CN114361637B - Method for separating electrode material and foil of lithium battery - Google Patents
Method for separating electrode material and foil of lithium battery Download PDFInfo
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- CN114361637B CN114361637B CN202210042729.XA CN202210042729A CN114361637B CN 114361637 B CN114361637 B CN 114361637B CN 202210042729 A CN202210042729 A CN 202210042729A CN 114361637 B CN114361637 B CN 114361637B
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Abstract
The invention provides a method for separating electrode materials from foil materials of a lithium battery, which comprises the following steps: mixing the positive electrode plate and/or the negative electrode plate with ball milling beads, vibrating, roasting in sections, and separating to obtain a positive electrode material and/or a negative electrode material and an aluminum foil and/or a copper foil. The invention adopts a simple method to effectively separate the anode/cathode material and the foil, can obtain electrode materials with different grades, has controllable aluminum and/or copper impurity content, and has the advantages of safe and environment-friendly whole recovery process, simple process, low energy consumption, good economy and the like.
Description
Technical Field
The invention relates to the field of treatment and recovery of waste materials of lithium ion batteries, in particular to a method for separating electrode materials from foil materials of lithium ion batteries.
Background
The lithium ion battery is widely applied to the fields of mobile intelligent terminals, small-sized electric equipment, power grid energy storage, electric automobiles and the like due to the advantages of high voltage, high energy density, good circularity and the like. Only 2019 is counted, and the number of lithium ion batteries produced in China is up to 157.2 hundred million. As the usage amount of the lithium ion battery increases, the retired amount of the lithium ion battery also increases. It is estimated that over the course of 2017-2030, over 1100 ten thousand tons of retired lithium ion batteries are expected to be produced worldwide.
A large amount of Li, ni, co, mn, fe, cu, al and other metals are used in the lithium ion battery, and the retired lithium ion battery is a rich valuable technical mineral. The recovery of the lithium ion battery has important economic and environmental significance.
And after the waste lithium ion batteries are subjected to pretreatment such as discharging, disassembling and the like, the anode/cathode material containing the foil is obtained. For the separation of anode/cathode materials and foil materials, there are mainly alkali solution dissolution method, organic solvent dissolution method, high temperature pyrolysis. The alkali solution dissolving method has serious heat release, uneasy control of reaction, hydrogen generation, serious corrosion to equipment and high treatment cost. The organic solvent dissolving method has serious solvent volatilization, poor cyclic utilization and toxicity. High-temperature pyrolysis, high energy consumption, and high production rate of fluorine-containing harmful waste gas, and is easy to cause secondary pollution.
Disclosure of Invention
In order to solve the problems of the prior art in separating the anode/cathode materials from the foil, the invention provides a method for separating the electrode materials from the foil of a lithium battery.
In order to achieve the above object, an embodiment of the present invention provides a method for separating an electrode material from a foil of a lithium battery, the method comprising the steps of:
s1: mixing a first-stage positive electrode plate and/or a second-stage negative electrode plate obtained after disassembling the retired lithium battery with ball milling beads, roasting and vibrating to obtain a first-stage recycled positive electrode material and/or a second-stage positive electrode plate and/or a second-stage negative electrode plate respectively;
s2: mixing the secondary positive electrode plate and/or the negative electrode plate with ball milling beads, roasting and vibrating to obtain a secondary recovered positive electrode material and/or a negative electrode material and a tertiary positive electrode plate and/or a negative electrode plate respectively;
s3: mixing the three-stage positive electrode plate and/or the negative electrode plate with ball milling beads, roasting and vibrating to obtain three-stage recovered positive electrode materials and/or negative electrode materials and four-stage positive electrode plates and/or negative electrode plates respectively;
s4: mixing the four-stage positive electrode plate and/or the negative electrode plate with ball milling beads, roasting and vibrating to obtain four-stage recovered positive electrode materials and/or negative electrode materials and waste aluminum foils and/or copper foils respectively.
Further, in the step S1, the mass ratio of the first-stage positive electrode plate and/or the negative electrode plate to the ball-milling beads is 1:1 to 10.
Further, in the step S1, the roasting temperature is 100-150 ℃, the roasting time is 2-30min, and the vibration frequency of ball milling beads is 20-300 times/min.
Further, in the step S2, the mass ratio of the secondary positive electrode plate and/or the secondary negative electrode plate to the ball-milling beads is 1:5 to 12.
Further, in the step S2, the roasting temperature is 150-200 ℃, the vibration frequency of ball milling beads is 60-300 times/min, and the roasting time is 5-60min.
Further, in the step S3, the mass ratio of the three-stage positive electrode piece and/or the three-stage negative electrode piece to the ball-milling beads is 1:10 to 20.
Further, in the step S3, the roasting temperature is 200-250 ℃, the vibration frequency of ball milling beads is 20-200 times/min, and the roasting time is 2-40min.
Further, in the step S4, the mass ratio of the mixture of the four-stage positive electrode plate and/or the negative electrode plate and the ball-milling beads is 1:5 to 25.
Further, in the step S4, the roasting temperature is 250-350 ℃, the vibration frequency of ball milling beads is 30-200 times/min, and the roasting time is 1-20min.
Further, the ball-milling bead material in the step S1 is one or more of zirconia, alumina, polyurethane and stainless steel, the ball-milling bead material in the step S2 is one or more of zirconia, alumina and stainless steel, the ball-milling bead material in the step S3 is one or two of zirconia and alumina, and the ball-milling bead material in the step S4 is zirconia.
The invention mixes the positive pole piece and/or the negative pole piece obtained after disassembling the retired lithium battery with ball-milling beads, then performs roasting in sections and vibrates at the same time, so that the ball-milling beads bounce to fully contact with the positive pole piece and/or the negative pole piece, and the positive pole material and/or the negative pole material are separated from the aluminum foil and/or the copper foil by utilizing the mechanical force generated when the ball-milling beads bounce to fully contact with the positive pole piece and/or the negative pole piece.
The scheme of the invention has the following beneficial effects:
1) The separation method of the scheme of the invention is a method of mixing the positive pole piece and/or the negative pole piece with ball milling beads, vibrating and roasting in sections, and obtaining reclaimed materials of different grades in sections: the aluminum content in the first-stage and second-stage recovered positive electrode materials is 0; the copper content in the first-stage and second-stage recovered anode materials is 0; the aluminum content in the three-stage recovered positive electrode material is 10ppm, the copper content in the three-stage recovered negative electrode material is 10ppm, the aluminum content in the four-stage recovered positive electrode material is 100ppm, and the copper content in the four-stage recovered negative electrode material is 30ppm;
2) The invention mixes the positive pole piece and/or the negative pole piece with ball milling beads, vibrates and roasting in sections, reduces the treatment cost, and simultaneously avoids the harm to the environment and human body caused by the existing alkali liquor, organic solvent and high-temperature pyrolysis technology.
Drawings
Fig. 1 is a process flow diagram of a method for separating positive/negative electrode materials from foil materials of a lithium battery according to an embodiment of the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention in which the various raw materials, reagents, instruments, equipment, etc. used in the present invention may be purchased commercially or may be prepared by existing methods unless otherwise specifically indicated.
The invention provides a method for separating electrode materials from foil materials of a lithium battery aiming at the existing problems.
As shown in fig. 1, an embodiment of the present invention provides a process flow diagram of a method for separating electrode materials from foil materials of a lithium battery.
Example 1
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:10, mixing, roasting for 30min at the temperature of 150 ℃ in a first interval, and vibrating at the frequency of 300 times/min to separate the anode material from the copper foil, so as to obtain a first-stage recovered anode material and a second-stage anode piece;
the secondary negative electrode piece and zirconia ball milling beads are mixed according to the mass ratio of 1:12, mixing, roasting at 200 ℃ for 60min in a second interval, and vibrating at 200 times/min to separate the anode material from the copper foil to obtain a secondary recovered anode material and a tertiary anode piece;
the three-level negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:20, then roasting for 40min at the temperature of 250 ℃ in a third interval, vibrating at the same time according to the frequency of 200 times/min, and separating the cathode material from the copper foil to obtain a three-level recovered cathode material and a four-level cathode pole piece;
the four-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:25, then roasting for 20min at the temperature of 350 ℃ in a fourth interval, vibrating for 200 times/min, and separating the anode material from the copper foil to obtain a four-stage recovered anode material and waste copper foil.
TABLE 1 copper content in recovered negative electrode material obtained in example 1 of the present invention
Example 2
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a primary positive/negative electrode mixed pole piece with zirconia or stainless steel ball milling beads according to a mass ratio of 1:5, mixing, roasting for 15min at the temperature of 125 ℃ in a first interval, and vibrating at the frequency of 150 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively to obtain a primary anode/cathode mixed material and a secondary anode/cathode mixed pole piece;
mixing a secondary anode/cathode mixed pole piece with zirconia and stainless steel ball milling beads according to a mass ratio of 1:10, then roasting for 30min at the temperature of 175 ℃ in a second interval, and vibrating at the frequency of 150 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively, so as to obtain a secondary anode/cathode mixed material and a tertiary anode/cathode mixed pole piece;
mixing a three-stage positive/negative electrode plate with zirconia and alumina ball-milling beads according to a mass ratio of 1:15, then roasting for 20min at 225 ℃ in a third interval, and vibrating at the same time according to the frequency of 100 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively, so as to obtain a three-level anode/cathode mixed material and a four-level anode/cathode mixed pole piece;
mixing a four-stage positive/negative electrode mixed pole piece with zirconia and alumina ball milling beads according to a mass ratio of 1:20, then roasting for 10min at the temperature of 275 ℃ in a fourth interval, and vibrating at the frequency of 100 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively, so as to obtain a four-stage anode/cathode mixed material and a waste anode/cathode mixed pole piece;
example 3
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage positive electrode plate, zirconia and polyurethane ball-milling beads are mixed according to the mass ratio of 1:1, mixing, roasting for 7.5min at the temperature of 100 ℃ in a first interval, and vibrating according to the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a first-stage recovered anode material and a second-stage anode plate;
the secondary positive electrode plate and the alumina ball-milling beads are mixed according to the mass ratio of 1:5, mixing, roasting for 15min at the temperature of 150 ℃ in a second interval, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a secondary recovered anode material and a tertiary anode plate;
mixing the three-level positive electrode plate with zirconia or alumina ball-milling beads according to the mass ratio of 1:10, mixing, roasting for 10min at the temperature of 200 ℃ in a third interval, and vibrating at the frequency of 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a three-level recovered anode material and a four-level anode sheet;
ball milling the four-stage positive electrode plate and zirconia ball according to the mass ratio of 1:15, then roasting for 5min at the temperature of 250 ℃ in a fourth interval, and simultaneously vibrating according to the frequency of 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a four-stage recovered anode material and waste aluminum foil;
TABLE 3 recovery of aluminum content in cathode materials obtained in example 3 of the present invention
TABLE 4 recovery of recovered cathode materials obtained in example 3 of the present invention
Comparative example 1
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:10, mixing, roasting for 30min at the temperature of 150 ℃ in a first interval, and vibrating at the frequency of 300 times/min to separate the anode material from the copper foil, so as to obtain a first-stage recovered anode material and a second-stage anode piece;
the secondary negative electrode piece and zirconia ball milling beads are mixed according to the mass ratio of 1:12, mixing, roasting for 60min at the temperature of 150 ℃ in a first interval, and vibrating at the frequency of 200 times/min to separate the anode material from the copper foil, so as to obtain a secondary recovered anode material and a tertiary anode piece;
the three-level negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:20, then roasting for 40min at the temperature of 150 ℃ in a first interval, vibrating at the same time according to the frequency of 200 times/min, and separating the cathode material from the copper foil to obtain a three-level recovered cathode material and a four-level cathode pole piece;
the four-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:25, then roasting for 20min at the temperature of 150 ℃ in the first interval, vibrating for 200 times/min, and separating the anode material from the copper foil to obtain a four-stage recovered anode material and waste copper foil.
TABLE 5 copper content in recovered negative electrode material obtained in comparative example 1 of the present invention
TABLE 6 recovery of recovered negative electrode material obtained in comparative example 1 of the present invention
Comparative example 2
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:10, mixing, roasting for 30min at the temperature of 150 ℃ in a first interval, and vibrating at the frequency of 300 times/min to separate the anode material from the copper foil, so as to obtain a first-stage recovered anode material and a second-stage anode piece;
the secondary negative electrode piece and zirconia ball milling beads are mixed according to the mass ratio of 1:12, mixing, roasting at 200 ℃ for 60min in a second interval, and vibrating at 200 times/min to separate the anode material from the copper foil to obtain a secondary recovered anode material and a tertiary anode piece;
the three-level negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:20, then roasting for 40min at the temperature of 250 ℃ in a third interval, vibrating at the same time according to the frequency of 200 times/min, and separating the cathode material from the copper foil to obtain a three-level recovered cathode material and a four-level cathode pole piece;
the four-stage negative electrode plate and zirconia ball milling beads are mixed according to the mass ratio of 1:25, then roasting for 20min at the temperature of 250 ℃ in a third interval, vibrating for 200 times/min, and separating the anode material from the copper foil to obtain a four-stage recovered anode material and waste copper foil.
TABLE 7 comparative example 2 of the present invention obtaining copper content in recovered negative electrode material
TABLE 8 recovery of recovered negative electrode Material obtained in comparative example 2 of the present invention
Comparative example 3
And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage positive electrode plate, zirconia and polyurethane ball-milling beads are mixed according to the mass ratio of 1:1, mixing, roasting for 7.5min at the temperature of 100 ℃ in a first interval, and vibrating according to the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a first-stage recovered anode material and a second-stage anode plate;
the secondary positive electrode plate and the alumina ball-milling beads are mixed according to the mass ratio of 1:5, mixing, roasting for 15min at the temperature of 100 ℃ in the first interval, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a secondary recovered anode material and a tertiary anode plate;
mixing the three-level positive electrode plate with zirconia or alumina ball-milling beads according to the mass ratio of 1:10, mixing, roasting for 10min at the temperature of 100 ℃ in a first interval, and vibrating for 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a three-level recovered anode material and a four-level anode sheet;
ball milling the four-stage positive electrode plate and zirconia ball according to the mass ratio of 1:15, mixing, roasting for 5min at the temperature of 100 ℃ in a first interval, and simultaneously vibrating according to the frequency of 50 times/min to separate the anode material from the aluminum foil, so as to obtain a four-stage recovered anode material and waste aluminum foil;
TABLE 9 comparative example 3 of the present invention to obtain aluminum content in recovered cathode material
TABLE 10 recovery of recovered cathode materials obtained in comparative example 3 of the present invention
Comparative example 4
This example is a control example. And (3) taking the waste lithium ion battery, cleaning the outer shell of the waste lithium ion battery, and completely drying the waste lithium ion battery at 20 ℃. Disassembling the dried waste lithium ion battery in protective atmosphere to obtain a shell and a battery core pack, and cutting the battery core pack into pieces at will to obtain a mixed piece containing the anode/cathode material and the foil.
The first-stage positive electrode plate, zirconia and polyurethane ball-milling beads are mixed according to the mass ratio of 1:1, mixing, roasting for 7.5min at the temperature of 100 ℃ in a first interval, and vibrating according to the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a first-stage recovered anode material and a second-stage anode plate;
the secondary positive electrode plate and the alumina ball-milling beads are mixed according to the mass ratio of 1:5, mixing, roasting for 15min at the temperature of 150 ℃ in a second interval, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil, so as to obtain a secondary recovered anode material and a tertiary anode plate;
mixing the three-level positive electrode plate with zirconia or alumina ball-milling beads according to the mass ratio of 1:10, mixing, roasting for 10min at the temperature of 200 ℃ in a third interval, and vibrating at the frequency of 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a three-level recovered anode material and a four-level anode sheet;
ball milling the four-stage positive electrode plate and zirconia ball according to the mass ratio of 1:15, then roasting for 5min at the temperature of 200 ℃ in a third interval, and simultaneously vibrating according to the frequency of 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a four-stage recovered anode material and waste aluminum foil;
TABLE 11 comparative example 4 recovery of aluminum content in cathode materials according to the present invention
TABLE 12 recovery of recovered cathode materials obtained in comparative example 4 of the present invention
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The separation method of the lithium battery electrode material and the foil is characterized by comprising the following steps:
s1: mixing a first-stage positive electrode plate and/or a first-stage negative electrode plate obtained after disassembling the retired lithium battery with ball milling beads, roasting and vibrating simultaneously to obtain a first-stage recycled positive electrode material and/or a first-stage recycled negative electrode material, a second-stage positive electrode plate and/or a second-stage negative electrode plate respectively;
s2: mixing the secondary positive electrode plate and/or the secondary negative electrode plate with ball milling beads, roasting and vibrating simultaneously to obtain secondary recycled positive electrode materials and/or secondary recycled negative electrode materials, tertiary positive electrode plates and/or tertiary negative electrode plates respectively;
s3: mixing the three-level positive electrode plate and/or the three-level negative electrode plate with ball milling beads, roasting and vibrating simultaneously to obtain three-level recycled positive electrode materials and/or three-level recycled negative electrode materials, four-level positive electrode plates and/or four-level negative electrode plates respectively;
s4: mixing the four-stage positive electrode plate and/or four-stage negative electrode plate with ball milling beads, roasting and vibrating simultaneously to obtain four-stage recovered positive electrode materials and/or four-stage recovered negative electrode materials and waste aluminum foils and/or copper foils respectively;
the roasting temperature in the step S1 is 100-150 ℃; the roasting temperature in the step S2 is 150-200 ℃; the roasting temperature in the step S3 is 200-250 ℃; the roasting temperature in the step S4 is 250-350 ℃; wherein the roasting temperatures of S1 to S4 are different;
in the step S1, the mass ratio of the first-stage positive electrode plate and/or the first-stage negative electrode plate to the ball-milling beads is 1: 1-10; in the step S2, the mass ratio of the secondary positive electrode plate and/or the secondary negative electrode plate to the ball-milling beads is 1: 5-12; in the step S3, the mass ratio of the three-level positive electrode plate and/or the three-level negative electrode plate to the ball-milling beads is 1: 10-20 parts of a base; in the step S4, the mass ratio of the mixture of the four-stage positive electrode plate and/or the four-stage negative electrode plate and the ball milling beads is 1: 5-25; the mass ratio of the first-stage positive electrode plate and/or the first-stage negative electrode plate to the ball-milling beads in the step S1, the mass ratio of the second-stage positive electrode plate and/or the second-stage negative electrode plate to the ball-milling beads in the step S2, the mass ratio of the third-stage positive electrode plate and/or the third-stage negative electrode plate to the ball-milling beads in the step S3, and the mass ratio of the fourth-stage positive electrode plate and/or the fourth-stage negative electrode plate to the ball-milling beads in the step S4 are sequentially increased.
2. The separation method according to claim 1, wherein the roasting time in the step S1 is 2-30min, and the vibration frequency of the ball mill beads is 20-300 times/min.
3. The separation method according to claim 1, wherein the ball milling beads in the step S2 have a vibration frequency of 60 to 300 times/min and a calcination time of 5 to 60min.
4. The separation method according to claim 1, wherein the ball milling beads in the step S3 have a vibration frequency of 20 to 200 times/min and a calcination time of 2 to 40min.
5. The separation method according to claim 1, wherein the ball milling beads in step S4 have a vibration frequency of 30 to 200 times/min and a calcination time of 1 to 20min.
6. The separation method according to claim 1, wherein the ball-milling beads in the step S1 are one or more of zirconia, alumina, polyurethane and stainless steel, the ball-milling beads in the step S2 are one or more of zirconia, alumina and stainless steel, the ball-milling beads in the step S3 are one or two of zirconia and alumina, and the ball-milling beads in the step S4 are zirconia.
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| CN110661055A (en) * | 2019-10-14 | 2020-01-07 | 赣州有色冶金研究所 | Method for efficiently stripping waste lithium ion battery material |
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