CN107959079B - Method for recycling waste lithium ion battery negative electrode material - Google Patents

Method for recycling waste lithium ion battery negative electrode material Download PDF

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Publication number
CN107959079B
CN107959079B CN201711463982.8A CN201711463982A CN107959079B CN 107959079 B CN107959079 B CN 107959079B CN 201711463982 A CN201711463982 A CN 201711463982A CN 107959079 B CN107959079 B CN 107959079B
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ion battery
lithium
lithium ion
waste
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CN107959079A (en
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杨越
孙伟
胡岳华
宋绍乐
江峰
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Central South University
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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
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Secondary Cells (AREA)
  • Processing Of Solid Wastes (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses aA method for recycling waste lithium ion battery cathode materials. Firstly, the graphite material of the negative electrode of the waste lithium ion battery is added with a certain concentration H+The aqueous solution of (A) is washed by shaking up and down or by refluxing and circulating. The graphite layers are expanded while recovering lithium resources. Then, lithium contained in the washing liquid was used as a raw material, and a lithium carbonate product was prepared by a precipitation method. And finally, preparing the graphene material by taking the washed waste graphite as a raw material and utilizing a liquid-phase mechanical stripping method. The method is simple and convenient for large-scale production and application. The lithium carbonate material and the graphene product with high added value are regenerated, the economy of recycling the waste lithium ion battery cathode material is improved, and the resource utilization of the waste lithium ion battery cathode material is realized.

Description

Method for recycling waste lithium ion battery negative electrode material
Technical Field
The invention relates to the field of waste battery recovery, in particular to a method for recycling a waste lithium ion battery cathode material.
Technical Field
With the development of new energy automobiles, the use and scrap number of power lithium ion batteries is continuously increased. The storage of a large amount of waste lithium ion batteries not only pollutes the environment, but also causes the waste of resources. At present, researches on recovering valuable metal components such as nickel, cobalt, manganese, lithium and the like from the anode material of the waste lithium ion battery are carried out, and good effects are obtained. Compared with the anode material, the value of the anode material of the waste lithium ion battery is relatively low. However, with the shortage of lithium resources and the rising price, the value contained in the negative electrode needs to be explored, and how to improve the economical efficiency of the recovery of the negative electrode graphite material is a more significant problem.
The waste lithium ion battery cathode material contains a certain amount of lithium resources. The lithium sources are mainly two: firstly, in the charge-discharge process of the lithium ion battery, the inserted lithium can not be removed and is retained between material layers; the second is lithium adsorbed onto the material by the electrolyte. Therefore, a primary goal of improving the recovery of the anode material is to recover this portion of the lithium resource.
In addition, the high-value utilization of graphite is another key factor for improving the recovery benefit of the waste lithium ion battery and realizing the resource utilization of the waste negative electrode material. The graphene is a novel two-dimensional nano material, and has the advantages of high strength, high electric and heat conductivity and huge application potential. Graphite is an important raw material for preparing graphene, and patent CN10325906A discloses a method for stripping regenerated graphene by using a redox method by taking a waste lithium ion battery cathode graphite material as a raw material. Actually, graphite in the negative electrode material of the waste lithium ion battery expands between graphite layers due to the intercalation of lithium ions, and the graphite is easier to peel off, so that whether a graphene regeneration preparation method which is safer and more environment-friendly and convenient for large-scale production can be developed based on the characteristics of the negative electrode graphite of the waste lithium ion battery, and the method has important significance for further improving the overall recovery value of the waste lithium ion battery. In order to achieve the aim, the invention develops a method for preparing high value-added graphene by extracting lithium from a waste lithium ion battery cathode material and directly stripping a liquid phase, and provides a new idea for realizing resource utilization of the waste lithium ion battery cathode material.
Disclosure of Invention
The invention aims to develop a method for recovering lithium resources from a waste lithium ion battery cathode material and preparing high value-added graphene.
The invention relates to a method for recycling a waste lithium ion battery cathode material, which mainly comprises the following steps:
step one
Placing the waste negative electrode graphite material in an acid solution for washing in an up-and-down shaking manner; obtaining a washed liquid and a washed solid;
or
Placing the waste negative graphite material in a reactor; introducing acid liquor from the bottom of the reactor; pumping the acid solution from the top of the reactor to form a circulation; obtaining a washed liquid and a washed solid;
or
Placing the waste negative graphite material in a reactor; introducing acid liquor from the top of the reactor; pumping acid liquor from the bottom of the reactor to form circulation; obtaining a washed liquid and a washed solid;
step two
After washing is finished, carrying out solid-liquid separation; obtaining a solid and a liquid; drying the solid; obtaining a standby solid;
step three
Adjusting the pH value of the liquid obtained in the step two to be more than or equal to 7, and then adding water-soluble carbonate or blowing carbon dioxide; generating a precipitate to obtain lithium carbonate;
step four
Stripping the solid obtained in the step two; and obtaining the graphene.
The invention relates to a method for recycling waste lithium ion battery negative electrode materials, which comprises the step one, wherein the particle size of the waste negative electrode graphite materials is less than or equal to 50 micrometers.
The invention relates to a method for recycling a waste lithium ion battery negative electrode material+The concentration of (B) is 0.3-1 mol/L.
The invention relates to a method for recycling waste lithium ion battery negative electrode materials, wherein in the first step, the liquid-solid ratio of the waste negative electrode graphite materials to acid liquor is 10-50 ml/g. The specific time of the step one is adjusted according to the amount of the waste cathode graphite material. Generally, the time is controlled to be 30-60 minutes.
The invention relates to a method for recycling waste lithium ion battery cathode materials, which comprises the following steps that in the first step, when the concentration of Li ions in a washing liquid is less than 1-1.5 mol/L; the material is reused in the next batch of materials in the first step, and H is ensured in the using process+The concentration of (A) is 0.3-1 mol/L; when the concentration of Li ions in the liquid after washing is 1-1.5mol/L, after the washing of the batch is finished; filtering; obtaining the solid and the liquid in the step two.
The invention relates to a method for recycling waste lithium ion battery cathode materials, wherein in the second step, the temperature is controlled to be 60-80 ℃ when the solid is dried.
The invention relates to a method for recycling a waste lithium ion battery cathode material, which comprises the following steps of obtaining liquid in a second step; adding NaOH or ammonia water to adjust the pH value of the solution to be more than 7, then adding water-soluble carbonate or introducing CO2。
The invention relates to a method for recycling waste lithium ion battery cathode materials, which comprises the following steps of, in step three, selecting water-soluble carbonate from at least one of sodium carbonate and ammonium carbonate; the molar ratio of the water-soluble carbonate to the Li ions in the liquid is 0.5 or more. Preferably 0.5-0.55.
The invention relates to a method for recycling waste lithium ion battery cathode materials, which comprises the third step of adopting any one of magnetic force or mechanical stirring in the process of preparing lithium carbonate, and controlling the rotating speed at 100-500 revolutions per minute. The addition rate of the carbonate solution is controlled to be 2-10 ml/min. The precipitation reaction temperature is controlled at 60-90 ℃.
The invention relates to a method for recycling waste lithium ion battery negative electrode materials. The mechanical stripping comprises ball milling stripping by adopting a ball mill or homogenizing stripping by adopting a homogenizer. When the ball milling is stripped, the material of the used grinding ball is zirconia or corundum.
The invention relates to a method for recycling waste lithium ion battery cathode materials, wherein the mechanical stripping time is 1.5-4 hours; after stripping, settling for 5-12 hours; then taking the upper suspension liquid for storage; the underlying particles continue to mechanically delaminate. The obtained supernatant suspension contains graphene. The lower layer particles are continuously stripped mechanically to form a closed circuit on the process.
The invention relates to a method for recycling a waste lithium ion battery cathode material. The dispersing agent is selected from any one of N-methyl pyrrolidone, dimethyl formamide, tetrahydrofuran solvent or sodium dodecyl benzene sulfonate and polyvinylpyrrolidone surfactant aqueous solution. The concentration of the dispersant is 0.03-5%.
According to the method for recycling the waste lithium ion battery cathode material, the recovery rate of lithium is more than or equal to 99%; the specific surface area of the obtained graphene is 250-550m2(iv)/g, preferably 400-2The number of layers is from 5 to 10, preferably from 5 to 7,/g.
Compared with the existing method for regenerating the cathode material of the waste lithium ion battery, the method has the following characteristics:
(1) the recycling of lithium resources is realized to the maximum extent through circulating acid washing or oscillating acid washing, the defects among graphite layers are overcome, graphite is expanded, and conditions are laid for subsequent preparation of high-quality graphene. Meanwhile, the process designed by the invention can also realize continuous and semi-continuous industrial application.
(2) The method for preparing the graphene from the waste lithium ion battery graphite material by adopting a mechanical stripping method is simple and convenient for large-scale production and application.
(3) The lithium carbonate material and the graphene product with high added value are regenerated, the economy of recycling the waste lithium ion battery cathode material is improved, and the resource utilization of the waste lithium ion battery cathode material is realized.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1
Crushing 5g of waste lithium ion battery negative electrode material to 20 microns, and placing the crushed material in 250ml of H+In an aqueous solution (hydrochloric acid) having a concentration of 1 mol/L. The solid-liquid mixture was placed in a 500ml separatory funnel and then placed in a shaker again to shake up and down for 1 hour. Then filtering by adopting a suction filtration method. The solid obtained after filtration is placed in an oven at 80 ℃ and kept warm for 3 hours. And detecting the concentration of lithium ions in the filtrate by utilizing ICP (inductively coupled plasma), and calculating to obtain that the leaching rate of lithium reaches 99%.
H in the filtrate+The concentration of the lithium ion battery is adjusted to 1mol/L again, and 5g of new waste lithium ion battery cathode material is added into the aqueous solution. Under the same washing condition, the leaching is repeated for several times, and after the concentration of lithium ions in the washing solution is accumulated to 1mol/L, the liquid is collected for standby.
100ml of collected 1mol/L lithium-containing washing solution is placed in a 500ml round-bottom three-neck flask. 100ml of 0.5mol/L sodium carbonate solution were injected at a rate of 2 ml/min by means of a peristaltic pump with magnetic stirring (300 revolutions/min). The whole reaction process is carried out under the condition of water bath at 80 ℃. After the liquid injection is finished, stirring for 2 hours under the condition of heat preservation, and then obtaining white precipitate. Filtering, washing and drying (80 ℃) to obtain the lithium carbonate product with the purity of 99.1 percent. The recovery of lithium was calculated to be 99.5%.
Example 2
The procedure of the method for extracting lithium in this example is the same as in example 1. And drying the waste lithium ion battery graphite material obtained after washing in an oven at 80 ℃ for 3 hours. Then, 5g of the treated waste graphite material is put into 500ml of 5% sodium dodecyl benzene sulfonate solution. The solid-liquid mixture was placed in a homogenizer for 2 hours. Then placing the graphene material into a 500ml measuring cylinder, settling for 8 hours, taking the upper layer suspension to obtain the graphene material with the specific surface area of 400m2The number of layers is 5-8. The large-particle graphite in the lower measuring cylinder can be used as a preparation raw material for repeated use.
Example 3
The procedure of the method for extracting lithium in this example is substantially the same as in examples 1 and 2. Except that carbon dioxide was used as the precipitant to prepare lithium carbonate with a purity of 99.2% and the calculated recovery of lithium was 99.8%. The method for preparing graphene in this example is substantially the same as that described in example 2. Except that the dispersant used in this example was N-methylpyrrolidone. After primary homogenizing and stripping; the specific surface area of the obtained graphene is 450g/m2The number of the layers is 5-7.
Example 4
The procedure of the method for extracting lithium in this example is the same as in examples 1 and 2. 10g of the separated solid graphite was put into 500ml of a 0.05% aqueous solution of a polyvinylpyrrolidone surfactant. Placing the mixture in a ball mill, using ZrO2Ball milling was performed for 4 hours for the ball milling media. And then placing the ball-milled solution in a 500ml measuring cylinder, settling and dispersing for 10 hours, and taking the upper layer suspension to obtain the graphene material. The specific surface area of the obtained graphene is 280m2The number of layers is 8-10.
Example 5
The other conditions were identical to those of example 1, except that the washing-leaching was carried out according to the following scheme:
crushing waste negative graphite materials and then placing the crushed waste negative graphite materials in a reactor; introducing acid liquor from the bottom of the reactor; pumping the acid solution from the top of the reactor to form a circulation; obtaining a washed liquid and a washed solid;
according to the scheme, the recovery rate of lithium is 99.6%, and the purity of lithium carbonate is 99.1%;
after primary homogenizing and stripping; the specific surface area of the obtained graphene is 410g/m2The number of the layers is 5-7.
Example 6
The other conditions were identical to those of example 1, except that the washing-leaching was carried out according to the following scheme:
crushing waste negative graphite materials and then placing the crushed waste negative graphite materials in a reactor; introducing acid liquor from the top of the reactor; pumping acid liquor from the bottom of the reactor to form circulation; obtaining a washed liquid and a washed solid;
according to the scheme, the recovery rate of lithium is 99.3%, and the purity of lithium carbonate is 99.1%;
after primary homogenizing and stripping; the specific surface area of the obtained graphene is 395g/m2The number of the layers is 5-8.
Comparative example 1
Otherwise the procedure was consistent with example 1; the difference lies in that:
5g of waste lithium ion battery cathode material is put into 250ml of H+1mol/L aqueous solution; stirring was carried out at 150 rpm for 1 hour. At the moment, the lithium leaching rate is only 65 percent;
h in the filtrate+The concentration of the lithium ion battery is adjusted to 1mol/L again, and 5g of new waste lithium ion battery cathode material is added into the aqueous solution. Under the same washing conditions (i.e., agitation leaching washing), leaching-washing was repeated several times, and after the concentration of lithium ions in the washing solution had accumulated to 1mol/L, the liquid was collected for use.
100ml of collected 1mol/L lithium-containing washing solution is placed in a 500ml round-bottom three-neck flask. 100ml of 0.5mol/L sodium carbonate solution were injected at a rate of 2 ml/min by means of a peristaltic pump with magnetic stirring (300 revolutions/min). The whole reaction process is carried out under the condition of water bath at 80 ℃. After the liquid injection is finished, stirring for 2 hours under the condition of heat preservation, and then obtaining white precipitate. Filtering, washing and drying (80 ℃) to obtain the lithium carbonate product with the purity of 99 percent. The recovery of lithium was calculated to be 71%.
Meanwhile, the waste lithium ion battery graphite material obtained after washing is dried in an oven at 80 ℃ for 3 hours. Then, 5g of the treated waste graphite material is put into 500ml of 5 wt% sodium dodecyl benzene sulfonate solution. The solid-liquid mixture was placed in a ball mill for 2 hours. Then placing the mixture into a 500ml measuring cylinder, settling for 8 hours, taking the upper suspension to obtain the graphene material, wherein the specific surface area of the obtained graphene is only 237g/m2The number of the layers is more than 10.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention relates, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are deemed to fall within the scope of the invention.

Claims (2)

1. A method for recycling a waste lithium ion battery negative electrode material is characterized by comprising the following steps:
crushing 5g of waste lithium ion battery negative electrode material to 20 microns, and placing the crushed material in 250ml of H+1mol/L hydrochloric acid aqueous solution; placing the solid-liquid mixture into a 500ml separating funnel, and then placing the separating funnel into an oscillator to shake for 1 hour up and down; repeating the leaching for several times, and collecting liquid for later use after the concentration of lithium ions in the washing solution is accumulated to 1 mol/L; then filtering by adopting a suction filtration method; putting the solid obtained after filtering into an oven at 80 ℃ for heat preservation for 3 hours;
taking 100ml of collected 1mol/L lithium-containing washing liquid, and placing the 1mol/L lithium-containing washing liquid into a 500ml round-bottom three-neck flask; under the condition of magnetic stirring at 300 revolutions per minute, a peristaltic pump is utilized to inject 100ml of sodium carbonate solution with the concentration of 0.5mol/L at the speed of 2ml per minute; the whole reaction process is carried out under the condition of water bath at 80 ℃; after the liquid is injected, stirring for 2 hours under the condition of heat preservation, and then obtaining a white precipitate; filtering, washing and drying at 80 ℃ to obtain a lithium carbonate product, wherein the purity of the lithium carbonate product is 99.1 percent, and the recovery rate of lithium is 99.5 percent by calculation;
drying the washed waste lithium ion battery graphite material in an oven at 80 ℃ for 3 hours; then, taking 5g of the treated waste graphite material, and placing the waste graphite material in 500ml of 5% sodium dodecyl benzene sulfonate solution; treating the solid-liquid mixture in a homogenizer for 2 hours; then placing the graphene material into a 500ml measuring cylinder, settling for 8 hours, taking the upper layer suspension to obtain the graphene material with the specific surface area of 400m2The large-particle graphite in the lower measuring cylinder is used as a preparation raw material for repeated use.
2. A method for recycling a waste lithium ion battery negative electrode material is characterized by comprising the following steps:
crushing 5g of waste lithium ion battery negative electrode material to 20 microns, and placing the crushed material in 250ml of H+1mol/L hydrochloric acid aqueous solution; placing the solid-liquid mixture into a 500ml separating funnel, and then placing the separating funnel into an oscillator to shake for 1 hour up and down; repeating the leaching for several times, and collecting liquid for later use after the concentration of lithium ions in the washing solution is accumulated to 1 mol/L; then filtering by adopting a suction filtration method; putting the solid obtained after filtering into an oven at 80 ℃ for heat preservation for 3 hours;
taking 100ml of collected 1mol/L lithium-containing washing liquid, and placing the 1mol/L lithium-containing washing liquid into a 500ml round-bottom three-neck flask; the purity of the lithium carbonate prepared by adopting carbon dioxide as a precipitator is 99.2 percent, and the recovery rate of lithium is calculated to be 99.8 percent;
drying the washed waste lithium ion battery graphite material in an oven at 80 ℃ for 3 hours; then, taking 5g of the treated waste graphite material, and putting the waste graphite material into 500ml of 5% N-methyl pyrrolidone solution; treating the solid-liquid mixture in a homogenizer for 2 hours; then placing the graphene material into a 500ml measuring cylinder, settling for 8 hours, taking the upper layer suspension to obtain the graphene material with the specific surface area of 450m2The number of layers is 5-7; the large-particle graphite in the lower measuring cylinder is used as a preparation raw material for repeated use.
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CN108923096B (en) * 2018-09-10 2020-05-19 厦门理工学院 Method for recycling and regenerating all components of negative electrode of waste lithium ion battery
CN110797534A (en) * 2019-10-30 2020-02-14 中南大学 Method for preparing expanded graphite by using battery graphite cathode
CN112670609B (en) * 2020-10-09 2022-05-17 武汉瑞杰特材料有限责任公司 Method and device for integrally recovering and regenerating all components of graphite cathode of waste lithium battery

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