CN112320802A - Recycling method of silicon-carbon negative electrode material - Google Patents
Recycling method of silicon-carbon negative electrode material Download PDFInfo
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- CN112320802A CN112320802A CN202011003922.XA CN202011003922A CN112320802A CN 112320802 A CN112320802 A CN 112320802A CN 202011003922 A CN202011003922 A CN 202011003922A CN 112320802 A CN112320802 A CN 112320802A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
The invention relates to the field of lithium ion batteries, in particular to a method for recycling a silicon-carbon negative electrode material. The recycling method comprises the following steps: carrying out three-order continuous constant temperature heat treatment on the silicon-carbon cathode recycled raw material, and specifically comprising the following steps: coking the SEI film in the silicon-carbon negative electrode recovery raw material at 400-650 ℃ in an inert atmosphere; depositing a carbon layer on the surface of the recovered raw material of the silicon-carbon negative electrode by vapor deposition at 700-900 ℃; carbonizing the carbon layer at 950-1200 deg.C under inert atmosphere. The invention effectively processes the collected cathode recycled raw materials aiming at the problems in the process of recycling the silicon-carbon cathode, so that the performance of the product obtained after recycling is close to the performance of the original material, and the invention has positive significance for improving the performance of the regenerated silicon-carbon cathode material product and the comprehensive recycling rate of the retired battery.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a method for recycling a silicon-carbon negative electrode material.
Background
Lithium ion batteries are consumables, and their capacity is constantly decreasing during use. With the new energy electric automobile becoming an important development direction of the automobile industry, the retirement and recycling of the power lithium battery of the electric automobile becomes a problem to be solved urgently in the fields of new energy automobiles and energy storage. The silicon-based material is considered to be one of the preferred negative electrode materials of the next generation of high-energy density lithium ion battery due to the fact that the silicon-based material has high specific capacity, proper working potential and abundant storage capacity. The price of the silicon carbon material in the current market is about 100 ten thousand per ton, so that the silicon carbon material in the retired lithium battery is effectively recycled, and great economic benefits are achieved.
The silicon-carbon material has large volume expansion in the circulation process, the negative electrode material can crack or even be pulverized after long-term circulation, and then a thick Solid Electrolyte Interface (SEI) film is formed on the surface. Meanwhile, the negative electrode powder material collected after the battery is disassembled contains some transition metal elements, and part of the metal elements are introduced in the disassembling process, and the metal elements of the adopted high-nickel positive electrode material are possibly deposited on the negative electrode in the circulating process. Therefore, the collected powder material after the battery is disassembled needs to be further processed, and the properties of the finally regenerated silicon-carbon material can meet the requirements of recycling.
CN 109065993A discloses a method for recycling a silicon-carbon negative electrode material in a failure battery, which comprises the steps of ultrasonically stripping the silicon-carbon material from a disassembled negative electrode piece through deionized water, then placing the silicon-carbon material in an inert atmosphere for high-temperature pretreatment, then placing the silicon-carbon material in the deionized water for multiple times of centrifugal washing, separation and drying to obtain a raw material, grinding and mixing the raw material and phenolic resin, then carrying out high-temperature sintering, and finally mixing and stirring a sintered product, a pyrrole monomer and conductive carbon black to obtain the silicon-oxygen-carbon/graphite negative electrode material. According to the scheme, phenolic resin is used as a carbon source for carbon coating, when the content of the phenolic resin is low, the phenolic resin is difficult to dip into gaps left after the coating is broken due to the fact that a large contact angle exists between softened phenolic resin and raw material particles, the coating is possibly uneven and incomplete, and the improvement of the cycle performance of a product is limited. Increasing the phenolic resin content will in turn decrease the reversible capacity and first coulombic efficiency of the final product. Meanwhile, the product manufactured by the scheme has the possibility that the content of metal elements is higher, and the metal elements are coated in the material by carbon, so that the impurity removal process is not very effective even if the impurity removal process is added, and the manufactured lithium battery has certain safety problem.
CN 108039530A discloses a recycling and regenerating process of a graphite material of a waste battery, which comprises the steps of carrying out wet grinding on a negative plate in the waste battery to separate a copper foil and negative powder, then adding a certain amount of dispersant, collector and foaming agent to enable the graphite material to float to separate the graphite and the copper foil, adding an oxidant and inorganic acid to remove metal impurities, then carrying out heat treatment to remove residual organic matters and obtain high-purity graphite, then dispersing the graphite in a phenolic resin solution and drying, and finally carrying out high-temperature heat treatment to carry out carbon coating. When the scheme is adopted for recycling the silicon-carbon cathode material, organic solvents such as acetone and the like are introduced to dissolve the phenolic resin, and the volatilization of the organic solvents can possibly pollute the environment. The carbon coating using phenolic resin as carbon source also produced similar problems as CN 109065993 a.
Disclosure of Invention
The invention optimizes the recycling method of the silicon-carbon cathode material and obtains the following scheme:
a method for recycling a silicon-carbon negative electrode material comprises the following steps: carrying out three-order continuous constant temperature heat treatment on the silicon-carbon cathode recovery raw material, wherein the three-order continuous constant temperature heat treatment specifically comprises the following steps:
coking the SEI film in the silicon-carbon negative electrode recovery raw material at 400-650 ℃ in an inert atmosphere;
depositing a carbon layer on the surface of the recovered raw material of the silicon-carbon negative electrode by vapor deposition at 700-900 ℃;
carbonizing the carbon layer at 950-1200 deg.C under inert atmosphere.
Compared with the prior art that solid carbon sources such as phenolic resin, asphalt and the like are adopted, the amorphous carbon layer generated by the method is more uniform and complete, and has good interface contact and conductivity enhancement effects. Meanwhile, for silicon carbon particles which are cracked in the battery cycle process, amorphous carbon can be filled in gaps of the cracked particles, and the integrity of a sample coating layer is improved. In addition, the required carbon content is less, so that the reversible capacity and the first coulombic efficiency of the finally obtained product are closer to those of the silicon-carbon material before circulation, and the circulation performance is good.
Before the chemical vapor deposition, the SEI film in the silicon-carbon cathode recovery raw material is coked at 400-650 ℃, which is beneficial to improving the integrity of a carbon layer on the surface of the material.
Preferably, the three-stage continuous constant temperature heat treatment is performed by a single temperature rise process.
Specifically, the temperature is raised to 400-650 ℃ for constant temperature heat treatment, then raised to 700-900 ℃ for constant temperature heat treatment, and then raised to 950-1200 ℃ for heat treatment.
More preferably, the rate of temperature rise is 2 to 10 ℃/min.
During the temperature rise (especially at the temperature rise rate) and the constant temperature heat treatment process at 400-650 ℃, carbon sources possibly contained in the recycled raw materials of the negative electrode can be utilized to carry out primary carbon coating on the recycled raw materials.
In addition, the invention can complete the coking treatment of the SEI film of the cathode recovered raw material in sequence through a one-time heating process, carry out vapor deposition by using a carbon source, and sinter and carbonize with a carbon layer, thereby reducing the process steps of the recovery treatment, improving the production efficiency and reducing the energy consumption.
Preferably, in the vapor deposition, the gas phase is a mixed gas of a carbon source gas and an inert gas, wherein the content of the carbon source gas is 20-40 vol%, more preferably 20-30 vol%, which is further beneficial to improving the electrical properties of the product.
Preferably, the carbon source gas is selected from one of methane, acetylene, ethylene, propylene and toluene.
The inert atmosphere or inert gas of the present invention includes, but is not limited to, nitrogen, argon.
Preferably, the D50 of the silicon-carbon negative electrode recycled raw material is 10-15 microns.
In some embodiments, the recycled silicon-carbon anode raw material particles are required to have a D50 of 10-15 μm after being subjected to particle size adjustment, and the particle size adjustment method includes, but is not limited to, ball milling, jet milling, classification, and the like.
In some embodiments, the holding time at 400-650 ℃ is 1-4 hours, the holding time at 700-900 ℃ is 2-10 hours, and the holding time at 950-1200 ℃ is 1-4 hours, and the holding time can be adjusted by one skilled in the art according to actual conditions, and is not further limited herein.
In the heat treatment process of 400-650 deg.C, 700-900 deg.C and 950-1200 deg.C (especially 700-900 deg.C), when the recovered raw material particles are fully contacted with the introduced gas, the treatment effect is better, and the method for fully contacting the recovered raw material particles includes but is not limited to stirring or fluidized bed.
Preferably, the silicon-carbon negative electrode recycled raw material particles are obtained by the following steps:
and performing acid leaching on the failed cathode material, removing metals contained in the failed cathode material, and collecting filter residues to obtain a silicon-carbon cathode recycled raw material.
Preferably, when the acid leaching is carried out, the concentration of acid is 2-10mol/L, the solid-to-liquid ratio is 1g/1ml-1g/10ml, the reaction temperature is 25-80 ℃, and the acid is selected from one of hydrochloric acid, sulfuric acid and nitric acid or a mixture of the hydrochloric acid, the sulfuric acid and the nitric acid.
In some embodiments, the acid leaching time is 1-10h, which can be adjusted by one skilled in the art according to actual conditions, and is not further limited herein.
Preferably, after the acid leaching, the metal-containing filtrate is collected and used for recovering the positive electrode material.
The metal elements in the cathode material have certain influence on the safety performance of the battery. The acid leaching can remove impurities of metal elements from the collected cathode material, so that the metal impurities in the silicon-carbon cathode product are reduced, and the influence of the metal elements introduced in the cathode material recovery process on the appearance of a subsequent vapor deposition carbon layer and the integrity of the carbon layer is reduced. On the other hand, the collected metal elements can be further processed according to the conventional method for recovering and regenerating the cathode material. Compared with the prior art, the comprehensive recovery rate of resources and the safety performance of applying the silicon-carbon material product to the battery can be improved.
Preferably, the obtaining process of the failed anode material is as follows:
and (3) placing the negative pole piece of the lithium ion battery in water, and stirring or ultrasonically treating to peel off the invalid negative pole material coated on the copper foil.
Silicon carbon negative electrodes generally use an aqueous binder, and the water-soluble binder can be used to achieve simple separation of the spent negative electrode material and the current collector copper foil. The separation efficiency can be accelerated by adopting methods such as ultrasonic or stirring, and the oxidation of silicon particles and the volume loss caused by long-time soaking are avoided. Meanwhile, the copper foil can be integrally collected, and compared with crushing and separating methods of other recovery processes, the method reduces the material grading step and the recovery difficulty.
In a preferred embodiment, the recycling process comprises the steps of:
(1) placing a negative pole piece of the lithium ion battery in water, and stirring or ultrasonically treating to enable the invalid negative pole material coated on the copper foil to be peeled off and dispersed in the water;
(2) performing acid leaching on the invalid cathode material dispersed in water, removing metals contained in the invalid cathode material, and collecting filter residues to obtain a silicon-carbon cathode recycled raw material;
(3) adjusting the granularity of the silicon-carbon negative electrode recycled raw material to enable the D50 to be 10-15 microns;
(4) carrying out three-order continuous constant-temperature heat treatment on the silicon-carbon cathode recycled raw material particles obtained by the treatment, and specifically comprising the following steps:
(4a) heating the recovered silicon-carbon cathode raw material from room temperature to 400-650 ℃ at the heating rate of 2-10 ℃/min under the inert atmosphere, and coking the SEI film in the recovered raw material at the temperature of 400-650 ℃;
(4b) heating to 700-900 ℃ at the heating rate of 2-10 ℃/min, and depositing a carbon layer on the surface of the recovered raw material through vapor deposition at the temperature of 700-900 ℃;
in the vapor deposition, the gas phase is a mixed gas of a carbon source gas and an inert gas, wherein the content of the carbon source gas is 20-40 vol%;
(4c) in inert atmosphere, raising the temperature to 950-1200 ℃ at the temperature raising rate of 2-10 ℃/min, and carbonizing the carbon layer at 950-1200 ℃.
The above-described schemes can be combined by those skilled in the art to obtain the preferred embodiments of the present invention.
Based on the technical scheme, the invention has the following beneficial effects:
the invention provides a method for recycling a silicon-carbon negative electrode material in a retired lithium ion battery, aiming at the problems existing in the silicon-carbon negative electrode recycling process, the collected negative electrode recycling raw materials are effectively processed, and the performance of a product obtained after recycling is close to the performance of an original material. Compared with the direct production of the silicon-carbon cathode, the method saves the raw materials and the processing cost of the product, and saves the energy raw materials consumed in the production process. Compared with other methods for recycling silicon-carbon negative electrode materials, the method has the advantages of shorter process, better efficiency, avoidance of introduction of organic solvent and positive significance in improving the product performance of the regenerated silicon-carbon negative electrode material and the comprehensive recycling rate of the retired battery.
Drawings
FIG. 1 is a flowchart of example 1 of the present invention;
figure 2 is a graph of the cycling performance of the button cells of the samples prepared in example 1;
figure 3 is a graph of the cycling performance of the button cells of the samples prepared in example 3.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The present embodiment provides a method for recycling a silicon-carbon negative electrode material, and a flow chart is shown in fig. 1, which specifically includes:
the method comprises the following steps: fully discharging the retired battery, disassembling the lithium ion battery, selecting and collecting the negative pole piece from the positive pole piece, the negative pole piece and the diaphragm. And placing the collected negative pole piece into deionized water, and stirring for 1 hour by using a stirrer, so that the block material coated on the copper foil is peeled off and is fully dispersed in the water.
Step two: the material dispersed in water was subjected to acid leaching at 65 ℃ for 2 hours in 5mol/L hydrochloric acid at a solid-to-liquid ratio of 1g/5 ml. The filtrate containing the metal elements obtained by suction filtration is used as the cathode recovery raw material, and the process for recovering the cathode raw material is not described in detail in this example. And taking filter residue washed to be neutral as a negative electrode recovery raw material.
Step three: the particle size of the recovered anode material was adjusted to 13 μm by a jet mill to D50.
Step four: and (3) placing the sample in a rotary tube furnace for three-stage continuous constant-temperature chemical vapor deposition carbon coating. Under the nitrogen environment, the sample is heated to 400 ℃ at the heating rate of 5 ℃/min and is kept at the constant temperature for 2 hours, then the sample is heated to 850 ℃ at the heating rate of 5 ℃/min, 20 vol% acetylene nitrogen mixed gas is introduced, and the constant temperature time at 850 ℃ is 2 hours. Then, the atmosphere is changed into nitrogen, the temperature is raised to 1000 ℃ at the heating rate of 10 ℃/min, the temperature is maintained for 2 hours, carbonization is carried out, and finally the temperature is lowered to the room temperature and the powder sample 1 is taken out.
The button cell preparation and test method comprises the following steps: the CR2032 button half-cell was assembled with an active material mass fraction of 86%, a conductive agent mass fraction of 6% (VGCF: SP: 1:5), and a binder mass fraction of 8% (CMC: SBR: 1). LiPF with electrolyte of 1mol/L6Dissolved in EC DMC EMC (1:1:1) solvent, and the surface density of the electrode is 3.5mg/cm2. Constant current charging and discharging are carried out on the button type half cell at the current of 0.1C, and the voltage range is 0.005-2V (vs Li/Li)+). The button cell cycle performance diagram of the sample is shown in figure 2, and the first charge-discharge specific capacity and efficiency are shown in table 1.
Example 2
This example differs from example 1 in that the volume fraction of acetylene in the acetylene nitrogen mixer was changed from 20 vol% to 40 vol%, and the constant temperature time at 850 ℃ was changed from 2 hours to 1 hour. The other steps are the same as in example 1.
Powder sample 2 was obtained by this example and its first charge-discharge specific capacity and efficiency are shown in table 1.
Example 3
The present example is different from example 1 in that step two is not included, and the particle size adjustment in step three is directly performed after the sample collected in step one is dried. The other steps are the same as in example 1.
The powder sample 3 obtained by the embodiment has a button cell cycle performance chart shown in fig. 3, and the first charge-discharge specific capacity and efficiency are shown in table 1.
TABLE 1
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for recycling a silicon-carbon negative electrode material is characterized by comprising the following steps: carrying out three-order continuous constant temperature heat treatment on the silicon-carbon cathode recovery raw material, wherein the three-order continuous constant temperature heat treatment specifically comprises the following steps:
coking the SEI film in the silicon-carbon negative electrode recovery raw material at 400-650 ℃ in an inert atmosphere;
depositing a carbon layer on the surface of the recovered raw material of the silicon-carbon negative electrode by vapor deposition at 700-900 ℃;
carbonizing the carbon layer at 950-1200 deg.C under inert atmosphere.
2. The recycling method according to claim 1, wherein the three-stage continuous constant temperature heat treatment is performed by a single temperature rise process.
3. The recycling method according to claim 2, wherein the temperature rise rate is 2 to 10 ℃/min.
4. The recycling method according to any one of claims 1 to 3, wherein in the vapor deposition, the vapor phase is a mixed gas of a carbon source gas and an inert gas, and the content of the carbon source gas is 20 to 40 vol%.
5. The recycling method according to claim 4, wherein the carbon source gas is selected from one of methane, acetylene, ethylene, propylene and toluene.
6. The recycling method according to claim 1, wherein D50 of the silicon-carbon negative electrode recycled raw material is 10-15 μm.
7. The recycling method according to claim 1 or 2, wherein the silicon-carbon anode recycled raw material is obtained by the following steps:
and performing acid leaching on the failed cathode material, removing metals contained in the failed cathode material, and collecting filter residues to obtain a silicon-carbon cathode recycled raw material.
8. The recycling method according to claim 7, wherein the acid leaching is carried out at a concentration of 2 to 10mol/L, a solid-to-liquid ratio of 1g/1ml to 1g/10ml, a reaction temperature of 25 to 80 ℃, and the acid is selected from one of hydrochloric acid, sulfuric acid and nitric acid or a mixture thereof.
9. The recycling method according to claim 7, wherein after the acid leaching, a filtrate containing the metal is collected for recovering the positive electrode material.
10. The recycling method according to claim 7, wherein the spent anode material is obtained by the following process:
and (3) placing the negative pole piece of the lithium ion battery in water, and stirring or ultrasonically treating to peel off the invalid negative pole material coated on the copper foil.
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