CN112259821A - Method for recovering valuable metals from waste lithium ion batteries - Google Patents
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
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- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention discloses a method for recovering valuable metals from waste lithium ion batteries, and belongs to the technical field of waste battery recovery. The method comprises the following steps: (1) charging the waste lithium ion battery; (2) crushing the charged battery, and sorting the materials to obtain a mixture of anode and cathode materials; (3) calcining the mixture of the anode material and the cathode material at high temperature; (4) and (3) placing the calcined material in water, stirring, filtering, adding sodium carbonate into the filtrate to obtain lithium carbonate, wherein the filter residue is a metal simple substance and an oxide thereof. According to the invention, part of lithium ions are transferred to the negative electrode material through charging, and then the mixture of the positive electrode and the negative electrode is calcined, and lithium and other metals can be recovered through simple processes such as water immersion and the like. The method is simple and effective, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of waste battery recovery, and particularly relates to a method for recovering valuable metals from waste lithium ion batteries.
Background
The lithium ion battery has the advantages of high energy density, long cycle life and good safety, and is widely applied to 3C digital products, electric tools and electric automobiles. In recent years, with the upgrading of technologies, the updating and upgrading speed of digital products is accelerated, the usage amount of lithium ion batteries is gradually increased, and meanwhile, with the increasing of environmental protection requirements and the improvement of power battery technologies, the output and sales of electric vehicles are rapidly increased, and the lithium ion batteries are driven to be used in large quantities. According to statistics, the scrappage of the power lithium ion battery reaches 28 ten thousand tons in 2020, and the scrappage of the power lithium ion battery on the scale needs to be recycled, so that the environment-friendly social concept is met, and the resource is maximally utilized.
Most of the waste lithium ion batteries are treated by recovering metal elements, and in practice, problems of complex process, high cost and the like are frequently encountered due to the imperfection of the method. The current mainstream process is generally to leach all metals in the anode material through reduction acid leaching, and then separate and recover the metals in sequence by adopting chemical precipitation, extraction and other modes according to intermetallic differences. The method has the problems of complex process, large consumption of chemical reagents, low metal recovery rate and the like. There have also been studies to selectively extract lithium and then recover other metals, for example, chinese patent application No.: 201911120565.2, filing date: 11 and 15 in 2019, the name of the invention is: a method for selectively extracting lithium from waste ternary cathode materials. The method of this application, comprising the steps of: mixing waste ternary anode material powder with acid, and performing primary roasting to obtain a primary roasted product; mixing the first-stage roasting product with an auxiliary agent, and carrying out second-stage roasting to obtain a second-stage roasting product; and (4) leaching the second-stage roasting product in water, and performing solid-liquid separation to obtain a lithium-rich solution. Although the technical scheme of the application can preferentially and selectively recover lithium, a large amount of acid is adopted in the roasting process, and the acid decomposition needs to be treated. In addition, other valuable ions are inevitably present in the leachate and need to be further separated. Therefore, it is important to provide a simple and efficient method for recovering lithium.
Disclosure of Invention
1. Problems to be solved
The invention provides a method for recovering valuable metals from waste lithium ion batteries, aiming at the problems of complex process, high chemical reagent consumption and low metal recovery rate in the existing process of extracting lithium from the waste lithium ion batteries. The technical scheme of the invention can effectively solve the problems, and has the advantages of simple process, low cost, environmental protection and higher metal recovery rate and purity.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention relates to a method for recovering valuable metals from waste lithium ion batteries, which comprises the following steps:
(1) charging the waste lithium ion battery;
(2) crushing and physically sorting the charged battery to obtain a mixture of the anode material and the cathode material;
(3) calcining the mixture of the anode material and the cathode material at high temperature;
(4) and (3) placing the calcined material in water, stirring, filtering, adding sodium carbonate into the obtained filtrate to obtain lithium carbonate, wherein the obtained filter residue is a metal simple substance and an oxide thereof.
Furthermore, in the step (1), the charging mode is constant current charging, the charging cut-off voltage is 3.5-4.5V, and the charging current is 0.05-1C (1C is 180 mA/g).
Furthermore, the positive electrode material of the lithium ion battery used in the step (1) is lithium cobaltate, lithium manganate, lithium nickel cobalt manganese and multi-component lithium nickel cobalt manganese; the cathode material is carbon.
Furthermore, in the step (3), a rotary kiln is selected for calcination, the calcination temperature is controlled to be 600-800 ℃, and the calcination time is 2-5 hours.
Furthermore, in the step (3), the carbon content in the mixture is controlled to be more than 30% of the mass of the mixture during calcination, and if the carbon content is insufficient, the carbon content is supplemented.
Furthermore, in the step (2), the lithium ion battery is crushed in a closed environment filled with protective gas, and the protective gas is nitrogen or argon; the physical separation comprises screening, magnetic separation and reselection which are sequentially carried out.
Furthermore, the screening step in the step (2) comprises a coarse screen and a fine screen, wherein the screen hole of the coarse screen is 0.5-4.75 mm, and the screen hole of the fine screen is less than 0.25 mm; carrying out magnetic separation on the materials under the fine sieve, wherein the magnetic separation induction intensity is 1000 Gs; and (3) reselecting the non-magnetic separation material on a winnowing machine, taking out the diaphragm and other metal objects, finally obtaining the anode material and the cathode material, and fully and uniformly mixing the anode material and the cathode material to obtain the anode and cathode mixture.
Furthermore, in the step (4), the solid-to-liquid ratio is controlled to be 1 (3-10), the water temperature is 20-90 ℃, and the stirring time is 1-5 hours.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method for recovering valuable metals from the waste lithium ion batteries, disclosed by the invention, the recovery process and operation are optimally designed, specifically, lithium ions are transferred to a negative electrode through charging, and then the negative electrode and a positive electrode material are uniformly mixed, calcined, soaked in water and precipitated, so that lithium, nickel, cobalt and other metals can be recovered, and compared with the traditional treatment modes such as reduction acid leaching, chemical precipitation, extraction and the like, on one hand, the process operation is simplified, the addition of chemical reagents is reduced, the cost is favorably reduced, and the environmental protection requirement is met; on the other hand, the recovery rate and the purity of valuable metals in the waste lithium ion battery can be obviously improved, and the recovery rate is ensured to be higher than 95%.
(2) According to the method for recovering valuable metals from the waste lithium ion batteries, lithium ions on the anode material are transferred to the cathode in a charging mode, and partial lithium can be preferentially separated, so that the separation effect between the lithium and other metals is improved, the subsequent separation steps are simplified, a large amount of acid-base reagents are obviously reduced, and the treatment cost is favorably reduced. Meanwhile, by controlling technological parameters such as charging cut-off voltage, charging current and the like, a good lithium accumulation effect can be obtained, so that the separation effect between lithium and other metals is further improved.
(3) According to the method for recovering valuable metals from the waste lithium ion batteries, the crushed mixture of the positive electrode and the negative electrode is treated in a high-temperature calcination mode, lithium and other metals in the positive electrode material can be converted into soluble substances and insoluble substances, and recovery of different metals is realized. On one hand, lithium transferred to the negative electrode material can be converted into lithium oxide to be separated; on the other hand, the reduction action of the negative electrode can convert lithium and other metals which are not transferred from the positive electrode material into lithium oxide, metal simple substances and oxides thereof respectively, thereby being beneficial to subsequent separation. Meanwhile, the calcination temperature and time are optimally designed, and the carbon content in the mixture (the carbon content is more than 30% of the mass of the mixture) is optimized, so that the reduction reaction can be further fully performed during calcination, and the recovery rate and purity of the obtained lithium and other metals can be further ensured.
(4) The method for recovering valuable metals from waste lithium ion batteries realizes the separation of lithium from other metals through two steps of charging and reduction calcining, wherein part of lithium can be preferentially separated from a positive electrode material through charging, and the rest of lithium is separated from other metals through reduction calcining. Meanwhile, when the charged waste lithium ion battery is crushed and physically sorted, the diaphragm and other metal objects in the waste lithium ion battery can be effectively removed by optimally designing relevant process parameters of crushing and physical sorting, so that the recovery process of lithium, nickel, cobalt, manganese and other metals can be greatly simplified, and the target anode material and the target cathode material can be obtained.
(5) According to the method for recovering valuable metals from the waste lithium ion batteries, the calcined materials are dissolved in water, and factors such as water temperature and stirring time are controlled, so that the separation and recovery effects of lithium and metals such as nickel, cobalt and manganese are favorably realized, the metal recovery rate and purity are further ensured, and the method is simple in process, environment-friendly and suitable for popularization and application.
Drawings
Fig. 1 is a process flow diagram of a method for recovering valuable metals from waste lithium ion batteries according to the invention.
Detailed Description
The invention relates to a method for recovering valuable metals from waste lithium ion batteries, which comprises the following steps:
(1) charging the waste lithium ion battery;
specifically, in the lithium ion battery selected by the invention, the positive electrode material is lithium cobaltate, lithium nickelate, lithium nickel cobalt manganese oxide and multi-component lithium nickel cobalt oxide, the negative electrode material is usually carbon, and the multi-component lithium nickel cobalt oxide includes but is not limited to lithium nickel cobalt manganese aluminate and lithium nickel cobalt manganese iron lithium titanate, and any lithium nickel cobalt formed by adding other one or more metals on the basis of the lithium nickel cobalt oxide belongs to the multi-component lithium nickel cobalt oxide. And then, the lithium ion battery is charged by adopting a constant current, lithium ions move back and forth in the anode material and the cathode material in the charging and discharging process of the battery, when the battery is in a charging state, the lithium ions are separated from the anode material and are embedded into the cathode material, and partial lithium ions can be stored on the cathode by controlling the charging voltage, so that the separation effect between the lithium ions and other metals is further improved. Wherein the reaction formula in the charging process is as follows;
and (3) positive electrode: LiMO2+xe-→xLi++Li1-xMO2；
Negative electrode: c + xLi+-e-→LixC；
Where M is nickel, cobalt, etc., and x is generally less than 0.5.
It should be noted that, the invention primarily accumulates lithium ions in the waste lithium ion battery by using a charging mode, and the lithium ions move back and forth in the anode and cathode materials in the charging and discharging process of the battery. When the battery is in a charging state, lithium ions are separated from the anode material and are embedded into the cathode material, the charging voltage is controlled, and partial lithium ions can be stored on the cathode, so that the separation effect between lithium and other metals can be improved, the subsequent separation steps are simplified, the addition of a large amount of acid-base reagents is obviously reduced, and the treatment cost is favorably reduced. In actual production, because the components of the waste lithium ion battery are complex, the lithium is enriched by adopting a charging mode, and the effect of the process is greatly influenced by relevant factors. The applicant carries out a great deal of related research in consideration of the problems of lithium enrichment and simplification of the subsequent treatment process, and needs to control the magnitude of current and the charging time in addition to control the charging voltage within the range of 0-4.5V. Specifically, the charge cut-off voltage is preferably 3.5 to 4.5V, and the charge current is preferably 0.05 to 1C (1C is 180mA/g), which can provide a preferable effect.
(2) Crushing and physically sorting the charged battery to obtain a mixture of the anode material and the cathode material;
the waste lithium ion battery is crushed in a closed environment filled with protective gas, and the protective gas can be nitrogen or argon. And then, carrying out physical sorting on the crushed batteries, wherein the physical sorting process comprises screening, magnetic separation and reselection which are sequentially carried out. Specifically, the screening is mainly divided into a coarse screen and a fine screen, and during screening, the screen aperture of the coarse screen is controlled to be 0.5-4.75 mm, and the screen aperture of the fine screen is controlled to be less than 0.25 mm. And (3) carrying out magnetic separation on the materials under the fine screen, controlling the induction intensity of the magnetic separation to be 1000Gs, carrying out re-separation on the non-magnetic separation materials after the magnetic separation on a winnowing machine, taking out a battery diaphragm and other metal objects, finally obtaining a positive electrode material and a negative electrode material, and fully and uniformly mixing the positive electrode material and the negative electrode material to obtain a positive electrode and negative electrode mixture.
(3) Calcining the mixture of the anode material and the cathode material at high temperature;
according to the invention, the rotary kiln is adopted to calcine the mixture, so that the sufficient calcination of the material can be effectively ensured, and the calcination temperature is controlled to be 600-800 ℃, the calcination time is 2-5 h, and the recovery rates of lithium and other metals are improved. In the calcining process, on one hand, lithium transferred to the cathode material can be converted into lithium oxide to be separated out, and on the other hand, lithium and other metals which are not transferred out in the anode material can be converted into lithium oxide, metal simple substances and oxides thereof respectively through the reduction action of the cathode, so that the subsequent separation is facilitated. The relevant reaction formula in the calcining process is as follows:
2LixC+(2+x)/2O2→xLi2O+CO2
4LiMO2+6C+7O2→2Li2O+4M+6CO2
4LiMO2+2C+O2→2Li2O+2MO+4CO2
wherein M is nickel, cobalt, etc. In addition, in order to further improve the calcination effect and ensure that the recovery rates of the obtained lithium and other metals are more than 95% and the purity is high, the applicant researches the data obtained by experiments through a large amount of experimental researches, and by controlling the carbon content in the mixture to be more than 30% of the mass of the mixture, the reduction reaction can be fully performed during calcination, and if the content is insufficient, the supplement is performed.
(4) Placing the calcined material in water, stirring, filtering, adding sodium carbonate into the obtained filtrate to obtain lithium carbonate, wherein the obtained filter residue is a metal simple substance;
according to the invention, the calcined material is dissolved in water, lithium oxide is converted into a lithium hydroxide solution, the metal simple substance and the oxide thereof are not easy to be washed, the lithium carbonate is obtained by adding sodium carbonate into the obtained filtrate, and the obtained filter residue is the metal simple substance, so that the separation and recovery of metals such as lithium, nickel, cobalt, manganese and the like are realized. The solid-liquid ratio is controlled to be 1 (3-10), the water temperature is 20-90 ℃, the stirring time is 1-5 hours, and the reaction in the dissolving process is as follows:
Li2O+H2O→2LiOH。
the invention is further described with reference to specific examples.
Example 1
And charging the waste lithium cobalt oxide battery at a constant current of 0.2C multiplying power until the battery voltage is 4.2V, then placing the battery in a closed environment filled with nitrogen, crushing and sorting the battery to obtain a mixture of the anode material and the cathode material. Calcining the mixture at 800 ℃ for 5h, taking out calcined slag, adding deionized water according to the solid-to-liquid ratio of 1:5, stirring for 2h in a water bath at 20 ℃, carrying out solid-liquid separation on the leachate, adding sodium carbonate into the filtrate to obtain lithium carbonate precipitate, wherein the filter residue is a metal cobalt simple substance and an oxide thereof. The recovery rate of the obtained lithium and other metals is more than 95 percent, and the purity is high.
Example 2
And charging the waste lithium manganate battery at a constant current of 0.1C multiplying power until the voltage of the battery is 3.5V, and then crushing and sorting the battery in a closed environment filled with nitrogen to obtain a mixture of the anode material and the cathode material. Calcining the mixture at 700 ℃ for 10h, taking out calcined slag, adding deionized water according to the solid-liquid ratio of 1:8, stirring for 3h in a water bath at 60 ℃, carrying out solid-liquid separation on the leachate, adding sodium carbonate into the filtrate to obtain lithium carbonate precipitate, wherein the filter residue is a simple substance of metal manganese and an oxide thereof. The recovery rate of the obtained lithium and other metals is more than 95 percent, and the purity is high.
Example 3
And charging the waste nickel cobalt lithium manganate battery at a constant current of 0.5C multiplying power until the voltage of the battery is 4.5V, and then crushing and sorting the battery in a closed environment filled with nitrogen to obtain a mixture of the anode material and the cathode material. Calcining the mixture at 900 ℃ for 2h, taking out calcined slag, adding deionized water according to a solid-to-liquid ratio of 1:10, stirring for 1h in a water bath at 80 ℃, carrying out solid-liquid separation on the leachate, adding sodium carbonate into the filtrate to obtain lithium carbonate precipitate, wherein the filter residue is a metal nickel cobalt manganese simple substance and an oxide thereof. The recovery rate of the obtained lithium and other metals is more than 95 percent, and the purity is high.
Example 4
And charging the waste nickel-cobalt-manganese lithium titanate battery at a constant current of 0.05 ℃ until the voltage of the battery is 4.0V, then placing the battery in a closed environment filled with nitrogen for crushing and sorting to obtain a mixture of the anode material and the cathode material. Calcining the mixture at 650 ℃ for 6h, taking out calcined slag, adding deionized water according to the solid-to-liquid ratio of 1:3, stirring for 2h in a water bath at 90 ℃, carrying out solid-liquid separation on the leachate, adding sodium carbonate into the filtrate to obtain lithium carbonate precipitate, wherein the filter residue is a metal nickel-cobalt-manganese-titanium elementary substance and an oxide thereof. The recovery rate of the obtained lithium and other metals is more than 95 percent, and the purity is high.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention.
Claims (8)
1. A method for recovering valuable metals from waste lithium ion batteries is characterized by comprising the following steps:
(1) charging the waste lithium ion battery;
(2) crushing and physically sorting the charged battery to obtain a mixture of the anode material and the cathode material;
(3) calcining the mixture of the anode material and the cathode material at high temperature;
(4) and (3) placing the calcined material in water, stirring, filtering, adding sodium carbonate into the obtained filtrate to obtain lithium carbonate, wherein the obtained filter residue is a metal simple substance and an oxide thereof.
2. The method for recovering valuable metals from waste lithium ion batteries according to claim 1, characterized in that: in the step (1), the charging mode is constant current charging, the charging cut-off voltage is 3.5-4.5V, and the charging current is 0.05-1C (1C is 180 mA/g).
3. The method for recovering valuable metals from waste lithium ion batteries according to claim 2, characterized in that: the positive electrode material of the lithium ion battery used in the step (1) is lithium cobaltate, lithium manganate, lithium nickel cobalt manganese and multi-component lithium nickel cobalt manganese; the cathode material is carbon.
4. The method for recovering valuable metals from waste lithium ion batteries according to any one of claims 1 to 3, characterized in that: in the step (3), a rotary kiln is selected for calcination, the calcination temperature is controlled to be 600-800 ℃, and the calcination time is 2-5 hours.
5. The method for recovering valuable metals from waste lithium ion batteries according to claim 4, characterized in that: in the step (3), the carbon content in the mixture is controlled to be more than 30% of the mass of the mixture during calcination, and if the carbon content is insufficient, the carbon content is supplemented.
6. The method for recovering valuable metals from waste lithium ion batteries according to any one of claims 1 to 3, characterized in that: in the step (2), the lithium ion battery is crushed in a closed environment filled with protective gas, wherein the protective gas is nitrogen or argon; the physical separation comprises screening, magnetic separation and reselection which are sequentially carried out.
7. The method for recovering valuable metals from waste lithium ion batteries according to claim 6, characterized in that: the screening step in the step (2) comprises a coarse screen and a fine screen, wherein the screen hole of the coarse screen is 0.5-4.75 mm, and the screen hole of the fine screen is less than 0.25 mm; carrying out magnetic separation on the materials under the fine sieve, wherein the magnetic separation induction intensity is 1000 Gs; and (3) reselecting the non-magnetic separation material on a winnowing machine, taking out the diaphragm and other metal objects, finally obtaining the anode material and the cathode material, and fully and uniformly mixing the anode material and the cathode material to obtain the anode and cathode mixture.
8. The method for recovering valuable metals from waste lithium ion batteries according to any one of claims 1 to 3, characterized in that: in the step (4), the solid-liquid ratio is controlled to be 1 (3-10), the water temperature is 20-90 ℃, and the stirring time is 1-5 hours.
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| CN115011790A (en) * | 2022-05-31 | 2022-09-06 | 湖南力合厚浦科技有限公司 | Method for recovering nickel, cobalt and manganese, material obtained by recovery and recovery system |
| CN115679101A (en) * | 2021-07-13 | 2023-02-03 | 钢研晟华科技股份有限公司 | Method and device for separating and purifying anode and cathode mixed powder of waste lithium iron phosphate battery |
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