crushed powder is as follows:
the crushed powder is firstly put into a specific gravity sorting machine and then is subjected to specific gravity sorting, at the moment, the crushed powder comprises powder with larger relative gravity and powder with smaller relative gravity, and then the powder with larger relative gravity is removed, so that the aim of removing the metal aluminum in the powder is fulfilled.
The powder with a large relative specific gravity refers to metallic aluminum or a powder containing metallic aluminum, and the powder with a small relative specific gravity refers to carbon or lithium cobalt powder.
In the high-temperature burning-out step, the parameters of high-temperature heating are as follows: the temperature is 180-600 ℃, and the time is 2-3H.
In the step of obtaining cobalt through electrolysis, the electrolysis anode is a graphite electrode or other inert electrodes, and the electrolysis cathode is a titanium plate or other inert electrodes.
In the step of obtaining cobalt by electrolysis, the current density of the electrolysis is 2-50A/square meter.
In the step of obtaining cobalt by electrolysis, after solid cobalt is obtained on an electrolysis cathode, the solid cobalt is taken down firstly, pure water is used for cleaning and removing the obtained cobalt electrolyte on the surface of the solid cobalt, and then the solid cobalt is dried to obtain the final cobalt with the purity of more than or equal to 99.9 percent.
The principle of the invention is illustrated as follows:
the positive electrode material of the lithium ion battery mainly comprises lithium cobaltate (LiCoO 2), a conductive agent (conductive graphite), a bonding agent (PVDF) and a current collector (aluminum foil). The conductive graphite as the conductive agent is inert, and the inert does not participate in the electrolysis, so that the residual material after the final electrolysis contains the conductive graphite, and meanwhile, the content of the conductive graphite is not high (about 2 percent), so that special treatment is not needed.
In the invention, the residue II obtained in the high-temperature burning-out step is in a dispersed flake shape, and in this case, if the residue II is to participate in the electrolytic reaction, the residue II and the electrolytic anode need to be bonded together (for example, bonded together by using a bonding agent), or the residue II needs to be stacked around the electrolytic anode.
Example 1:
a lithium ion battery positive electrode material recycling process, comprising the steps of:
specific gravity dealuminization: crushing the lithium ion battery anode material, then carrying out specific gravity sorting on the crushed powder to remove metal aluminum in the powder, and then carrying out dust removal on the residual powder to obtain a first residue;
high-temperature burning-out step: putting the first residue into a furnace for high-temperature heating (preferably, the high-temperature heating parameters are that the temperature is 180-600 ℃, and the time is 2-3H) to obtain a second residue;
and (3) electrolyzing to obtain cobalt: firstly, arranging the second residue in a cobalt electrolyte, wherein the solute of the cobalt electrolyte is 2.6mol/l of organic acid radical and 2.4mol/l of inorganic acid radical, the solvent of the cobalt electrolyte is ultrapure water, the PH value of the cobalt electrolyte is 1.0, after arrangement, the second residue is accumulated around an electrolytic anode or is adhered on the electrolytic anode, and then electrifying the electrolytic anode and the electrolytic cathode which are inserted into the cobalt electrolyte for electrolysis until solid cobalt is obtained on the electrolytic cathode, and the solid cobalt is coated on the outer surface of the electrolytic cathode. The purity of the solid cobalt was 99.90% and the recovery was 99.20%.
Example 2:
the basic contents are the same as example 1, except that:
preferably, the solute of the obtained cobalt electrolyte is 4.8mol/l of organic acid radical, 0.02mol/l of inorganic acid radical and the PH value is 1.3; the purity of the solid cobalt was 99.91% and the recovery was 99.10%.
Example 3:
the basic contents are the same as example 1, except that:
preferably, the solute of the obtained cobalt electrolyte is 0.02mol/l of organic acid radical, 4.9mol/l of inorganic acid radical and the PH value is 0.7; the purity of the solid cobalt was 99.92% and the recovery was 99.05%.
Example 4:
the basic contents are the same as example 1, except that:
preferably, the solute of the obtained cobalt electrolyte is 0.01mol/l of organic acid radical, 5mol/l of inorganic acid radical and the PH value is 0.5; the purity of the solid cobalt was 99.93% and the recovery was 99.15%.
Example 5:
the basic contents are the same as example 1, except that:
preferably, the solute of the obtained cobalt electrolyte is 5.0mol/l of organic acid radical, 0.01mol/l of inorganic acid radical and the PH value is 1.5; the purity of the solid cobalt was 99.90% and the recovery was 99.10%.
Example 6:
the basic contents are the same as example 1, except that:
the organic acid radical is any one or any mixture of a sulfonic acid radical, a citrate radical, a formate radical and a sulfinate radical; the inorganic acid radical is any one or any mixture of sulfate radical and nitrate radical.
Example 7:
the basic contents are the same as example 1, except that:
in the specific gravity dealuminization step, the specific gravity sorting of the crushed powder is as follows: the crushed powder is firstly put into a specific gravity sorting machine and then specific gravity sorting is carried out, in this case, the crushed powder comprises powder with larger relative gravity (preferably metal aluminum or powder containing metal aluminum) and powder with smaller relative gravity (preferably carbon and lithium cobalt powder), and then the powder with larger relative gravity is removed, so as to achieve the purpose of removing the metal aluminum in the powder.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention as set forth in the appended claims.
Claims (10)
1. A lithium ion battery anode material recovery process is characterized by comprising the following steps:
specific gravity dealuminization: crushing the lithium ion battery anode material, then carrying out specific gravity sorting on the crushed powder to remove metal aluminum in the powder, and then carrying out dust removal on the residual powder to obtain a first residue;
high-temperature burning-out step: putting the first residue into a furnace for high-temperature heating to obtain a second residue;
and (3) electrolyzing to obtain cobalt: the second residue is firstly arranged in the cobalt electrolyte, after the arrangement, the second residue is stacked around the electrolytic anode or bonded on the electrolytic anode, and then the electrolytic anode and the electrolytic cathode which are inserted into the cobalt electrolyte are electrified for electrolysis until solid cobalt is obtained on the electrolytic cathode, and the solid cobalt is coated on the outer surface of the electrolytic cathode.
2. The lithium ion battery positive electrode material recovery process according to claim 1, characterized in that: the solute of the obtained cobalt electrolyte is 0.01-5 mol/l of organic acid radical and 0.01-5 mol/l of inorganic acid radical, and the solvent of the electrolyte is ultrapure water; the PH value of the obtained cobalt electrolyte is between 0.5 and 1.5.
3. The lithium ion battery positive electrode material recovery process according to claim 2, characterized in that:
the organic acid radical is any one or any mixture of a sulfonic acid radical, a citrate radical, a formate radical and a sulfinate radical;
the inorganic acid radical is any one or any mixture of sulfate radical and nitrate radical.
4. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the specific gravity dealuminization step, the crushing of the lithium ion battery anode material refers to: and crushing the lithium ion battery anode material by using a multi-cutter crusher.
5. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the specific gravity dealuminization step, the specific gravity sorting of the crushed powder is as follows:
the crushed powder is firstly put into a specific gravity sorting machine and then is subjected to specific gravity sorting, at the moment, the crushed powder comprises powder with larger relative gravity and powder with smaller relative gravity, and then the powder with larger relative gravity is removed, so that the aim of removing the metal aluminum in the powder is fulfilled.
6. The lithium ion battery positive electrode material recovery process according to claim 5, characterized in that: the powder with a large relative specific gravity refers to metallic aluminum or a powder containing metallic aluminum, and the powder with a small relative specific gravity refers to carbon or lithium cobalt powder.
7. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the high-temperature burning-out step, the parameters of high-temperature heating are as follows: the temperature is 180-600 ℃, and the time is 2-3H.
8. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the step of obtaining cobalt through electrolysis, the electrolysis anode is a graphite electrode or other inert electrodes, and the electrolysis cathode is a titanium plate or other inert electrodes.
9. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the step of obtaining cobalt by electrolysis, the current density of the electrolysis is 2-50A/square meter.
10. The recycling process of the lithium ion battery positive electrode material according to the claim 1, 2 or 3, characterized in that: in the step of obtaining cobalt by electrolysis, after solid cobalt is obtained on an electrolysis cathode, the solid cobalt is taken down firstly, pure water is used for cleaning and removing the obtained cobalt electrolyte on the surface of the solid cobalt, and then the solid cobalt is dried to obtain the final cobalt with the purity of more than or equal to 99.9 percent.
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| CN112718800A (en) * | 2020-12-16 | 2021-04-30 | 天津华庆百胜能源有限公司 | Recovery processing method of waste lithium battery |
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2021
- 2021-08-13 CN CN202110928945.XA patent/CN113802000A/en active Pending
Patent Citations (8)
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| CN101381817A (en) * | 2007-12-07 | 2009-03-11 | 佛山市邦普镍钴技术有限公司 | Method for directly recovering and producing electrowinning cobalt from waste and old lithium ionic cell |
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