CN108808150B - Method for comprehensively recycling waste ternary electrode material - Google Patents
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Abstract
The invention discloses a method for comprehensively recycling waste ternary electrode materials, which selectively removes lithium ions from ternary positive active substances under the drive of an external electric field by utilizing the structural characteristics of layered ternary electrode materials, and adopts a precipitator for precipitation and recycling; in addition, the lithium-deficient ternary cathode material is used as a catalyst for an oxygen evolution reaction. The recovery method can effectively recover the lithium element, can also functionally and integrally utilize the electrode material as the catalyst, has simple process and easy implementation, and is beneficial to popularization and application.
Description
Technical Field
The invention relates to a method for comprehensively recycling waste ternary electrode materials, and belongs to the technical field of lithium ion battery recycling.
Background
With the progress of science and technology and the rapid development of social economy, the process of industrialization and urbanization is accelerated continuously, and the demand of energy sources is in an increasing situation all the time. Human conventional energy fuels such as coal, oil, and natural gas have been largely exploited, so that non-renewable energy represented by fossil energy is gradually exhausted, and the global energy crisis problem is becoming severe. The use of renewable energy sources such as solar, wind and nuclear requires stable energy storage carriers. The lithium ion battery has the advantages of high specific energy, long cycle life, no memory effect, light weight and the like, so that the lithium ion battery becomes a high-efficiency secondary battery with the most application prospect and a chemical energy storage power source which is developed fastest at present.
The nickel-cobalt-manganese composite ternary material integrates LiCoO2、LiNiO2And LiMnO2And the like 3 common advantages of the layered materials have the performance superior to that of a single component, obvious ternary synergistic effect exists, and the basic physical properties and the charging platform of the layered materials are both equal to those of LiCoO2The lithium ion battery has the advantages of low cost, environmental friendliness and the like, and has become a research hotspot of people as a high-capacity positive electrode material, and the nickel-cobalt-manganese composite ternary material lithium ion battery is already put into commercial application. According to statistics, the installation amount of the nickel-cobalt-manganese composite ternary material lithium ion battery in the Chinese electric automobile market in 2017 is increased by 134.4% in the same ratio by 15 GWH. The positive ternary material transformation and the positive replacement of lithium iron phosphate by the ternary material in the positive direction of the power battery route become the anode material with the highest acceleration in 2017. However, with the increase of service time, the capacity, discharge efficiency, safety and other performances of the lithium ion battery are all obviously reduced, and the application requirements are difficult to meet. The service life of the lithium ion battery is generally 2-4 years, and the cycle period of use is about 500-1000 times. The number of the retired lithium ion batteries is increased rapidly year by year, and the number of the waste lithium ion batteries in China can reach 250 hundred million and the total weight is 50 ten thousand tons in 2020 predicted, wherein the ternary material lithium ion batteries account for a considerable proportion. The average content of lithium in the waste ternary material lithium ion battery is 1.9%, the average content of nickel is 12.1%, and the average content of cobalt is 2.3%, wherein metal lithium is a rare resource, the price of cobalt is high, and the content of waste batteries is higher than that of raw ores, so that the waste ternary material lithium ion battery is an important strategic material. From another perspective, the discarded lithium battery will cause serious pollution to the environment if not recycled. At present, imbalance of supply and demand of transition metal resources required by lithium ion battery production is gradually highlighted, the capacity of lithium ion ternary batteries is expanded by domestic power battery manufacturers in two years, and the market value created by recovering cobalt, nickel, manganese, lithium, iron, aluminum and other metals from waste power lithium batteries is predicted to reach 52 hundred million yuan in 2018. Therefore, the method has economic value and good social and environmental benefits when used for recycling the waste lithium batteries. Has attracted the attention of scholars at home and abroad.
At present, the recovery methods for lithium ion batteries are mainly divided into two main types, namely pyrometallurgical and hydrometallurgical methods. The so-called pyrometallurgical process is a process for purifying metals or metal compounds by treating waste lithium batteries at high temperature. The main process of the hydrometallurgical recovery of the electrode material of the lithium ion ternary battery is as follows: discharge disassembly of waste batteries → material pretreatment → alkaline leaching and acid leaching for recovering metal ions → fractional precipitation separation or synthesis and conversion, and mainly aims to enrich transition metal elements in electrode materials to prepare related metal compounds or ternary electrode materials and the like again so as to realize recycling. The method has the defects of complex process, difficult subsequent waste liquid treatment, low recovery rate and the like.
The existing recovery processing method is that the metal elements such as lithium, manganese and the like in the electrode material are recovered and purified to become basic chemical raw materials through separation processes such as dissolution, enrichment, precipitation and the like, but the recovery processing and the reasonable utilization are not purposefully carried out in the application process, so that the recovery processing method is obviously infeasible in economy. Effective recovery processing methods and technologies must be explored, and effective and reasonable ways are provided for solving the problems of environmental pollution and resource waste caused by waste lithium ion batteries, so that the use of materials is truly realized, and waste materials are changed into valuable materials.
Disclosure of Invention
The invention aims to provide a method for comprehensively recycling waste ternary electrode materials. The method utilizes the structural characteristics of the layered ternary electrode material, and an external electric field drives the lithium ions to be selectively removed from the ternary positive active material, and sodium phosphate or sodium carbonate and other precipitants are adopted for precipitation and recovery; in addition, the delithiated ternary electrode material can serve as an excellent catalyst for Oxygen Evolution Reaction (OER). The recovery method can effectively recover the lithium element, can also functionally and integrally utilize the electrode material as the catalyst, has simple process and easy implementation, and is beneficial to popularization and application.
The method for comprehensively recycling the waste ternary electrode material comprises the following steps:
step 1: soaking and dissolving a binder (PVDF) in a waste ternary electrode material by adopting an N-methylpyrrolidone solvent, stripping the electrode material from a current collector aluminum foil, and stripping a waste ternary positive electrode active substance LiNi obtained after strippingxCoyMnzO2Mixing (x + y + z ═ 1) and a binder (polyvinylidene fluoride PVDF or polytetrafluoroethylene PTFE) and coating the mixture on a conductive substrate, and drying the mixture in vacuum to obtain a ternary cathode material composite membrane; constructing an electrolytic cell by taking the obtained ternary cathode material composite membrane as an anode, an inert electrode as a cathode and a supporting electrolyte solution as an electrolyte, applying an electric field potential of 0.5-5V, and maintaining for 1-20 h, and selectively extracting lithium ions from a ternary cathode active substance into the electrolyte by using the structural characteristics of a layered ternary electrode material;
the waste ternary positive electrodeThe active material is LiNi1/3Co1/3Mn1/3O2(NCM111)、LiNi0.4Co0.2Mn0.4O2(NCM424)、LiNi0.5Co0.2Mn0.3O2(NCM523)、LiNi0.6Co0.2Mn0.2O2(NCM622)、LiNi0.7Co0.1Mn0.2O2(NCM712)、LiNi0.8Co0.1Mn0.1O2(NCM811), and the like.
The waste ternary electrode material also comprises LiCoO2、LiNiO2、Li2MnO4、LiNi0.5Mn0.5O2、LiNi0.75Mn0.25O2、LiNi0.5Mn1.5O4、LiNi0.7Co0.3O2Electrode material of equal composition (considering LiNi)xCoyMnzO2Wherein any one or two of x, y, z may take on a value of zero). The process is likewise suitable for nLi2MnO3·(1-n)Li(NixCoyMnz)O2(n is 0 to 1, and x + y + z is 1) and comprehensively recovering the lithium-rich electrode material.
The inert electrode is one of a graphite, carbon fiber cloth and other non-metal electrodes or a platinum electrode, a titanium mesh and other metal electrodes.
The supporting electrolyte solution is one or more of metal ion compound solutions such as sodium chloride, potassium chloride, lithium chloride and the like; the concentration range of the supporting electrolyte solution is 0.1-2 mol/L.
The conductive substrate is one of carbon fiber cloth, titanium mesh and graphite paper.
In the process of lithium removal driven by an external electric field, the temperature range of the electrolyte is 0-90 ℃, and the pH value range is 1-12.
Step 2: taking out the lithium-deficient ternary cathode material composite membrane obtained in the step (1), and sequentially cleaning the composite membrane with distilled water and ethanol to remove impurities such as residual chloride ions on the surface; then placing the composite membrane in NMP (N-methyl pyrrolidone) solvent, dissolving to remove the binder, removing the lithium-deficient ternary positive electrode material from the carbon fiber cloth or titanium mesh, centrifuging, washing and drying to obtain lithium-deficient nickel-cobalt-manganese composite metal oxide powder; the obtained lithium-deficient nickel-cobalt-manganese composite metal oxide powder can be directly used as a catalyst for Oxygen Evolution Reaction (OER).
And step 3: adding a precipitator into the electrolyte obtained in the step 1 to precipitate lithium ions in the electrolyte to obtain lithium carbonate or lithium phosphate; the obtained lithium carbonate or lithium phosphate can be used as a lithium source to be ground and mixed with raw materials such as iron phosphate, glucose and the like, and then the lithium carbonate or lithium phosphate is synthesized into a lithium iron phosphate electrode material through solid-phase calcination, so that the lithium iron phosphate electrode material can be recycled.
The precipitant is selected from sodium bicarbonate, sodium carbonate or sodium phosphate.
Coating the lithium-deficient nickel-cobalt-manganese composite metal oxide powder prepared by the invention on a glassy carbon rotary disk electrode for OER catalytic performance test, or carrying out OER catalytic performance test after the treatment by the following treatment modes:
taking out the lithium-deficient ternary cathode material composite membrane obtained in the step (1), and sequentially cleaning the composite membrane with distilled water and ethanol to remove impurities such as residual chloride ions on the surface; and then cutting the composite membrane into an electrode plate with a certain area, preparing the electrode plate into an OER sample to be tested, and directly clamping the electrode plate on a working electrode of an Oxygen Evolution Reaction (OER) test instrument to test the OER catalytic performance. The problem of poor conductivity of the material can be well solved by integrating the catalytic material with a conductive substrate (e.g., carbon cloth).
The method comprises the steps of firstly disassembling and sorting the waste ternary lithium ion battery, soaking a positive plate in an organic solvent, carrying out ultrasonic treatment to peel a positive material from a current collector aluminum foil, re-mixing a waste ternary positive active substance obtained after peeling with a binder, coating the mixture on a carbon fiber cloth or a titanium mesh, and constructing the electrolytic cell by taking a formed ternary positive material composite membrane as an anode, an inert electrode as a cathode and a supporting electrolyte solution with a certain concentration as an electrolyte. Lithium ions embedded between the layers of the layered nickel-cobalt-manganese ternary electrode material are removed and dissolved in aqueous solution under the drive of an external direct current electric field, so that the nickel-cobalt-manganese composite ternary material LiNi is realizedxCoyMnzO2Preparation of delithiated Li by in-situ conversion of (x + y + z ═ 1)1-NixCoyMnzO2(. ltoreq.1). Based on the good electrocatalytic properties of the nickel-cobalt-manganese composite metal oxide, the nickel-cobalt-manganese layered composite metal oxide obtained after lithium removal is used as a catalyst for an Oxygen Evolution Reaction (OER). Meanwhile, sodium phosphate or sodium carbonate is added into the solution after lithium removal to serve as a precipitator, lithium phosphate or lithium carbonate can be precipitated and recovered, lithium carbonate is a common recovery form of lithium element, and lithium phosphate can serve as an important raw material for re-synthesizing the lithium iron phosphate electrode material.
Drawings
FIG. 1 is a LiNi before and after delithiation treatment in example 1 of the present invention1/3Co1/3Mn1/3O2And (3) an X-ray diffraction (XRD) test comparison diagram of the (NCM111) type waste ternary cathode material.
FIG. 2 is a LiNi before and after delithiation treatment in example 1 of the present invention1/3Co1/3Mn1/3O2And (NCM111) type waste ternary cathode material Scanning Electron Microscope (SEM) comparison image. a is before delithiation, and b is after delithiation.
FIG. 3 is a LiNi before and after delithiation treatment in example 1 of the present invention1/3Co1/3Mn1/3O2The catalytic performance of the (NCM111) type waste ternary cathode material for Oxygen Evolution Reaction (OER) is compared.
FIG. 4 is LiNi before and after delithiation treatment in example 2 of the present invention0.5Co0.2Mn0.3O2And (2) an X-ray diffraction (XRD) test comparison diagram of the (NCM523) type waste ternary cathode material.
FIG. 5 shows LiNi before and after delithiation treatment in example 2 of the present invention0.5Co0.2Mn0.3O2A Scanning Electron Microscope (SEM) comparison picture of the (NCM523) type waste ternary cathode material. a is before delithiation and b is after delithiation.
FIG. 6 shows LiNi before and after delithiation treatment in example 2 of the present invention0.5Co0.2Mn0.3O2The catalytic performance of the (NCM523) type waste ternary cathode material for Oxygen Evolution Reaction (OER) is compared with that of the prior art.
Detailed Description
Example 1: LiNi1/3Co1/3Mn1/3O2Comprehensive recovery of (NCM111) type waste ternary material
The electrode material and a current collector aluminum foil are stripped by adopting a binder (PVDF) which is soaked and dissolved in an N-methyl pyrrolidone solvent, and the anode active material obtained after stripping, the binder PVDF and a conductive agent acetylene black are mixed according to the ratio of (8): 1: 1, mixing the raw materials into slurry, coating the slurry on carbon fiber cloth, placing the carbon fiber cloth in a vacuum oven for drying for 10 hours to form a composite membrane serving as an anode, taking blank carbon cloth as a cathode, and taking a sodium chloride solution with the concentration of 0.8mol/L as electrolyte to construct an electrolytic cell. An electric field voltage of 2V is applied and maintained for 6 h. And (3) carrying out an inductively coupled plasma spectrometer (ICP-MS) test on the electrolyte after lithium removal to obtain the concentration of lithium ions in the electrolyte, and calculating to obtain that the lithium removal rate reaches 97.6 percent as shown in Table 1.
The obtained composite membrane coated with the lithium-deficient NCM111 type ternary positive electrode material is taken down and washed for a plurality of times by distilled water and ethanol solution to remove impurities such as residual chloride ions on the surface, the composite membrane is characterized by X-ray diffraction (XRD), and is compared with XRD of NCM111 active substances which are not subjected to lithium removal and recovery, the result is shown in figure 1, XRD after lithium removal and recovery is greatly changed compared with XRD before lithium removal and recovery, a Scanning Electron Microscope (SEM) test is carried out to obtain the appearance of the composite membrane before and after lithium removal and recovery, for example, as shown in figure 2, the appearance and the composition of a sample are greatly changed after lithium removal driven by an electric field, the composite membrane is reasonably cut into an electrode plate with the thickness of 1cm × 1cm, the electrode plate is prepared into a sample to be tested by OER, and is directly clamped on a working electrode to carry out a catalyst performance test of Oxygen Evolution Reaction (OER), the performance of the NCM111 type ternary positive electrode material after lithium removal and recovery is shown in figure 3, and the NCM111 type ternary positive electrode2The lower overpotential is 246mV, and the performance is excellent.
Example 2: LiNi0.5Co0.2Mn0.3O2Comprehensive recovery of (NCM523) type waste ternary material
The electrode material and a current collector aluminum foil are stripped by adopting a binder (PVDF) which is soaked and dissolved in an N-methyl pyrrolidone solvent, and the anode active material obtained after stripping, the binder PVDF and a conductive agent acetylene black are mixed according to the ratio of (8): 1: 1, mixing the raw materials into slurry, coating the slurry on carbon fiber cloth, placing the carbon fiber cloth in a vacuum oven for drying for 10 hours to form a composite membrane serving as an anode, taking blank carbon cloth as a cathode, and taking a sodium chloride solution with the concentration of 0.8mol/L as electrolyte to construct an electrolytic cell. An electric field voltage of 2V is applied and maintained for 6 h. And (3) carrying out an inductively coupled plasma spectrometer (ICP-MS) test on the electrolyte after lithium removal to obtain the concentration of lithium ions in the electrolyte, and calculating to obtain that the lithium removal rate reaches 96.5%, as shown in Table 1.
The obtained composite membrane coated with the lithium-deficient NCM 523-type ternary positive electrode material is taken down and washed for a plurality of times by distilled water and ethanol solution to remove impurities such as residual chloride ions on the surface, the composite membrane is characterized by X-ray diffraction (XRD), and is compared with XRD of NCM111 active substances which are not subjected to lithium removal and recovery, the result is shown in figure 4, XRD after lithium removal and recovery is greatly changed compared with XRD before lithium removal and recovery, a Scanning Electron Microscope (SEM) test is carried out to obtain the appearance of the composite membrane before and after lithium removal and recovery, for example, as shown in figure 5, the appearance and the composition of a sample are greatly changed after lithium removal driven by an electric field, the composite membrane is reasonably cut into an electrode plate with the thickness of 1cm × 1cm, the electrode plate is prepared into an OER test sample to be tested, and is directly clamped on a working electrode to carry out the catalytic performance test of Oxygen Evolution Reaction (OER), the performance of the NCM 523-type ternary positive electrode material after lithium removal and recovery is shown in figure 6, and the NCM 523-2The lower overpotential is 179mV, and the performance is excellent.
Table 1 is a table of the results of inductively coupled plasma spectrometer (ICP-MS) tests of the electrolyte solutions after delithiation in examples 1 and 2.
TABLE 1
| Electrode material | Electric field voltage/V | Active substance mass/g | Electrolyte lithium ion concentration (mg/L) after lithium removal | De-lithiation rate/%) |
| NCM111 | 2.0 | 0.1071 | 37.37 | 97.6 |
| NCM523 | 2.0 | 0.1226 | 42.34 | 96.5 |
Claims (4)
1. A method for comprehensively recycling waste ternary electrode materials is characterized by comprising the following steps:
selectively removing lithium ions from the ternary positive active material under the drive of an external electric field by utilizing the structural characteristics of the layered ternary electrode material, and precipitating and recovering by adopting a precipitator; in addition, the lithium-deficient ternary cathode material is used as a catalyst for an oxygen evolution reaction; the method comprises the following steps:
step 1: soaking and dissolving a binder in the waste ternary electrode material by adopting an N-methyl pyrrolidone solvent, stripping the electrode material from a current collector aluminum foil, mixing a waste ternary positive electrode active substance obtained after stripping with the binder, coating the mixture on a conductive substrate, and drying in vacuum to obtain a ternary positive electrode material composite film; constructing an electrolytic cell by taking the obtained ternary cathode material composite membrane as an anode, an inert electrode as a cathode and a supporting electrolyte solution as electrolyte, driving to remove lithium by an external electric field, and selectively removing lithium ions from a ternary cathode active substance into the electrolyte by utilizing the structural characteristics of a layered ternary electrode material;
step 2: taking out the lithium-deficient ternary cathode material composite membrane obtained in the step (1), and sequentially cleaning the composite membrane with distilled water and ethanol to remove residual chloride ion impurities on the surface; then placing the composite membrane in NMP, dissolving and removing the binder, removing the lithium-deficient ternary positive electrode material from the carbon fiber cloth or the titanium mesh, centrifuging, washing and drying to obtain lithium-deficient nickel-cobalt-manganese composite metal oxide powder; the obtained lithium-deficient nickel-cobalt-manganese composite metal oxide powder can be directly used as a catalyst for oxygen precipitation reaction;
and step 3: adding a precipitator into the electrolyte obtained in the step 1 to precipitate lithium ions in the electrolyte to obtain lithium carbonate or lithium phosphate; the obtained lithium carbonate or lithium phosphate is used as a lithium source to prepare the lithium iron phosphate electrode material, so that the lithium iron phosphate electrode material can be recycled;
the precipitant is selected from sodium bicarbonate, sodium carbonate or sodium phosphate;
the waste ternary positive active substance is LiNi1/3Co1/3Mn1/3O2、LiNi0.5Co0.2Mn0.3O2One or more of the above;
the supporting electrolyte solution is 0.8mol/L sodium chloride solution; and in the process of driving the lithium removal by the external electric field, the potential of the external electric field is 2V and is maintained for 6 h.
2. The method of claim 1, wherein:
the inert electrode is one of graphite, carbon fiber cloth non-metal electrode or platinum electrode, and titanium mesh metal electrode.
3. The method of claim 1, wherein:
the conductive substrate is one of carbon fiber cloth, titanium mesh and graphite paper.
4. The method of claim 1, wherein:
in the process of lithium removal driven by an external electric field, the temperature range of the electrolyte is 0-90 ℃, and the pH value range is 1-12.
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| CN110743528B (en) * | 2019-11-05 | 2022-07-29 | 珠海冠宇电池股份有限公司 | Method for preparing water decomposition catalyst by using waste battery |
| CN110801844B (en) * | 2019-11-28 | 2022-06-07 | 江西理工大学 | Method for preparing demercuration catalyst by using waste anode material and application of demercuration catalyst |
| CN113355690B (en) * | 2020-03-03 | 2022-05-06 | 天津大学 | Method for preparing efficient water electrolysis catalyst on large scale by using waste lithium ion battery anode material |
| CN112695198A (en) * | 2020-12-04 | 2021-04-23 | 中南大学 | Method for producing hydrogen by combining recovery of waste lithium iron phosphate positive electrode material and electrochemical process |
| CN112551600B (en) * | 2020-12-08 | 2022-03-25 | 中南大学 | Method for preparing hydrogen by recovering waste lithium ion battery anode material in combined electrochemical manner |
| CN112645362B (en) * | 2020-12-23 | 2023-05-26 | 北京化工大学 | Method for preparing lithium carbonate by electrochemical extraction of lithium from chloride type lithium-containing brine |
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