CN113193255B - New energy battery material recycling and regenerating treatment method - Google Patents
New energy battery material recycling and regenerating treatment method Download PDFInfo
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- CN113193255B CN113193255B CN202110401208.4A CN202110401208A CN113193255B CN 113193255 B CN113193255 B CN 113193255B CN 202110401208 A CN202110401208 A CN 202110401208A CN 113193255 B CN113193255 B CN 113193255B
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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 discloses a new energy battery material recycling and regenerating treatment method, and belongs to the technical field of battery recycling. The processing method comprises the following steps: crushing battery pole pieces of waste batteries, and heating and dipping to obtain treatment slurry; carrying out solid-liquid separation on the treated slurry to obtain a treated substance; leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate; adding a surfactant mixed solution into the first filtrate, and uniformly stirring and mixing to obtain a mixed solution; adding strong ammonia water into the mixed solution under stirring to adjust the pH value to be alkaline, and filtering to obtain a precipitate; and calcining the precipitate to obtain the battery material. According to the invention, the electrode material and the current collector are easily separated by the separation tank, the electrode material and the current collector are leached by a leachate wet process, a surfactant mixed solution is added, the nickel-cobalt-manganese intermediate is precipitated by adjusting the pH value, and then the battery material is obtained by calcining. The whole recovery method is simple and efficient, and the quality of the regenerated battery material is high.
Description
Technical Field
The invention relates to the technical field of battery recycling, in particular to a new energy battery material recycling and regenerating treatment method.
Background
Since the commercialization of lithium ion batteries has been achieved in 1990, lithium ion batteries have advantages of high energy density, high operating voltage, good safety, long cycle life, and small self-discharge, and thus have been widely used in the fields of mobile communication, instruments, meters, computers, and the like instead of conventional secondary batteries such as nickel hydrogen batteries, nickel cadmium batteries, lead-acid batteries, and have become the mainstay of the secondary battery market. Meanwhile, with the development of new energy strategies in various countries in recent years, electric vehicles, particularly hybrid electric vehicles, are developed particularly rapidly, and the market share of lithium ion batteries in power batteries used by the electric vehicles is gradually increased. At present, china has become a world with large production and consumption of lithium ion batteries, and in 2007, the yield of lithium ion batteries in China reaches 15.5 hundred million (accounting for 16.9 percent of the global yield), and the yield of lithium ion batteries in China exceeds that in Japan for the first time and is the first in the world.
However, the huge battery consumption also brings huge amount of waste batteries, which not only wastes resources, but also causes serious pollution to the environment.
The recovery of the waste lithium ion power battery mainly comprises two methods: and (5) performing gradient utilization and disassembly recovery. If the power battery of the new energy automobile is directly disassembled after being attenuated, serious resource waste can be caused, and the automobile power battery with the capacity reduced to below 80 percent can be utilized in a gradient manner. The disassembly and recycling is to disassemble the battery and recycle the battery as resources, and refers to the battery with the battery capacity reduced to below 50% and the discarded battery after the battery is used for a plurality of times. The research on relevant theories and engineering demonstration of domestic lithium ion battery recycling are late, the commercialization standardization of the echelon utilization of the power battery is low, the market management is disordered, and the method mainly comprises the steps of disassembling and recycling raw materials at present. The recovery process of the waste power battery generally comprises pretreatment, separation, recovery, impurity removal and reutilization. The recovery process of the lithium iron phosphate battery comprises the following steps: the waste LiFePO4 battery is discharged and disassembled, and components such as a battery shell, a negative electrode material, a positive electrode material, a diaphragm and the like are disassembled and separated and then are respectively recovered. The positive electrode material is subjected to heat treatment, alkaline leaching or organic solvent method to separate active substances, and valuable metals in the positive electrode material are recovered by high-temperature direct regeneration or wet process.
According to the method for regenerating the anode material in the prior art, when the coarse precipitation of the lithium iron phosphate precursor is carried out, the flocculant needs to be manually controlled to be added, and the flocculant needs to be added according to a certain amount while filtrate and an organic solvent are added, so that the flocculant is often added under the control of third-party manpower, manpower is wasted, and the flocculant is easily added excessively through manual addition of the flocculant, the quality of the coarse precipitation of the lithium iron phosphate precursor can be influenced by the excessive flocculant, and the quality of the final battery material recovery is influenced.
Disclosure of Invention
The invention aims to provide a new energy battery material recycling and regenerating treatment method, which aims to solve the problem that the recycling and regenerating quality of a battery material is influenced by adding a large amount of flocculating agent in the existing battery material recycling and regenerating treatment process.
The technical scheme for solving the technical problems is as follows:
a new energy battery material recycling and regenerating treatment method comprises the following steps:
(1) Discharging the waste lithium ion battery, removing the shell, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation tank containing a solution, heating and dipping to separate an electrode material from a current collector to obtain a treated slurry;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate;
(4) Adding a surfactant mixed solution into the first filtrate, and uniformly stirring and mixing to obtain a mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to be alkaline, and filtering to obtain a precipitate;
(6) And calcining the precipitate to obtain the battery material.
Further, in a preferred embodiment of the present invention, the solution in the step (1) is N-methylpyrrolidone, N-dimethylacetamide and polyethylene glycol in a mass ratio of (2-5): (1.5-4.5): (1-3) mixing.
Further, in a preferred embodiment of the present invention, the heating impregnation treatment conditions in the step (1) are as follows: the temperature is 50-65 ℃, and the dipping time is 10-15 h.
Further, in a preferred embodiment of the present invention, the leaching solution in the step (3) is a mixture of formic acid, citric acid and glucose.
Further, in a preferred embodiment of the present invention, the concentration of formic acid is 1.0 to 1.5mol/L, the concentration of citric acid is 0.25 to 0.75mol/L, and the volume ratio of formic acid to citric acid is (2 to 5): 1, adding 5-12 wt% of glucose based on the total volume of formic acid and citric acid.
Further, in a preferred embodiment of the present invention, in the step (4), the surfactant mixed solution is prepared by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and stirring uniformly; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.05 to 0.1 percent, 0.01 to 0.1 percent and 0.5 to 1 percent of the total volume of the mixed solution of the surfactant.
Further, in a preferred embodiment of the present invention, the pH is adjusted to 8.5 to 9.0 in the step (3).
Further, in a preferred embodiment of the present invention, the calcination conditions in the step (6) are: calcining at 700-900 deg.c for 10-20 hr.
The invention has the following beneficial effects:
1. according to the invention, the electrode material and the current collector are easily separated by the separation tank, the electrode material and the current collector are leached by a leachate wet process, a surfactant mixed solution is added, the nickel-cobalt-manganese intermediate is precipitated by adjusting the pH value, and then the battery material is obtained by calcining. The whole recovery method is simple and efficient, and the quality of the regenerated battery material is high.
2. The separation pool contains the treatment solution of N-methyl pyrrolidone, N-dimethylacetamide and polyethylene glycol, can well separate the electrode material and the current collector under the heating condition, simplifies the complicated treatment steps, and has simple operation and obvious treatment effect.
3. The leachate is the mixture of formic acid, citric acid and glucose, and the glucose reduces the transition metal in high valence state into transition leaching in low valence state and is oxidized into small molecular acid. Therefore, the acid leaching agent not only has a reduction effect, but also has a dissolving effect, so that the leaching of valuable metals is enhanced, and the concentration of acid required by a leaching system is reduced.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
A new energy battery material recycling and regenerating treatment method comprises the following steps:
(1) Discharging the waste lithium ion battery, removing the shell, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation tank containing a solution, and heating and dipping for 10-15 hours at the temperature of 50-65 ℃ to separate an electrode material from a current collector to obtain a treated slurry;
wherein the solution is N-methyl pyrrolidone, N-dimethyl acetamide and polyethylene glycol in a mass ratio of (2-5): (1.5-4.5): (1-3) mixing;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate;
wherein the leaching solution is prepared by mixing formic acid, citric acid and glucose; the concentration of formic acid is 1.0-1.5 mol/L, the concentration of citric acid is 0.25-0.75 mol/L, and the volume ratio of formic acid to citric acid is (2-5): 1, adding glucose which is 5-12 wt% of the total volume of formic acid and citric acid;
(4) Adding a surfactant mixed solution into the first filtrate, and uniformly stirring and mixing to obtain a mixed solution;
wherein, the surfactant mixed solution is prepared by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and stirring uniformly; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.05 to 0.1 percent, 0.01 to 0.1 percent and 0.5 to 1 percent of the total volume of the surfactant mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to 8.5-9.0, and filtering to obtain a precipitate;
(6) And calcining the precipitate at 700-900 ℃ for 10-20 h to obtain the battery material.
Example 1:
the new energy battery material recycling and regenerating treatment method comprises the following steps:
(1) Discharging a waste lithium ion battery, removing a shell, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation tank containing a solution, and heating and dipping for 10 hours at the temperature of 50 ℃ to separate an electrode material from a current collector to obtain a treated slurry;
wherein the solution is prepared from N-methyl pyrrolidone, N-dimethylacetamide and polyethylene glycol according to a mass ratio of 2:1.5:1, mixing;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate;
wherein the leaching solution is prepared by mixing formic acid, citric acid and glucose; the concentration of formic acid is 1.0mol/L, the concentration of citric acid is 0.25mol/L, and the volume ratio of formic acid to citric acid is 2:1, adding glucose to 5wt% of the total volume of formic acid and citric acid;
(4) Adding a surfactant mixed solution into the first filtrate, and uniformly stirring and mixing to obtain a mixed solution;
wherein, the surfactant mixed solution is prepared by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and stirring uniformly; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.05 percent, 0.01 percent and 0.5 percent of the total volume of the surfactant mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to 8.5, and filtering to obtain a precipitate;
(6) And calcining the precipitate at 700 ℃ for 10h to obtain the battery material.
The obtained battery material, acetylene black and a binder polytetrafluoroethylene emulsion (the mass fraction is 60%) are uniformly mixed in an ethanol solution according to a certain mass ratio (82: 13: 5), and the anode is prepared by film stirring, tabletting and drying. A2032 button cell is assembled by using a metal lithium sheet as a negative electrode, using a 1M solution of lithium hexafluorophosphate, ethylene carbonate and dimethyl carbonate as an electrolyte and a polypropylene microporous membrane as a diaphragm to perform charge and discharge tests. The first charging specific capacity is 157.2mAh/g under the multiplying power of 0.1C, the first discharging specific capacity is 150.3mAh/g, the first charging and discharging efficiency reaches 96.3%, and the first discharging specific capacity is 128.3mAh/g under the multiplying power of 1C.
Example 2:
the new energy battery material recycling and regenerating treatment method comprises the following steps:
(1) Discharging and shell removing a waste lithium ion battery, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation cell containing a solution, and heating and dipping for 12 hours at the temperature of 60 ℃ to separate an electrode material from a current collector to obtain a treated slurry;
wherein the solution is prepared from N-methylpyrrolidone, N-dimethylacetamide and polyethylene glycol according to a mass ratio of 3.5:3:2, mixing;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate;
wherein the leaching solution is prepared by mixing formic acid, citric acid and glucose; the concentration of formic acid is 1.2mol/L, the concentration of citric acid is 0.5mol/L, and the volume ratio of formic acid to citric acid is 3.5:1, adding glucose to 7wt% of the total volume of formic acid and citric acid;
(4) Adding a surfactant mixed solution into the first filtrate, and stirring and mixing uniformly to obtain a mixed solution;
wherein, the surfactant mixed solution is prepared by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and stirring uniformly; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.075 percent, 0.05 percent and 0.75 percent of the total volume of the surfactant mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to 9.0, and filtering to obtain a precipitate;
(6) And calcining the precipitate at 800 ℃ for 15h to obtain the battery material.
The obtained battery material, acetylene black and adhesive polytetrafluoroethylene emulsion (the mass fraction is 60%) are uniformly mixed in ethanol solution according to a certain mass ratio (82: 13: 5), and the anode is prepared by film stirring, tabletting and drying. A2032 button cell is assembled by using a metal lithium sheet as a negative electrode, using a 1M solution of lithium hexafluorophosphate, ethylene carbonate and dimethyl carbonate as an electrolyte and a polypropylene microporous membrane as a diaphragm to perform charge and discharge tests. The first charge specific capacity is 152.9mAh/g under the multiplying power of 0.1C, the first discharge specific capacity is 145.6mAh/g, the first charge-discharge efficiency is 95.5%, and the discharge specific capacity is 132.8mAh/g under the multiplying power of 1C.
Example 3:
the new energy battery material recycling and regenerating treatment method comprises the following steps:
(1) Discharging the waste lithium ion battery, removing the shell, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation tank containing a solution, and heating and dipping for 15 hours at the temperature of 65 ℃ to separate an electrode material from a current collector to obtain a treated slurry;
wherein the solution is prepared from N-methyl pyrrolidone, N-dimethylacetamide and polyethylene glycol according to a mass ratio of 5:4.5:3, mixing;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching solution, and performing filter pressing on the leached substance to obtain a first filtrate;
wherein the leaching solution is prepared by mixing formic acid, citric acid and glucose; the concentration of formic acid is 1.5mol/L, the concentration of citric acid is 0.75mol/L, and the volume ratio of formic acid to citric acid is 2:1, adding glucose into the mixture to form a mixture, wherein the adding amount of the glucose is 12wt% of the total volume of formic acid and citric acid;
(4) Adding a surfactant mixed solution into the first filtrate, and stirring and mixing uniformly to obtain a mixed solution;
wherein, the surfactant mixed solution is prepared by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and stirring uniformly; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.1 percent, 0.1 percent and 1 percent of the total volume of the surfactant mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to 9.0, and filtering to obtain a precipitate;
(6) And calcining the precipitate at 900 ℃ for 20h to obtain the battery material.
The obtained battery material, acetylene black and adhesive polytetrafluoroethylene emulsion (the mass fraction is 60%) are uniformly mixed in ethanol solution according to a certain mass ratio (82: 13: 5), and the anode is prepared by film stirring, tabletting and drying. A2032 button cell is assembled by using a metal lithium sheet as a negative electrode, using a 1M solution of lithium hexafluorophosphate, ethylene carbonate and dimethyl carbonate as an electrolyte and a polypropylene microporous membrane as a diaphragm to perform charge and discharge tests. The first charging specific capacity is 145.2.8mAh/g under the multiplying power of 0.1C, the first discharging specific capacity is 137.8mAh/g, the first charging and discharging efficiency is 94.5%, and the first discharging specific capacity is 123.1mAh/g under the multiplying power of 1C.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A new energy battery material recycling and regenerating treatment method is characterized by comprising the following steps:
(1) Discharging the waste lithium ion battery, removing the shell, separating a battery pole piece, crushing the battery pole piece, putting the crushed battery pole piece into a separation tank containing a solution, heating and dipping to separate an electrode material from a current collector to obtain a treated slurry; wherein, the adopted solution is N-methyl pyrrolidone, N-dimethyl acetamide and polyethylene glycol according to the mass ratio of (2-5): (1.5-4.5): (1-3) mixing;
(2) Carrying out solid-liquid separation on the treated slurry to obtain a treated substance;
(3) Leaching the treated substance with a leaching agent, and performing filter pressing on the leached substance to obtain a first filtrate;
(4) Adding a surfactant mixed solution into the first filtrate, and uniformly stirring and mixing to obtain a mixed solution; wherein, the adopted surfactant mixed solution is formed by adding methanol, ethyl didodecyl ammonium phosphate and triethanolamine into deionized water and uniformly stirring; wherein, the methanol, the ethyl didodecyl ammonium phosphate and the triethanolamine respectively account for 0.05 to 0.1 percent, 0.01 to 0.1 percent and 0.5 to 1 percent of the total volume of the surfactant mixed solution;
(5) Adding strong ammonia water into the mixed solution under stirring to adjust the pH value to be alkaline, and filtering to obtain a precipitate;
(6) And calcining the precipitate to obtain the battery material.
2. The method for recycling and regenerating the new energy battery material as claimed in claim 1, wherein the heating impregnation treatment conditions in step (1) are as follows: the temperature is 50-65 ℃, and the dipping time is 10-15 h.
3. The method for recycling and regenerating new energy battery materials according to claim 1, wherein the leachate in step (3) is a mixture of formic acid, citric acid and glucose.
4. The new energy battery material recycling and regenerating treatment method according to claim 3, characterized in that the concentration of formic acid is 1.0 to 1.5mol/L, the concentration of citric acid is 0.25 to 0.75mol/L, and the volume ratio of formic acid to citric acid is (2 to 5): 1, the addition of the glucose is 5-12 wt% of the total volume of the formic acid and the citric acid.
5. The method for recycling and regenerating a new energy battery material according to claim 1, characterized in that in the step (5), the pH is adjusted to 8.5 to 9.0.
6. The new energy battery material recycling and regenerating treatment method according to claim 5, characterized in that the calcining conditions in the step (6) are as follows: calcining at 700-900 deg.c for 10-20 hr.
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