CN115241555A - Method for recycling waste battery negative electrode graphite - Google Patents
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- CN115241555A CN115241555A CN202210893005.6A CN202210893005A CN115241555A CN 115241555 A CN115241555 A CN 115241555A CN 202210893005 A CN202210893005 A CN 202210893005A CN 115241555 A CN115241555 A CN 115241555A
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- 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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a method for recycling waste battery negative electrode graphite, and relates to the field of lithium ion battery material recycling. According to the invention, the lithium carbonate fine powder and graphite are uniformly mixed to obtain the preliminary pre-lithiated graphite, and then the lithium atoms in the waste graphite are activated through calcination to realize double pre-lithiation. Lithium oxide generated in the process of high-temperature calcination of lithium carbonate becomes a fluxing agent, and the small-particle-size graphite is gathered together by utilizing the surface tension generated when the lithium oxide is cooled and shrunk in the slow cooling process, so that necessary conditions are provided for increasing the graphite particle size and reducing the specific surface area. And finally, coating the surface of the graphite by adopting a carbon source for heat treatment, thereby realizing high-value utilization of the cathode material of the retired lithium ion battery. According to the method, double pre-lithium, high-temperature calcination and carbon coating processes are organically integrated, the internal structure and the surface coating layer of the damaged graphite cathode material are simultaneously repaired, the first charge-discharge efficiency of the obtained regenerated graphite material is obviously improved, and large-scale preparation and production are facilitated.
Description
Technical Field
The invention relates to the field of lithium ion battery material recovery, in particular to a method for recovering and regenerating waste battery negative electrode graphite.
Background
In recent years, energy and environmental problems are increasingly highlighted, and the development of novel energy has become a great trend of energy strategies. The electrochemical energy storage has the advantages of high energy storage efficiency, less dependence on external environment, relatively mature technology, wide application range and the like, and is widely applied all over the world. Due to the strong support of the country, new energy automobiles are rapidly developed in China. However, as the heart of the new energy automobile, the service life of the power battery is only 4-6 years. At present, the power batteries on the first new energy automobiles in China are already in full service in the 'retirement period', and the accumulated retirement amount of the domestic power lithium batteries is estimated to be close to 80 ten thousand tons by 2025 years. The power lithium battery contains a plurality of metal elements and organic substances, and serious resource waste and environmental pollution can be caused if the power lithium battery cannot be effectively treated after being retired. Based on this, a series of policy specifications are provided in China to guide the healthy development of the lithium battery recycling industry, and relevant research and industrialization promotion are highly regarded.
At present, the material recovery of lithium batteries mainly focuses on positive active materials such as lithium, cobalt, nickel, manganese and the like and valuable metals such as metal current collectors aluminum, copper and the like. Because the negative electrode graphite has wide sources and low recycling added value, the recycling technology and the industrial development aiming at the negative electrode are still in the initial stage. As an important strategic resource of China, the graphite has limited reserves and has very important economic value. With the annual increase of the retirement amount of power batteries, the recycling of retired graphite is urgent.
At present, some recycling manufacturers can recycle waste graphite to obtain a graphite material as a lithium ion battery negative electrode material, and the first coulombic efficiency of the recycled graphite negative electrode material is lower than that of a fresh graphite negative electrode material in actual application. The reason for this is that the ex-service graphite has structural damage of different degrees on the bulk phase and the surface after long-term circulation, and therefore needs to be repaired by a structural regeneration method. Chinese patent CN 109524736A discloses a method for recovering graphite from waste batteries and its use: the method comprises the steps of taking graphite slag obtained by recycling waste batteries as a recycling raw material, carrying out acid washing to obtain primarily purified graphite, then placing the primarily purified graphite in a reaction kettle for oxidation to obtain secondarily purified graphite, and finally carrying out coating carbonization on the secondarily purified graphite by using asphalt to obtain a regenerated graphite material. The carbon source is adopted to coat the graphite surface, so that the surface electron/ion transmission channel is improved and reconstructed to a certain extent, and the generation of SEI is reduced. But the restoration of crystal structure defects in the retired graphite cannot be effectively realized only through surface coating, and the graphitization degree in the graphite is not effectively improved. Meanwhile, the acid washing removes the lithium in the activated cathode powder to a certain extent, and ignores the positive effect of the lithium in the repair process of the retired graphite. Chinese patent CN 111924836A discloses a method for recycling graphite from the negative electrode of a decommissioned lithium ion battery: the ex-service graphite is calcined to convert organic components into amorphous carbon, and the pre-lithiation of the ex-service graphite is realized by utilizing the migration characteristic of lithium atoms at different temperatures. On the one hand, however, the pre-lithiation only by means of a small amount of lithium remaining in the retired graphite cannot meet the requirement of subsequent use. On the other hand, the solvated lithium ions are co-inserted into the graphite layer in the earlier cycle process of the battery to cause the damage of the crystal structure, and the negative electrode particles are easy to damage in the later process of separating the current collector from the active material, so that the obtained retired graphite has smaller particle size, thereby causing the increase of the contact area between the regenerated graphite and the electrolyte, the increase of side reactions and finally the reduction of the first charge-discharge efficiency.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for recycling waste battery negative electrode graphite. Firstly, uniformly mixing lithium carbonate fine powder and graphite to carry out pre-lithiation, and then activating lithium in the SEI of the original waste graphite at high temperature and re-applying the lithium in the graphite to realize double pre-lithiation. In addition, lithium carbonate generates a small amount of lithium oxide at high temperature to serve as a fluxing agent, and the surface tension generated by the lithium oxide in the slow cooling process can gather crushed small-particle-size graphite together, thereby creating necessary conditions for increasing the graphite particle size and reducing the specific surface area. And finally, coating the surface of the graphite by adopting a carbon source for heat treatment, and finally realizing high-value utilization of the retired lithium ion battery cathode material. According to the method, double pre-lithium, high-temperature calcination and carbon coating processes are organically integrated, the internal structure and the surface structure of the damaged graphite cathode material are simultaneously repaired, and the obtained regenerated graphite material is good in consistency and easy to prepare and produce on a large scale.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) Taking graphite mixed materials obtained by disassembling retired batteries from different sources as raw materials, and separating retired graphite powder from copper foil through current collector stripping pretreatment;
(2) Screening and grading the retired graphite powder obtained in the step (1) through an electric vibrating screen machine, and recovering a middle grain size sample obtained through grading to obtain a graphite crude product;
(3) Uniformly mixing the obtained graphite coarse product with lithium carbonate fine powder to obtain pre-lithiated graphite;
(4) Calcining in an inert atmosphere, and cooling to room temperature after the calcination is finished to obtain dual pre-lithiated graphite;
(5) And (4) mixing a carbon source material with the double pre-lithiated graphite obtained in the step (4), then carrying out carbon coating, and then carbonizing the coating in a rotary furnace to obtain the regenerated graphite cathode material.
Preferably, the current collector stripping pretreatment in the step (1) adopts one or more of crushing-gas separation, calcination and solvent leaching.
Preferably, the screen of the electric vibrating screen machine in the step (2) is 300-2500 meshes.
Preferably, the particle size of the graphite crude product in the step (2) is 5-50 microns.
Preferably, the inert atmosphere in step (4) and step (5) is one or more of nitrogen, argon, etc.
Preferably, the particle size of the lithium carbonate fine powder in the step (3) is 100 nm-1000 nm, and the addition amount of the lithium carbonate fine powder is 0.5% -10% of the mass of the graphite coarse product.
Preferably, the calcination process in the step (4) is firstly heated to 900-1200 ℃ at a heating rate of 0.5-10 ℃/min, the calcination temperature is maintained for 1-12 h, and then the temperature is slowly reduced to the room temperature at 0.5-10 ℃/min.
Preferably, the carbon source in the step (5) is one or more of coal pitch, petroleum pitch, emulsified asphalt, citric acid, phenolic resin, chitosan, sucrose, polyvinyl alcohol, polyallyl alcohol or polyaniline, and the addition amount of the carbon source is 0.1-5% of the mass of the secondary-treated graphite.
Preferably, the rotary kiln in the step (5) has a rotation speed of 25-150 r/min, and the calcination process in the rotary kiln is completed by two stages: the temperature of the first stage of calcination process is 300-600 ℃, and the heat preservation time is 0.5-2.5h; the second-stage calcination temperature is 900-1300 ℃, and the calcination time is 0.5-12 h; the heating rate is 1-10 deg.C/min during the calcination process.
Preferably, the material mixing manner in step (3) and step (5) is one or more of mechanical mixing, pneumatic mixing and impulse mixing.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, on one hand, lithium carbonate fine powder and graphite are uniformly dispersed in a mixing manner for pre-lithiation, and on the other hand, lithium in SEI (solid electrolyte interphase) of waste graphite is activated and re-applied to the graphite according to the migration characteristics of lithium atoms at different temperatures, so that double pre-lithiation is realized;
(2) In the method, part of lithium oxide generated in the calcining process of lithium carbonate becomes a fluxing agent, and crushed graphite with small particle size is gathered together by virtue of surface tension generated when the lithium oxide shrinks in the slow cooling process, so that necessary conditions are provided for increasing the graphite particle size and reducing the specific surface area;
(3) The method can effectively repair the internal defects of the graphite in the two high-temperature heat treatment processes, and the graphitization degree of the graphite can also be effectively improved;
(4) According to the method, the carbon source is adopted to coat the surface of the graphite, so that the surface electron/ion transmission channel of the graphite can be effectively improved and reconstructed, the generation of SEI (solid electrolyte interphase) is reduced, and the high-value utilization of the cathode material of the retired lithium ion battery is finally realized;
(5) The preparation process is simple and feasible, and is easy to realize large-scale production. The whole double pre-lithiation process is very simple, the prepared regenerated negative electrode material has good consistency, the first charge-discharge efficiency of the regenerated graphite can be effectively improved, and the method is worthy of market popularization.
Drawings
Fig. 1 is a process flow diagram of the method for recycling the graphite of the negative electrode of the waste battery.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more clearly and fully with reference to the accompanying description and preferred embodiments, but the scope of the invention is not limited solely to the specific embodiments described below.
Example 1
The method for recycling the graphite of the negative electrode of the waste battery comprises the following steps:
(1) Taking a negative pole piece obtained by disassembling a waste lithium ion battery of company A as a raw material, respectively processing the raw material by a hammering type crusher and a universal crusher for 10min and 15min, respectively, and screening the obtained crushed material to separate the retired graphite from the copper foil to obtain a graphite crude product.
(2) And (2) fully performing ball milling dispersion on the nano lithium carbonate powder (200 nm) and the crude graphite product in a planetary ball mill according to the mass ratio of 1.
(3) And calcining the pre-lithiated graphite, namely firstly raising the temperature to 500 ℃ at the heating rate of 5 ℃/min, then slowly raising the temperature to 1100 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 5h, and then slowly lowering the temperature to 50 ℃ at 1 ℃/min to obtain the dual pre-lithiated graphite.
(4) The preparation method comprises the following steps of ball-milling and uniformly mixing coal tar pitch and double pre-lithiated graphite according to a mass ratio of 1.
Example 2
The method for recycling the graphite of the negative electrode of the waste battery comprises the following steps:
(1) Taking a negative pole piece obtained by disassembling a waste lithium ion battery of company A as a raw material, weighing 1 part of the recovered negative pole piece, adding 9 parts of pure water into the negative pole piece, mechanically stirring the mixture for 3 hours at the rotating speed of 300r/min at the temperature of 60 ℃ to leach, adding the leached mixed material into an automatic vibrating screen machine after drying, and grading to obtain a crude graphite product.
(2) And (2) fully stirring and dispersing the nano-scale lithium carbonate powder (200 nm) and the graphite coarse product in a mixer according to the mass ratio of 1.
(3) Calcining the pre-lithiated graphite, firstly heating to 500 ℃ at a heating rate of 5 ℃/min, then slowly heating to 950 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 12h, and then slowly cooling to 50 ℃ at 2 ℃/min to obtain the dual pre-lithiated graphite.
(4) Uniformly mixing phenolic resin and double pre-lithiated graphite according to a mass ratio of 3.
Example 3
The method for recycling the graphite of the negative electrode of the waste battery comprises the following steps:
(1) Taking a negative pole piece obtained by disassembling a waste lithium ion battery of company A as a raw material, respectively processing the raw material by a hammering type crusher and a universal crusher for 15min and 20min, respectively, and screening the obtained crushed material to separate the retired graphite from the copper foil to obtain a graphite crude product.
(2) Fully stirring and dispersing nano lithium carbonate powder (200 nm) and a graphite crude product in a ball mill according to a mass ratio of 1.
(3) And calcining the pre-lithiated graphite, namely firstly raising the temperature to 600 ℃ at the heating rate of 5 ℃/min, then slowly raising the temperature to 1050 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 9h, and then slowly lowering the temperature to 50 ℃ at 1 ℃/min to obtain the dual pre-lithiated graphite.
(4) Uniformly mixing petroleum asphalt and the double pre-lithiated graphite in a mixer according to the mass ratio of 1.
Example 4
The method for recycling the graphite of the negative electrode of the waste battery comprises the following steps:
(1) Taking a negative pole piece obtained by disassembling a waste lithium ion battery of company A as a raw material, weighing 1 part of the recovered negative pole piece, adding 8 parts of pure water into the negative pole piece, mechanically stirring the mixture at the rotating speed of 300r/min at 70 ℃ for 1.5 hours for leaching, adding the leached and mixed material into an automatic vibrating screen machine for grading to obtain a crude graphite product.
(2) And (3) fully stirring and dispersing the nano lithium carbonate powder (200 nm) and the crude graphite product in a mixer according to the mass ratio of 1.
(3) And calcining the pre-lithiated graphite, namely firstly raising the temperature to 600 ℃ at the heating rate of 5 ℃/min, then slowly raising the temperature to 1100 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 12h, and then slowly lowering the temperature to 50 ℃ at the temperature of 2 ℃/min to obtain the dual pre-lithiated graphite.
(4) Uniformly mixing citric acid and double pre-lithiated graphite according to a mass ratio of 3.
Example 5
The method for recycling the graphite of the negative electrode of the waste battery comprises the following steps:
(1) Taking a negative pole piece obtained by disassembling a waste lithium ion battery of company A as a raw material, respectively processing the raw material by a hammering type crusher and a universal crusher for 8min and 15min, and screening the obtained crushed material to separate the decommissioned graphite from the copper foil to obtain a crude graphite product.
(2) And (3) fully stirring and dispersing the nano lithium carbonate powder (200 nm) and the graphite crude product in a ball mill according to the mass ratio of 1.
(3) And calcining the pre-lithiated graphite, namely firstly raising the temperature to 500 ℃ at the temperature rise rate of 5 ℃/min, then raising the temperature to 1200 ℃ at the temperature rise rate of 1 ℃/min, keeping the temperature for 5 hours, and then reducing the temperature to 50 ℃ at 1 ℃/min to obtain the dual pre-lithiated graphite.
(4) Uniformly mixing sucrose and the double pre-lithiated graphite in a mixer according to a mass ratio of 1.
Comparative example 1
And in the comparative example, the negative pole piece obtained by disassembling the waste lithium ion battery of company A is taken as a raw material, the negative pole piece is treated by a hammering type crusher and a universal crusher respectively for 10min and 15min, and the obtained crushed material is screened to separate the retired graphite from the copper foil to obtain a crude graphite product.
Calcining the crude graphite product, firstly raising the temperature to 500 ℃ at the heating rate of 5 ℃/min to convert organic components in the retired graphite into amorphous carbon, then raising the temperature to 1100 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 5h, and then reducing the temperature to 50 ℃ at 1 ℃/min to obtain the pre-lithiated graphite.
And then ball-milling and uniformly mixing the coal pitch and the pre-lithiated graphite according to the mass ratio of 1.
Comparative examples 2 to 5
The difference from examples 2 to 5 is only that prelithiation in which fine lithium carbonate powder and crude graphite were uniformly dispersed was not performed (the procedure was the same as in comparative example 1).
The following table shows the particle size test results and electrochemical performance of the double prelithiation regenerated graphite prepared in examples 1 to 5 and the single prelithiation graphite negative electrode material prepared in comparative examples 1 to 5.
As can be seen from the above table, the particle sizes of the dual pre-lithiation regenerated graphite prepared in the embodiment of the present invention are all larger than those of the graphite material prepared in the comparative example, and the corresponding first discharge specific capacity and first charge-discharge efficiency of the dual pre-lithiation regenerated graphite are also significantly higher than those of the single pre-lithiation graphite negative electrode material prepared in the comparative example.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for recycling waste battery negative electrode graphite is characterized by comprising the following steps:
(1) Taking a negative plate obtained by disassembling a retired battery as a raw material, and separating retired graphite powder from copper foil through current collector stripping pretreatment;
(2) Screening and grading the retired graphite powder obtained in the step (1) through an electric vibrating screen machine, and recovering a middle grain size sample obtained through grading to obtain a graphite crude product;
(3) Uniformly mixing the obtained graphite coarse product with lithium carbonate fine powder to obtain pre-lithiated graphite;
(4) Calcining the pre-lithiated graphite in an inert atmosphere, and cooling to room temperature after the calcination is finished to obtain dual pre-lithiated graphite;
(5) And (5) mixing a carbon source material with the double pre-lithiated graphite obtained in the step (4), then carrying out carbon coating, and then carbonizing the coating in an inert atmosphere of a rotary furnace to obtain the regenerated graphite cathode material.
2. The method for recycling and regenerating the graphite of the negative electrode of the waste battery as claimed in claim 1, is characterized in that: in the step (1), the current collector stripping pretreatment adopts one or more of crushing-gas separation, calcination and solvent leaching.
3. The method for recycling and regenerating the graphite of the negative electrode of the waste battery as claimed in claim 1, is characterized in that: the screen mesh of the electric vibrating screen machine in the step (2) is 300-2500 meshes; the particle size of the graphite coarse product is 5-50 microns.
4. The method for recycling and regenerating the waste battery negative electrode graphite as claimed in claim 1, is characterized in that: the granularity of the lithium carbonate fine powder in the step (3) is 100-1000 nm, and the addition amount of the lithium carbonate fine powder is 0.5-10% of the mass amount of the graphite coarse product.
5. The method for recycling and regenerating the graphite of the negative electrode of the waste battery as claimed in claim 1, is characterized in that: in the calcining process in the step (4), the temperature is raised to 900-1200 ℃ at the heating rate of 0.5-10 ℃/min, the calcining temperature is maintained for 1-12 h, and then the temperature is reduced to the room temperature at the speed of 0.5-10 ℃/min.
6. The method for recycling and regenerating the waste battery negative electrode graphite as claimed in claim 1, is characterized in that: and (3) neutralizing the inert atmosphere in the step (5) by adopting one or more of nitrogen and argon.
7. The method for recycling and regenerating the waste battery negative electrode graphite as claimed in claim 1, is characterized in that: the carbon source material in the step (5) is one or more of coal pitch, petroleum pitch, emulsified asphalt, citric acid, phenolic resin, chitosan, sucrose, polyvinyl alcohol, polyallyl alcohol or polyaniline, and the adding amount of the carbon source material is 0.1-5% of the mass of the double pre-lithiated graphite.
8. The method for recycling and regenerating the graphite of the negative electrode of the waste battery as claimed in claim 1, is characterized in that: the rotating speed of the rotary furnace in the step (5) is 25-150 r/min, and the calcining process in the rotary furnace is completed by two stages: the calcination temperature of the first section is 300-600 ℃, and the heat preservation time is 0.5-2.5h; the second-stage calcination temperature is 900-1300 ℃, and the calcination time is 0.5-12 h; the heating rate is 1-10 deg.C/min during the calcination process.
9. The method for recycling and regenerating the waste battery negative electrode graphite as claimed in claim 1, is characterized in that: the material mixing mode in the step (3) and the step (5) is one or more of mechanical mixing, pneumatic mixing and impulse mixing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117712542A (en) * | 2023-12-27 | 2024-03-15 | 浙江中创资源循环利用创新中心有限公司 | Regeneration method of negative electrode material of invalid lithium ion battery |
| CN117766761A (en) * | 2023-12-29 | 2024-03-26 | 百色鑫茂新材料技术有限公司 | Regeneration process of graphite negative electrode of lithium ion battery for vehicle and regenerated graphite negative electrode |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117712542A (en) * | 2023-12-27 | 2024-03-15 | 浙江中创资源循环利用创新中心有限公司 | Regeneration method of negative electrode material of invalid lithium ion battery |
| CN117766761A (en) * | 2023-12-29 | 2024-03-26 | 百色鑫茂新材料技术有限公司 | Regeneration process of graphite negative electrode of lithium ion battery for vehicle and regenerated graphite negative electrode |
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