CN112310498A - Method for preparing nickel-cobalt-manganese ternary material precursor by using waste ternary battery - Google Patents
Method for preparing nickel-cobalt-manganese ternary material precursor by using waste ternary battery Download PDFInfo
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- CN112310498A CN112310498A CN201910692174.1A CN201910692174A CN112310498A CN 112310498 A CN112310498 A CN 112310498A CN 201910692174 A CN201910692174 A CN 201910692174A CN 112310498 A CN112310498 A CN 112310498A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses a method for preparing a high-nickel-cobalt-manganese ternary material precursor by utilizing nickel-cobalt-manganese slag, which comprises the following steps of: step (1): washing and cleaning the disassembled anode slag of the waste ternary battery, and then carrying out solid-liquid separation to obtain a washing material; step (2): reducing and leaching the water washing material by hydrogen peroxide, chemically removing impurities, extracting and purifying to obtain a nickel-cobalt-manganese solution; and (3): regulating and controlling the ion molar ratio of nickel, cobalt and manganese, and then preparing the high-nickel, cobalt and manganese ternary material precursor through coprecipitation. In the invention, the disassembled anode slag of the waste ternary battery is subjected to reduction leaching, impurity removal, purification and coprecipitation, so that the high-nickel-cobalt-manganese ternary material precursor meeting the requirements is further prepared.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to a method for preparing a high-nickel-cobalt-manganese ternary positive electrode material precursor by utilizing a waste ternary battery.
Background
Since the commercialization of the lithium ion battery was realized in the last 90 years, the lithium ion battery has been widely used in cameras, mobile phones, notebook computers, portable measuring instruments and the like due to its advantages of high energy density, high voltage, good cycle performance, small self-discharge, safe operation and the like. A large amount of lithium ion batteries are produced and consumed every year in China, the rate of the lithium ion batteries is increased by more than 10% every year, and the recovery rate of waste batteries in China is not more than 5% and is far lower than that in developed countries. Numerous scientific research institutions at home and abroad carry out a great deal of work on waste battery recovery, and although the recovery methods are numerous, the recovery process usually comprises three steps: pretreatment of the battery, separation of active substances and a current collector, and recycling of valuable metals.
After the battery is discharged, the industry typically uses mechanical crushing. In a lithium battery, a certain amount of NMP (N-methylpyrrolidone) organic binder is present, and it is necessary to separate the active material from the binder by soaking, calcining, or the like before recovering the active material. The recovery of active substances is generally realized by immersing valuable metals into a solution by adopting a hydrometallurgy process and achieving the aim of recovering waste batteries through the purification and separation of the metals. The recycling of consumer batteries has become widespread in industry, while the recycling of power batteries is still in the beginning. The scrappage of the waste power lithium ion battery reaches 20 ten thousand tons in 2020, and the recovery value is very high. At present, the scrappage of the power battery is less, and the retired part is used for research by colleges and scientific research units. In fact, the route for recycling the power battery is complex, the recycling difficulty is large, the cost is high, the yield is not clear, and the related standards for recycling the power battery are still in the process.
With the increase of the number of the waste ternary batteries year by year, the demand pressure of nickel-cobalt-manganese resources can be effectively relieved by recovering nickel, cobalt and manganese from the waste ternary batteries, and the sustainable development of nickel-cobalt-manganese alloy can be realized. The recovery of waste batteries has been studied very early in developed countries in europe and america, and a series of achievements have been achieved. Generally, the anode material disassembled is used as an anode for dissolution by an electrochemical method, and when the voltage reaches a certain value under the action of current, the metal in the anode material undergoes an oxidation reaction and enters the solution. The recycled waste batteries can also be mechanically crushed and then ball-milled to obtain the mixed alloy material. Under the condition of high temperature, cobalt and zinc can form cobalt-zinc alloy, and the regenerated hard alloy is prepared by the conventional process after crushing and grinding. However, the method has low recovery rate and long process flow time, and cannot be used on a large scale. Raney-Ni alloys can also be recovered by acid leaching the nickel and cobalt under reducing conditions. Practice has proved that each method for recovering the alloy has certain limitations and needs to be combined with a plurality of methods.
Disclosure of Invention
In order to overcome the defects of high cost, complex process and the like in the prior art, the invention provides a method for preparing a high-nickel-cobalt-manganese ternary positive electrode material precursor by utilizing a waste ternary battery; aiming at simplifying the process and reducing the process cost.
A method for preparing a nickel-cobalt-manganese ternary material precursor by using a waste ternary battery comprises the following steps:
step (1): washing and cleaning the disassembled anode material of the waste ternary battery to obtain a washing material;
step (2): mixing the washing material, hydrogen peroxide and sulfuric acid for reduction leaching, and then carrying out chemical impurity removal and extraction purification to obtain a nickel-cobalt-manganese solution;
and (3): regulating and controlling the proportion of nickel, cobalt and manganese in the nickel, cobalt and manganese solution to obtain a precursor solution, and then carrying out coprecipitation to obtain the nickel, cobalt and manganese ternary material precursor.
According to the invention, the disassembled anode slag of the waste ternary battery is washed and cleaned by water, then the washed material is obtained through solid-liquid separation, and then the reduction leaching, impurity removal, purification and nickel source coprecipitation are carried out, so that the high-nickel, cobalt and manganese ternary material precursor meeting the requirements is further prepared. The method does not need to carry out independent pretreatment on various nickel-cobalt-manganese slag materials, greatly simplifies the treatment process, obviously reduces the preparation cost, does not need special equipment, and is suitable for industrial large-scale production.
The positive electrode material can be obtained by adopting the existing method, for example, the positive electrode plate is crushed and stripped at high temperature to obtain the positive electrode material.
In the invention, hydrogen peroxide is preferably used as a reducing agent; sulfuric acid is used as the leaching solution.
Preferably, in the step (2), the concentration of the hydrogen peroxide is 20-30 wt%, and the adding amount is 1.5-3 times of the theoretical amount.
Preferably, in the step (2), the molar concentration of the sulfuric acid adopted in the reduction leaching process is 1.0-3 mol/L.
The volume of the hydrogen peroxide and the weight ratio of the water washing material are 2-8 ml/g. Namely adding 2-8 ml of hydrogen peroxide into each gram of washing material.
Preferably, the temperature of the reduction leaching is 30-100 ℃; more preferably 50 to 70 ℃.
Preferably, in the step (2), in the reduction leaching process, the liquid-solid volume-to-weight ratio is 5-10 mL: 1g of the total weight of the composition. Namely, 5-10 mL of sulfuric acid and hydrogen peroxide are added into each gram of the washing material.
Under the condition of the reduction leaching process, the preferable reduction leaching time is 2-4 h.
In the invention, the reduction leachate contains nickel, cobalt, manganese, iron, aluminum and other ions, and the pH gradient impurity removal method is preferably adopted to carry out impurity removal treatment on the reduction leachate.
Preferably, the impurity removal process comprises:
(a) firstly, adjusting the pH value of a system to be 1.0-1.5 by using an alkali metal hydroxide;
(b) adjusting the pH value of the system to 2.5-3.0 by using alkali carbonate, and reacting at 90-95 ℃ under the condition of maintaining the pH value;
(c) and performing solid-liquid separation to obtain a filtrate, then regulating the pH value of the filtrate to 3.5-4, then adding ammonium fluoride, and performing solid-liquid separation to obtain an impurity-removed solution.
The alkali metal hydroxide is, for example, sodium hydroxide, and the alkali metal carbonate is, for example, sodium carbonate.
Further preferably, in the step (2), the chemical impurity removal step for the reduction leachate comprises: adjusting the pH value of the reduction leaching solution to 1.0-1.5 by using an alkali metal hydroxide, and stirring for 1.0-2.0 h; then adjusting the pH value to 2.0-3.0 by using alkali metal carbonate, heating to 80-95 ℃, stirring and maintaining the pH value for 1.0-2.0 h; then cooling to room temperature, adjusting the pH value to 3.5-4.0, adding ammonium fluoride, stirring for reaction for 1.0-2.0 h, and filtering to obtain the nickel-cobalt-manganese impurity-removing solution.
In the invention, the nickel-cobalt-manganese impurity-removed liquid after chemical impurity removal in the step (2) is subjected to extraction purification treatment to obtain nickel-cobalt-manganese purified liquid (nickel-cobalt-manganese solution).
Preferably, in the step (2), in the extraction and purification process, the adopted extracting agent is P204-sulfonated kerosene, the volume percentages of P204 and sulfonated kerosene are respectively 10-30% and 90-70%, and the saponification rate of P204 is 20-80%.
Preferably, the extraction in the step (2) adopts 5-10 stages of extraction, and the extraction time of each stage is 3-5 minutes.
In the present invention, the preferred extraction method is countercurrent extraction.
In the invention, nickel sulfate solution and a certain amount of high-purity cobalt are prepared into the nickel-cobalt-manganese purification solution obtained in the step (2), the molar ratio of nickel, cobalt and manganese is in a required ratio (5: 2: 3, 6:2:2, 8:1:1 and the like) to obtain precursor solution, and then coprecipitation treatment is carried out to obtain the precursor.
And (3) coprecipitating the precursor solution with alkali and ammonia water, and washing and drying the obtained solid after the reaction is finished to obtain the high-nickel-cobalt-manganese ternary cathode material precursor.
Preferably, in the step (3), in the coprecipitation process, the concentration of the nickel-cobalt-manganese mixed ions in the precursor solution is 1-3 mol/L.
The concentration of the alkali is 1.0-5.0 mol/L.
The concentration of ammonia water is 1-3 mol/L.
The coprecipitation reaction temperature is 30-80 ℃.
And keeping the pH value to be 10-12 in the coprecipitation reaction process.
In the step (3), the ammonia content in the reaction system is controlled to be 1-5 g/L.
And (3) after the coprecipitation reaction is finished, carrying out solid-liquid separation on the reaction liquid, and washing and drying the obtained solid to obtain the high-nickel-cobalt-manganese ternary cathode material precursor.
In the invention, the nickel/cobalt ratio is regulated and controlled by regulating and controlling the parameters of the acid leaching process, so that the nickel/cobalt grouping recycling is realized, the process is simple and the cost is low.
Advantageous effects
The method does not need to carry out independent pretreatment on various nickel-cobalt-manganese slag materials, greatly simplifies the treatment process, obviously reduces the preparation cost, does not need special equipment, and is suitable for industrial large-scale production.
The invention innovatively discovers that the NCM precursor without impurity phase can be obtained by adopting the water washing-reduction leaching-gradient impurity removal-extraction process. The NCM precursor with high crystalline phase and purity can not be obtained by any process, such as water washing, gradient impurity removal process, required pH condition and combined extraction condition.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The following examples are intended to illustrate the invention without further limiting it.
Example 1
The raw materials adopted in the embodiment are purchased waste ternary lithium batteries and nickel sulfate.
Step (1): firstly, disassembling a waste ternary battery to obtain a positive electrode material, adding the positive electrode material into water, and stirring and cleaning for 2 hours at the temperature of 20-50 ℃. And filtering, washing and drying the solution after the water washing reaction to obtain the water washing material.
Step (2):
step (2-a): reduction leaching:
adding 1.5mol/L sulfuric acid (the volume of the sulfuric acid is 10mL/g of the nickel cobalt manganese acid leaching residue material weight ratio) and 30 wt% of hydrogen peroxide (the volume of the hydrogen peroxide is 2.0mL/g of the nickel cobalt manganese acid leaching residue material weight ratio) into the nickel cobalt manganese acid washing material prepared in the step (1); controlling the reaction temperature to be 50 ℃ and the reaction time to be 3 h; obtaining the nickel-cobalt-manganese reduction leaching solution, wherein the main ions are nickel, cobalt, manganese, iron, aluminum and the like.
Step (2-b): chemical impurity removal of reduction leaching solution:
taking a nickel-cobalt-manganese reduction leaching solution, adding a NaOH solution with the mass fraction of 10% into the solution to adjust the pH value (1.0-1.5), stirring for 1.0h, then adding saturated sodium carbonate to adjust the pH value to 2.5-3.0, adding alkali into the reaction at the temperature of 90-95 ℃ to keep the pH value stable for reaction for 150min, and cooling and filtering. Adjusting the pH value of the solution to 4, adding 1.5 times of ammonium fluoride, and reacting for two hours at normal temperature; filtering to obtain the impurity-removing solution of nickel, cobalt and manganese.
Step (2-c): extraction and purification:
a mixed solution of 30 volume percent of p204 (the saponification rate is 30 percent) and 70 volume percent of sulfonated kerosene is adopted as an extracting agent; the volume ratio of the components is 1: the extracting agent of 1 is used for extracting the nickel-cobalt-manganese impurity-removed liquid, and the extraction grade is 5 to 8; the extraction mode is countercurrent extraction, and the extraction purification liquid is obtained by enrichment.
And (3): adding nickel sulfate into the extraction purification solution to ensure that the molar ratio of nickel, cobalt and manganese is 5: 3: 2; the total ion concentration of nickel, cobalt and manganese is 2mol/L, ammonia water and sodium hydroxide (1.5mol/L) are added into a coprecipitation reaction kettle for coprecipitation reaction, the pH value of a reaction system is controlled to be 11 in the reaction process, the ammonia content of the reaction system is controlled to be 2g/L, the temperature of the reaction system is controlled to be 50 ℃, the stirring speed is 500r/min, argon is introduced for protection, the argon flow is 0.6ml/min, and the reaction is carried out for 5 hours. And after the coprecipitation reaction is finished, continuously stirring the obtained slurry, aging for 2h at 50 ℃, washing with water until the pH value of the filtrate is 8.0, and drying for 10h at 100 ℃ to obtain the high-nickel ternary cathode material precursor with extremely low impurity content (no impurity phase is detected by XRD).
Example 2
Compared with the example 1, the difference is only that in the step (2-a) reduction leaching, sulfuric acid with the concentration of 2.0mol/L is added into the nickel cobalt manganic acid leaching residue material prepared in the step (1).
Example 3
The only difference compared to example 1 is that in step (1), step (3): adding a nickel source solution into the extraction purification solution, and introducing a small amount of nickel, cobalt and manganese from the outside to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, then coprecipitating to prepare a high-nickel ternary cathode material precursor (no impurity phase is detected by XRD).
Claims (10)
1. A method for preparing a nickel-cobalt-manganese ternary material precursor by using a waste ternary battery is characterized by comprising the following steps:
step (1): washing and cleaning the disassembled anode material of the waste ternary battery to obtain a washing material;
step (2): mixing the washing material, hydrogen peroxide and sulfuric acid for reduction leaching, and then carrying out chemical impurity removal and extraction purification to obtain a nickel-cobalt-manganese solution;
and (3): regulating and controlling the proportion of nickel, cobalt and manganese in the nickel, cobalt and manganese solution to obtain a precursor solution, and then carrying out coprecipitation to obtain the nickel, cobalt and manganese ternary material precursor.
2. The method as claimed in claim 1, wherein in the step (2), the concentration of the hydrogen peroxide is 20-30 wt%, and the adding amount is 1.5-3 times of the theoretical amount;
the molar concentration of the sulfuric acid in the reduction leaching process is 1.0-3 mol/L.
3. A method according to claim 2, wherein the temperature of the reductive leach is 30-100 ℃.
4. A method according to claim 3, wherein the reduction leaching is carried out for a period of 2 to 4 hours.
5. The method of claim 1, wherein the dedoping process comprises:
(a) firstly, adjusting the pH value of a system to be 1.0-1.5 by using an alkali metal hydroxide;
(b) adjusting the pH value of the system to 2.5-3.0 by using alkali carbonate, and reacting at 90-95 ℃ under the condition of maintaining the pH value;
(c) and performing solid-liquid separation to obtain a filtrate, then regulating the pH value of the filtrate to 3.5-4, then adding ammonium fluoride, and performing solid-liquid separation to obtain an impurity-removed solution.
6. The method of claim 1, wherein in the step (2), the extracting agent used in the extraction purification process is P204-sulfonated kerosene, the volume percentages of P204 and sulfonated kerosene are 10-30% and 90-70%, respectively, and the saponification rate of P204 is 20-80%.
7. The method of claim 6, wherein the extraction in step (2) is performed by 5-10 stages of counter-current extraction, and the extraction time of each stage is 3-5 minutes.
8. The method according to claim 1, wherein in the step (3), the molar ratio of the elements of nickel, cobalt and manganese in the precursor solution is 5-8: 1-3: 1-2; more preferably 5: 2: 3. 6:2:2 or 8:1: 1.
9. The method of claim 8, wherein in step (3), the concentration of total ions in the precursor solution is controlled, and ammonia and a base are added to perform the co-precipitation.
10. The method according to claim 9, wherein in the step (3), the concentration of the mixed ions in the precursor solution is 1 to 3 mol/L; in the reaction process, alkali is used for maintaining the pH of the system to be 10-12; controlling the ammonia content in the reaction system to be 1-5 g/L;
the temperature of the coprecipitation reaction is 30-80 ℃.
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| CN115924989A (en) * | 2022-11-30 | 2023-04-07 | 宁波力勤资源科技股份有限公司 | Method for recycling nickel cobalt hydroxide from waste ternary batteries |
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