CN112048621A - Method for recovering cobalt and lithium from waste lithium cobalt oxide batteries - Google Patents
Method for recovering cobalt and lithium from waste lithium cobalt oxide batteries Download PDFInfo
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- CN112048621A CN112048621A CN202010700972.7A CN202010700972A CN112048621A CN 112048621 A CN112048621 A CN 112048621A CN 202010700972 A CN202010700972 A CN 202010700972A CN 112048621 A CN112048621 A CN 112048621A
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- C—CHEMISTRY; METALLURGY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B23/00—Obtaining nickel or cobalt
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for recovering cobalt and lithium from waste lithium cobaltate batteries, which comprises the following steps: (1) pretreating the waste lithium cobaltate battery, and separating out positive and negative active substances to obtain black powder 1; (2) placing the black powder 1 in a closed high-temperature furnace for high-temperature treatment at the temperature of 800-; (3) carrying out leaching reaction on the black powder 2 by using water, wherein the solid-to-liquid ratio is 1:20-1:100, stirring for 2-4h, dissolving lithium carbonate into a liquid phase, and keeping cobalt metal in a solid phase; then carrying out solid-liquid separation to obtain leachate and filter residue; (4) evaporating the leaching solution to obtain white powder, namely lithium carbonate; (5) drying the filter residue, and separating the metal cobalt from the filter residue by adopting a magnetic separation method. According to the invention, the lithium cobaltate is reduced by graphite at high temperature based on the existing substances in the battery, sulfuric acid leaching is not used, sodium carbonate is not used for precipitating lithium, and materials can be saved; the lithium is extracted at the front end, and the lithium recovery rate is high.
Description
Technical Field
The invention relates to the technical field of scrapped lithium battery recovery processing, in particular to a method for recovering cobalt and lithium from waste lithium cobalt oxide batteries.
Background
Lithium cobaltate batteries, as the earliest commercialized lithium ion batteries, have wide application in electronic products such as mobile phones, notebook computers and the like due to stable structure and outstanding comprehensive performance. Along with the increasing speed of the update of electronic products, the retired lithium cobalt oxide batteries are also increased rapidly. The anode material of the battery contains a large amount of cobalt and lithium elements which are scarce resources in China, particularly cobalt which is a strategic metal, 80 percent of the cobalt needs to be imported, and if the cobalt is not recycled, the cobalt is greatly wasted; on the other hand, electrolyte in the lithium ion battery can generate corrosive substances such as hydrofluoric acid when meeting water, and serious threats can be caused to the ecological environment and human health if the electrolyte is not properly treated.
The recovery treatment of waste lithium batteries is generally divided into a wet method and a dry method. The wet recovery is to transfer metal ions from electrode materials to leachate by using various acid-base solutions as transfer media, and then extract the metal ions from the solutions in the forms of salts, oxides and the like by means of extraction, precipitation and the like. However, wet recovery consumes more acid and alkali, and a large amount of high-salinity wastewater is generated in the recovery process, so that the treatment cost is high. Dry recovery generally enriches valuable components in the waste batteries by mechanical methods, high-temperature roasting and other methods, so as to achieve the purpose of recovery.
At present, the recovery of lithium cobalt oxide batteries is generally carried out by combining a dry method and a wet method. The method mainly comprises the steps of pretreatment (obtaining powder containing lithium cobaltate by crushing and sorting), leaching (acid dissolution), extraction, crystallization and the like to obtain cobalt sulfate or cobalt chloride crystals; and evaporating and concentrating the lithium-containing raffinate after cobalt extraction through a multi-effect evaporator or MVR, and finally precipitating with sodium carbonate to obtain lithium carbonate. The method has a long flow, and needs to consume a large amount of auxiliary materials such as sulfuric acid, liquid caustic soda, an extracting agent and the like; in addition, the recovery rate of lithium is low and is less than 80%.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for recovering cobalt and lithium from waste lithium cobaltate batteries, which is a method for recovering cobalt and lithium from lithium cobaltate batteries by carbothermic reduction in the air and has the advantages of simple and convenient operation and low cost.
The purpose of the invention can be realized by the following technical scheme:
a method for recovering cobalt and lithium from waste lithium cobalt oxide batteries comprises the following steps:
(1) pretreatment: pretreating a waste lithium cobaltate battery, and separating out positive and negative active substances to obtain black powder 1, wherein the black powder 1 comprises a positive material lithium cobaltate and a negative material graphite;
(2) roasting: placing the black powder 1 in a closed high-temperature furnace for high-temperature treatment at the temperature of 800 ℃ and 900 ℃ for 10-30min, and reducing lithium cobaltate by graphite to obtain black powder 2;
(3) water leaching and filtering: carrying out leaching reaction on the black powder 2 by using water, wherein the solid-to-liquid ratio is 1:20-1:100, stirring for 2-4h, dissolving lithium carbonate into a liquid phase, and keeping cobalt metal in a solid phase; then carrying out solid-liquid separation to obtain leachate and filter residue;
(4) and (3) evaporation: evaporating the leaching solution to obtain white powder, namely lithium carbonate;
(5) magnetic separation: drying the filter residue, and separating the metal cobalt from the filter residue by adopting a magnetic separation method.
Further, the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at the temperature of 400-450 ℃ for 1-1.2h to carbonize and decompose the binder and the electrolyte, so that the anode and cathode materials can fall off from the aluminum foil or the copper foil conveniently; and finally, screening the anode and cathode mixed powder by using a vibrating screen to obtain black powder 1.
Preferably, the roasting treatment in the step (2) adopts a crucible for high-temperature roasting.
Further, the roasting treatment in the step (2) specifically comprises the steps of placing the black powder 1 in a crucible, covering the crucible with a cover, and roasting at 850 ℃ for 20min to obtain the black powder 2.
Preferably, in the evaporation treatment in the step (4), an evaporation kettle is adopted.
Further, the specific method of evaporation treatment in the step (4) is to evaporate the leachate to dryness by using an evaporation kettle at 95-100 ℃ to obtain white lithium carbonate powder with the purity of 98%.
Preferably, a magnetic separator is used for magnetic separation in the magnetic separation treatment in the step (5).
Further, the step (5) of magnetic separation treatment is to dry the filter residue by using a drying kiln, and then carry out magnetic separation on the dried product by using a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so as to obtain the cobalt metal powder with the purity of 98.5%.
The invention has the beneficial effects that:
1. the method has short process flow and avoids adopting a complex extraction process flow.
2. The material is saved, the graphite reduces lithium cobaltate based on the oxidation-reduction reaction of the existing substances in the battery at high temperature, sulfuric acid leaching is not used, sodium carbonate is not used for precipitating lithium, and an extracting agent is not used for extraction.
3. The lithium recovery rate is high, lithium is extracted at the front end, the loss in a long process flow at the back end is avoided, and the recovery rate reaches over 90 percent.
4. The reaction does not need vacuum pumping or inert gas protection, and the operation is simple and convenient.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic flow chart of the method for recovering cobalt and lithium from waste lithium cobalt oxide batteries.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a method for recovering cobalt and lithium from waste lithium cobalt oxide batteries includes the following steps:
(1) pretreatment: pretreating a waste lithium cobaltate battery, and separating out anode and cathode mixed powder, wherein the mixed powder comprises anode and cathode active substances and is black powder 1;
specifically, the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at 400 ℃ for 1h to carbonize and decompose the binder and the electrolyte, so that the positive and negative electrode materials can fall off from the aluminum foil or the copper foil conveniently; and finally, screening the anode and cathode mixed powder by using a vibrating screen to obtain black powder 1.
(2) Roasting: and (3) placing the black powder 1 in a closed high-temperature furnace for high-temperature treatment at the temperature of 800-900 ℃ for 10-30min, and reducing lithium cobaltate by graphite to obtain a roasted product black powder 2.
(3) Water leaching and filtering: carrying out leaching reaction on the black powder 2 by using water, wherein the solid-to-liquid ratio is 1:20-1:100, stirring for 2-4h, dissolving lithium carbonate into a liquid phase, and keeping cobalt metal in a solid phase; then carrying out solid-liquid separation to obtain leachate and filter residue.
(4) And (3) evaporation: evaporating the leaching solution to obtain white powder, namely lithium carbonate;
specifically, the leachate is evaporated to dryness at 95 ℃ by using an evaporation kettle to obtain white lithium carbonate powder with the purity of 98%.
(5) Magnetic separation: drying the filter residue, and separating the metal cobalt from the filter residue by adopting a magnetic separation method;
specifically, the filter residue is dried by using a drying kiln, and the dried product is subjected to magnetic separation by a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so that the cobalt metal powder with the purity of 98.5% is obtained.
Example 1:
the first step is as follows: firstly, pretreating a waste lithium cobaltate battery to separate positive and negative active substances; the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at 400 ℃ for 1h to carbonize and decompose the binder and the electrolyte, so that the positive and negative electrode materials can fall off from the aluminum foil or the copper foil conveniently; finally, screening the positive and negative mixed powder by using a vibrating screen to obtain black powder 1; the black powder 1 includes a positive electrode material lithium cobaltate and a negative electrode material graphite.
The second step is that: placing the black powder 1 in a crucible, covering the crucible with a cover, and roasting at 850 ℃ for 20min to obtain black powder 2.
The third step: leaching the black powder 2 by pure water with a solid-to-liquid ratio of 1:50, stirring for 3h, and filtering to obtain a leaching solution and filter residues.
The fourth step: and evaporating the leaching solution to dryness at 95 ℃ by using an evaporation kettle to obtain white lithium carbonate powder with the purity of 98%.
The fifth step: and drying the filter residue by using a drying kiln, and then carrying out magnetic separation on the dried product by using a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so that the cobalt metal powder with the purity of 98.5% is obtained.
Example 2:
the first step is as follows: firstly, pretreating a waste lithium cobaltate battery to separate positive and negative active substances; the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at 400 ℃ for 1.2h to carbonize and decompose the binder and the electrolyte, so that the positive and negative electrode materials can fall off from the aluminum foil or the copper foil conveniently; finally, screening the positive and negative mixed powder by using a vibrating screen to obtain black powder 1; the black powder 1 includes a positive electrode material lithium cobaltate and a negative electrode material graphite.
The second step is that: placing the black powder 1 in a crucible, covering the crucible with a cover, and roasting at 800 ℃ for 30min to obtain black powder 2.
The third step: leaching the black powder 2 by pure water with a solid-to-liquid ratio of 1:20, stirring for 2h, and filtering to obtain a leaching solution and filter residues.
The fourth step: and evaporating the leaching solution to dryness by adopting an evaporation kettle at the temperature of 100 ℃ to obtain white lithium carbonate powder with the purity of 98%.
The fifth step: and drying the filter residue by using a drying kiln, and then carrying out magnetic separation on the dried product by using a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so that the cobalt metal powder with the purity of 98.3% is obtained.
Example 3:
the first step is as follows: firstly, pretreating a waste lithium cobaltate battery to separate positive and negative active substances; the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at 450 ℃ for 1h to carbonize and decompose the binder and the electrolyte, so that the positive and negative electrode materials can fall off from the aluminum foil or the copper foil conveniently; finally, screening the positive and negative mixed powder by using a vibrating screen to obtain black powder 1; the black powder 1 includes a positive electrode material lithium cobaltate and a negative electrode material graphite.
The second step is that: placing the black powder 1 in a crucible, covering the crucible with a cover, and roasting at 900 ℃ for 10min to obtain black powder 2.
The third step: leaching the black powder 2 by pure water with a solid-to-liquid ratio of 1:100, stirring for 4h, and filtering to obtain a leaching solution and filter residues.
The fourth step: and evaporating the leaching solution to dryness at 95 ℃ by using an evaporation kettle to obtain white lithium carbonate powder with the purity of 98%.
The fifth step: and drying the filter residue by using a drying kiln, and then carrying out magnetic separation on the dried product by using a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so that the cobalt metal powder with the purity of 98.7% is obtained.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned. Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A method for recovering cobalt and lithium from waste lithium cobalt oxide batteries is characterized by comprising the following steps: (1) pretreatment: pretreating a waste lithium cobaltate battery, and separating out positive and negative active substances to obtain black powder 1, wherein the black powder 1 comprises a positive material lithium cobaltate and a negative material graphite;
(2) roasting: placing the black powder 1 in a closed high-temperature furnace for high-temperature treatment at the temperature of 800 ℃ and 900 ℃ for 10-30min, and reducing lithium cobaltate by graphite to obtain black powder 2;
(3) water leaching and filtering: carrying out leaching reaction on the black powder 2 by using water, wherein the solid-to-liquid ratio is 1:20-1:100, stirring for 2-4h, dissolving lithium carbonate into a liquid phase, and keeping cobalt metal in a solid phase; then carrying out solid-liquid separation to obtain leachate and filter residue;
(4) and (3) evaporation: evaporating the leaching solution to obtain white powder, namely lithium carbonate;
(5) magnetic separation: drying the filter residue, and separating the metal cobalt from the filter residue by adopting a magnetic separation method.
2. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries as claimed in claim 1, wherein the pretreatment method comprises the following steps: firstly, discharging the waste battery by adopting a 10% sodium sulfate aqueous solution to reduce the voltage to below 1V; crushing the discharged battery in a crusher, roasting the fragments at the temperature of 400-450 ℃ for 1-1.2h to carbonize and decompose the binder and the electrolyte, so that the anode and cathode materials can fall off from the aluminum foil or the copper foil conveniently; and finally, screening the anode and cathode mixed powder by using a vibrating screen to obtain black powder 1.
3. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claims 1-2,
and (3) roasting at high temperature by using a crucible in the roasting treatment in the step (2).
4. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claims 1-3,
the roasting treatment in the step (2) specifically comprises the steps of placing the black powder 1 in a crucible, covering the crucible with a cover, and roasting at 850 ℃ for 20min to obtain black powder 2.
5. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claim 2, wherein an evaporation kettle is adopted in the evaporation treatment in the step (4).
6. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claim 5, wherein the specific method of evaporation treatment in the step (4) is to evaporate the leachate to dryness at 95-100 ℃ by using an evaporation kettle, so as to obtain white lithium carbonate powder with the purity of 98%.
7. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claim 2, wherein the magnetic separation in the step (5) is performed by using a magnetic separator.
8. The method for recovering cobalt and lithium from waste lithium cobalt oxide batteries according to claim 7, wherein the step (5) of magnetic separation treatment comprises the steps of drying filter residues by using a drying kiln, and then carrying out magnetic separation on the dried products by using a magnetic separator, wherein the magnetic field intensity is 1000 gauss, so that cobalt metal powder with the purity of 98.5% is obtained.
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| CN114381605A (en) * | 2022-03-23 | 2022-04-22 | 中南大学 | Method for comprehensively recovering valuable metals in black powder of waste lithium ion battery |
| CN114956131A (en) * | 2021-12-16 | 2022-08-30 | 昆明理工大学 | Method for recovering metal lithium and cobalt from waste lithium cobalt oxide battery positive electrode material |
| CN115893511A (en) * | 2022-12-28 | 2023-04-04 | 武汉大学 | Method for recovering waste cobalt acid lithium battery cathode material by reduction of biomass pyrolysis gas |
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