CN114883681A - Method for efficiently recovering lithium battery positive electrode material with low energy consumption - Google Patents

Method for efficiently recovering lithium battery positive electrode material with low energy consumption Download PDF

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Publication number
CN114883681A
CN114883681A CN202210483076.9A CN202210483076A CN114883681A CN 114883681 A CN114883681 A CN 114883681A CN 202210483076 A CN202210483076 A CN 202210483076A CN 114883681 A CN114883681 A CN 114883681A
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lithium battery
low
active material
energy consumption
mass
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陈振利
刘新华
冯磊
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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
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • 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
    • C22B47/00—Obtaining manganese
    • 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
    • C22B7/007—Wet processes by acid leaching
    • 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 provides a method for efficiently recovering a lithium battery positive electrode material with low energy consumption. Separating out positive active materials from waste lithium batteries, and then performing acid leaching on the active materials by using sodium hypophosphite, ammonium formate and tannic acid as reducing agents and humic acid-acrylic acid graft copolymer as a dispersing agent to obtain leachate containing recovered metal ions. The method can reduce and leach the metal in the lithium battery anode material at normal temperature, has high leaching rate and high dispersion stability, and ensures that the reduction and leaching processes can be carried out under low-speed stirring, thereby realizing low-energy-consumption and high-efficiency recovery of the metal in the lithium battery anode material.

Description

Method for efficiently recycling lithium battery cathode material with low energy consumption
Technical Field
The invention relates to the technical field of lithium battery recovery, and provides a method for efficiently recovering a lithium battery positive electrode material with low energy consumption.
Background
The lithium battery, one of the most spotlighted new energy batteries in the world today, has the advantages of long service life, low self-discharge rate, high energy density, light weight, environmental friendliness and the like, is widely applied to energy storage systems such as solar energy, water conservancy, firepower and the like, and is also widely applied to the fields of electronic products such as mobile phones, computers and the like, electric automobiles and the like.
The lithium battery mainly comprises a positive electrode, a negative electrode, a diaphragm, electrolyte (electrolyte) and a shell, and the main materials are polymer and metal materials. The waste lithium battery contains toxic and harmful substances such as heavy metals, organic electrolyte (electrolyte), polymers and the like, causes environmental pollution and influences human health, and can cause resource waste. Therefore, the recycling of the lithium battery has important significance for the development of the lithium battery industry.
At present, the recycling process of the waste lithium battery is mainly divided into pyrometallurgical process, hydrometallurgical process, biological process and the like. Pyrometallurgical processes are complex, costly and prone to the production of environmentally polluting substances. The biological metallurgy needs to culture microorganisms which can be used as metal dissolution media, the culture difficulty is high, and the effect is general. The hydrometallurgy mainly comprises the processes of leaching, precipitation, extraction and the like, wherein the leaching mainly adopts a leaching agent to dissolve target metals in the positive active material, and is a key step of the hydrometallurgy. The leaching agent conventionally adopted in hydrometallurgy is mainly acid liquor, and comprises common organic acid and inorganic acid, a certain amount of reducing agent and dispersing agent can be added during acid liquor leaching, the reducing agent can improve the leaching rate of metal, and the dispersing agent can avoid the aggregation of active materials and improve the leaching effect.
However, when the conventional acid solution leaching is used for recovering the lithium battery cathode material, not only higher temperature is required, but also high-speed stirring is required, so that the energy consumption is higher, and the leaching process is longer.
Disclosure of Invention
In order to reduce the energy consumption of metal recovery by acid liquor leaching and improve the leaching efficiency, the invention provides a method for efficiently recovering a lithium battery anode material with low energy consumption.
In order to achieve the purpose, the invention relates to the following specific technical scheme:
a method for efficiently recovering a lithium battery positive electrode material with low energy consumption comprises the following steps:
(1) discharging the recycled waste lithium batteries, then disassembling the waste lithium batteries to separate a positive electrode, a negative electrode, a diaphragm and a shell, and then separating an active material of the positive electrode and a current collector to obtain an active material;
(2) adding sodium hypophosphite, ammonium formate and tannic acid serving as reducing agents and a dispersing agent into water, mixing and stirring uniformly, adjusting the pH value to 6, then adding the active material obtained in the step (1), stirring at a low speed at normal temperature for reaction, reducing high-valence metal ions in the active material, then adding acid liquor into the system, adjusting the pH value to 2-3, continuing stirring at a low speed for leaching, and filtering to obtain a leachate containing recovered metal ions; the dispersing agent is humic acid-acrylic acid graft copolymer.
Before the waste lithium battery is recycled, the residual electric quantity is ensured to be fully consumed, and the explosion risk caused by local overheating due to rapid release of the residual electric quantity caused by battery short circuit in the disassembling process is prevented. The traditional discharge mode mainly comprises physical discharge and chemical discharge, preferably, the discharge process in the step (1) is to place the waste lithium battery into a sodium chloride solution with the mass concentration of 2-4%, discharge for 3-5h, and air-dry for later use.
After the waste lithium battery is completely discharged, the components such as the positive electrode, the negative electrode, the separator, the housing, and the like are disassembled manually or mechanically, and the active material is generally bonded to the aluminum foil by using a binder for the positive electrode. Preferably, the process of separating the active material of the positive electrode and the current collector in the step (1) is divided into 2 steps, a, the positive electrode is added into a sodium hydroxide solution with the mass concentration of 4-5% and stirred for 20-30min, so that aluminum foil falls off and is separated, the mixture is filtered and washed until the filtrate is neutral, and filter residues are dried; b. and adding the dried filter residue into an organic solvent, carrying out ultrasonic treatment for 5-8h, removing the binder, then carrying out centrifugal separation, washing with absolute ethyl alcohol, and drying to obtain the active material. More preferably, the organic solvent is at least one of N-methylpyrrolidone, dimethylacetamide, dimethylformamide and dimethylsulfoxide.
In the leaching process, acid liquor is used as a leaching agent, and metals such as cobalt, manganese, nickel, iron, lithium and the like in the anode material can be leached. Because chemical bonds among atoms of various valuable metals in the active material are extremely strong, and the valence states of cobalt, nickel and manganese are higher, if the active material is completely leached, a certain amount of reducing agent needs to be added to form an oxidation-reduction reaction, and further the leaching rate is improved. Preferably, the acid solution in the step (2) is a hydrochloric acid solution with a mass concentration of 37%.
The invention takes sodium hypophosphite, ammonium formate and tannic acid as reducing agents, can realize reduction reaction at normal temperature, has low energy consumption and simple reaction flow, and is suitable for large-scale application. During specific operation, the reducing agent and the dispersing agent are added into water and stirred uniformly, the pH value of the system is adjusted to 6, and the weak acid environment is favorable for reduction reaction. Preferably, in the step (2), the adding amount of the sodium hypophosphite is 2-3% of the mass of the water, the adding amount of the ammonium formate is 3-5% of the mass of the water, and the adding amount of the tannic acid is 2-3% of the mass of the water. Further preferably, the adding amount of the active material in the step (2) is 3-6% of the mass of water.
Since the active material is liable to aggregate, especially as the reduction and leaching proceeds, the particle size of the active material decreases and the tendency to aggregate increases, it is necessary to add a dispersant. Although tannic acid has a certain dispersing effect, the tannic acid has poor dispersion stability and needs high-speed stirring to ensure effective dispersion. The current commonly used dispersing agents (such as polyvinylpyrrolidone) also need to be stirred at a high speed to achieve a high leaching rate. The invention adopts the humic acid-acrylic acid graft copolymer as the dispersant, obviously improves the dispersion stability, can ensure that the reduction and leaching processes are carried out under low-speed stirring, and solves the problems of high-speed stirring and high energy consumption in the prior art of reduction leaching. Preferably, the addition amount of the dispersing agent is 0.03-0.05% of the mass of water. Preferably, the stirring speed of the low-speed stirring reaction in the step (2) is 30-60rpm, and the time is 30-50 min; in the step (2), the stirring speed of the low-speed stirring leaching is 30-60rpm, and the time is 10-20 min. The humic acid-acrylic acid graft copolymer can be prepared according to the prior art.
The invention provides a method for efficiently recovering a lithium battery cathode material with low energy consumption, which has the outstanding characteristics and excellent effects compared with the prior art: on one hand, the invention takes sodium hypophosphite, ammonium formate and tannic acid as reducing agents, can reduce and leach metals in the lithium battery anode material at normal temperature, and has higher leaching rate. On the other hand, the invention takes the humic acid-acrylic acid graft copolymer as the dispersant, improves the dispersion stability, and leads the reduction and leaching processes to be carried out under low-speed stirring. Therefore, the recovery process of the invention has low energy consumption and high efficiency, and is convenient for large-scale popularization and application.
Detailed Description
Example 1
(1) Discharging the recycled waste lithium cobalt oxide lithium battery, then disassembling the lithium cobalt oxide lithium battery to realize the separation of the anode, the cathode, the diaphragm and the shell, and then separating the active material of the anode and the current collector to obtain the active material; the discharging process comprises the steps of putting the waste lithium battery into a sodium chloride solution with the mass concentration of 2%, discharging for 5 hours, and air-drying for later use; firstly, adding the positive electrode into a sodium hydroxide solution with the mass concentration of 4% and stirring for 30min to enable aluminum foil to fall off and separate, filtering and washing until filtrate is neutral, and drying filter residues; b. adding the dried filter residue into N-methyl pyrrolidone, performing ultrasonic treatment for 5h, removing the binder, performing centrifugal separation, washing with absolute ethyl alcohol, and drying to obtain an active material;
(2) adding sodium hypophosphite, ammonium formate and tannic acid serving as reducing agents and a dispersing agent into water, mixing and stirring uniformly, adjusting the pH value to 6, then adding the active material obtained in the step (1), stirring at a low speed at normal temperature for reaction, reducing high-valence metal ions in the active material, then adding acid liquor into the system, adjusting the pH value to 2, continuing stirring at a low speed for leaching, and filtering to obtain a leachate containing recovered metal ions; the dispersant is humic acid-acrylic acid graft copolymer, and the addition amount of the dispersant is 0.03 percent of the mass of water; the adding amount of the active material is 6 percent of the mass of the water; the adding amount of the sodium hypophosphite is 2% of the mass of the water, the adding amount of the ammonium formate is 3% of the mass of the water, and the adding amount of the tannic acid is 2% of the mass of the water; the stirring speed of the low-speed stirring reaction is 30rpm, and the time is 40 min; the acid solution is a hydrochloric acid solution with the mass concentration of 37%; the stirring speed of the low-speed agitation leaching is 30rpm, and the time is 15 min.
Example 2
(1) Discharging the recycled waste lithium manganate battery, then disassembling to realize the separation of the anode, the cathode, the diaphragm and the shell, and then separating the active material of the anode and the current collector to obtain the active material; the discharging process comprises the steps of putting the waste lithium battery into a sodium chloride solution with the mass concentration of 3%, discharging for 4 hours, and air-drying for later use; firstly, adding the positive electrode into a sodium hydroxide solution with the mass concentration of 4.5%, stirring for 25min to enable an aluminum foil to fall off and separate, filtering and washing until filtrate is neutral, and drying filter residues; b. adding the dried filter residue into dimethylacetamide, carrying out ultrasonic treatment for 6.5h, removing the binder, then carrying out centrifugal separation, washing with absolute ethyl alcohol, and drying to obtain an active material;
(2) adding sodium hypophosphite, ammonium formate and tannic acid serving as reducing agents and a dispersing agent into water, mixing and stirring uniformly, adjusting the pH value to 6, then adding the active material obtained in the step (1), stirring at a low speed at normal temperature for reaction, reducing high-valence metal ions in the active material, then adding acid liquor into the system, adjusting the pH value to 2.5, continuing to stir and leach at a low speed, and filtering to obtain leachate containing recovered metal ions; the dispersing agent is humic acid-acrylic acid graft copolymer, and the addition amount of the dispersing agent is 0.04 percent of the mass of water; the adding amount of the active material is 4.5 percent of the mass of the water; the adding amount of the sodium hypophosphite is 2.5 percent of the mass of the water, the adding amount of the ammonium formate is 4 percent of the mass of the water, and the adding amount of the tannic acid is 2.5 percent of the mass of the water; the stirring speed of the low-speed stirring reaction is 45rpm, and the time is 40 min; the acid solution is a hydrochloric acid solution with the mass concentration of 37%; the stirring speed of the low-speed agitation leaching is 45rpm, and the time is 15 min.
Example 3
(1) Discharging the recovered waste nickel cobalt lithium manganate battery, then disassembling to realize the separation of the anode, the cathode, the diaphragm and the shell, and then separating the active material of the anode and the current collector to obtain the active material; the discharging process comprises the steps of putting the waste lithium battery into a sodium chloride solution with the mass concentration of 4%, discharging for 3 hours, and air-drying for later use; the method comprises the following steps of (a) firstly, adding the positive electrode into a sodium hydroxide solution with the mass concentration of 5% and stirring for 20min to enable an aluminum foil to fall off and separate, filtering and washing until filtrate is neutral, and drying filter residues; b. adding the dried filter residue into dimethylformamide, carrying out ultrasonic treatment for 8h, removing the binder, then carrying out centrifugal separation, washing with absolute ethyl alcohol, and drying to obtain an active material;
(2) adding sodium hypophosphite, ammonium formate and tannic acid serving as reducing agents and a dispersing agent into water, mixing and stirring uniformly, adjusting the pH value to 6, then adding the active material obtained in the step (1), stirring at a low speed at normal temperature for reaction, reducing high-valence metal ions in the active material, then adding acid liquor into the system, adjusting the pH value to 3, continuing stirring at a low speed for leaching, and filtering to obtain a leaching solution containing recovered metal ions; the dispersing agent is humic acid-acrylic acid graft copolymer, and the addition amount of the dispersing agent is 0.05 percent of the mass of water; the adding amount of the active material is 3 percent of the mass of the water; the adding amount of the sodium hypophosphite is 3% of the mass of the water, the adding amount of the ammonium formate is 5% of the mass of the water, and the adding amount of the tannic acid is 3% of the mass of the water; the stirring speed of the low-speed stirring reaction is 60rpm, and the time is 40 min; the acid solution is a hydrochloric acid solution with the mass concentration of 37%; the stirring speed of the low-speed agitation leaching is 60rpm, and the time is 15 min.
Comparative example 1
Comparative example 1 polyvinylpyrrolidone was used as the dispersant, and the rest was the same as in example 1.
Comparative example 2
Comparative example 2 polyvinylpyrrolidone was used as the dispersant, and the rest was the same as in example 2.
Comparative example 3
Comparative example 3 polyvinylpyrrolidone was used as the dispersant, the other being the same as in example 3.
The humic acid-acrylic acid graft copolymer is prepared by adopting the prior art: adding humic acid into distilled water, adjusting pH to 9 with dilute sodium hydroxide solution, heating to 70 deg.C under nitrogen protection, stirring and dissolving completely; slowly dropwise adding a potassium persulfate initiator solution and an acrylic acid solution within 1h, and then keeping the temperature for reaction for 2 h; cooling to room temperature, adjusting the pH value to be neutral by using dilute hydrochloric acid, and filtering to obtain a humic acid-acrylic acid graft copolymer; the using amount of the acrylic acid monomer is 35 percent of the mass of the humic acid; the amount of the initiator is 4% of the total mass of the humic acid and acrylic acid monomers.
And (4) performance testing: collecting the leachate and the filter residue obtained in the embodiments 1-3 and the comparative examples 1-3, drying the filter residue, cooling to room temperature, digesting by using aqua regia, and filtering to obtain a filter residue digestion solution. Performing ion analysis on the leaching solution and the filter residue digestion solution by adopting an ICP-AES (inductively coupled plasma atomic emission spectrometry) to determine the concentration of various recovered metals; and calculating the leaching rate of various recovered metals by using a formula: q = C 1 V 1 /（C 1 V 1 +C 2 V 2 ) Wherein Q is the leaching rate of each recovered metal, C 1 Concentration of each recovered metal, V, in the leach solution 1 Volume of leachate, C 2 Concentration of each recovered metal in the filter residue digestion solution, V 2 The volume of the filter residue digestion liquid is shown. The calculation results are shown in table 1.
Table 1:
Figure DEST_PATH_IMAGE001

Claims (7)

1. the method for efficiently recovering the lithium battery cathode material with low energy consumption is characterized by comprising the following steps of:
(1) discharging the recycled waste lithium batteries, then disassembling the waste lithium batteries to separate a positive electrode, a negative electrode, a diaphragm and a shell, and then separating an active material of the positive electrode and a current collector to obtain an active material;
(2) adding sodium hypophosphite, ammonium formate and tannic acid serving as reducing agents and a dispersing agent into water, mixing and stirring uniformly, adjusting the pH value to 6, then adding the active material obtained in the step (1), stirring at a low speed at normal temperature for reaction, reducing high-valence metal ions in the active material, then adding acid liquor into the system, adjusting the pH value to 2-3, continuing stirring at a low speed for leaching, and filtering to obtain a leachate containing recovered metal ions; the dispersing agent is humic acid-acrylic acid graft copolymer.
2. The method for low-energy-consumption and high-efficiency recovery of the lithium battery cathode material as claimed in claim 1, wherein the discharging process in the step (1) is to place the waste lithium battery into a sodium chloride solution with a mass concentration of 2-4%, discharge for 3-5h, and air-dry for later use.
3. The method for recovering the lithium battery cathode material with low energy consumption and high efficiency as claimed in claim 1, wherein the process of separating the active material of the cathode from the current collector in step (1) is divided into 2 steps, a, the cathode is added into a sodium hydroxide solution with a mass concentration of 4-5% and stirred for 20-30min, so that aluminum foil falls off and is separated, the solution is filtered and washed until the filtrate is neutral, and filter residues are dried; b. adding the dried filter residue into an organic solvent, carrying out ultrasonic treatment for 5-8h, removing the binder, then carrying out centrifugal separation, washing with absolute ethyl alcohol, and drying to obtain an active material; the organic solvent is at least one of N-methyl pyrrolidone, dimethylacetamide, dimethylformamide and dimethyl sulfoxide.
4. The method for recovering the lithium battery cathode material with low energy consumption and high efficiency as claimed in claim 1, wherein the adding amount of the sodium hypophosphite in the step (2) is 2-3% of the mass of water, the adding amount of the ammonium formate in the step (2) is 3-5% of the mass of water, the adding amount of the tannic acid in the step (2) is 2-3% of the mass of water, the adding amount of the dispersant in the step (2) is 0.03-0.05% of the mass of water, and the adding amount of the active material in the step (2) is 3-6% of the mass of water.
5. The method for low-energy consumption and high-efficiency recovery of the lithium battery cathode material as claimed in claim 1, wherein the stirring speed of the low-speed stirring reaction in the step (2) is 30-60rpm and the time is 30-50 min.
6. The method for recovering the lithium battery cathode material with low energy consumption and high efficiency as claimed in claim 1, wherein the acid solution in the step (2) is a hydrochloric acid solution with a mass concentration of 37%.
7. The method for low-energy consumption and high-efficiency recovery of the lithium battery cathode material according to claim 1, wherein the agitation speed of the low-speed agitation leaching in the step (2) is 30-60rpm, and the time is 10-20 min.
CN202210483076.9A 2022-05-06 2022-05-06 Method for efficiently recovering lithium battery positive electrode material with low energy consumption Pending CN114883681A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116598636A (en) * 2023-07-14 2023-08-15 兰溪博观循环科技有限公司 Method for separating and recovering valuable metals in waste ternary lithium ion battery anode materials

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116598636A (en) * 2023-07-14 2023-08-15 兰溪博观循环科技有限公司 Method for separating and recovering valuable metals in waste ternary lithium ion battery anode materials
CN116598636B (en) * 2023-07-14 2023-09-19 兰溪博观循环科技有限公司 Method for separating and recovering valuable metals in waste ternary lithium ion battery anode materials

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