CN117154270A - Method for preparing battery raw material by taking waste lithium ion battery as raw material and application - Google Patents

Method for preparing battery raw material by taking waste lithium ion battery as raw material and application Download PDF

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Publication number
CN117154270A
CN117154270A CN202310644626.5A CN202310644626A CN117154270A CN 117154270 A CN117154270 A CN 117154270A CN 202310644626 A CN202310644626 A CN 202310644626A CN 117154270 A CN117154270 A CN 117154270A
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China
Prior art keywords
raw material
battery
preparing
waste lithium
lithium ion
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CN202310644626.5A
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Chinese (zh)
Inventor
王新昌
崔彩霞
李欣
陈杨文
张亚夫
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Kaifeng Zhuojian New Energy Technology Co ltd
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Henan Zhuojian New Energy Technology Research Institute Co ltd
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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
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • 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
    • 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 preparing a battery raw material by taking a waste lithium ion battery as a raw material and application thereof. Belonging to the field of waste lithium ion battery material recovery, the method comprises the following steps: s01, discharging, disassembling and classifying the waste lithium batteries to obtain pole piece mixed powder; s02, sintering the pole piece mixed powder obtained in the step S01, and removing the binder electrolyte and acetylene black of the pole piece mixed powder; s03, washing the sintered powder in the step S02 with water to remove lithium, thereby obtaining a lithium-containing aqueous solution; s04, placing the washed lithium powder in the step S03 into an alkali solution to remove aluminum iron impurities, and performing suction filtration separation; s05, placing filter residues obtained in the step S04 into pickle liquor for leaching; s06, carrying out further impurity removal on the metal leaching solution obtained in the step S05 to obtain a high-purity solution containing nickel, cobalt and manganese, and obtaining the raw material for preparing the new battery. The leaching process is safe and controllable, is environment-friendly, greatly reduces the risks of drug transportation and storage, and has good industrial prospect.

Description

Method for preparing battery raw material by taking waste lithium ion battery as raw material and application
Technical Field
The invention belongs to the field of waste lithium ion battery material recovery, and particularly relates to a method for preparing a battery raw material by taking a waste lithium ion battery as a raw material and application thereof.
Background
With the adjustment of global energy structures and the development of technologies such as electronic information, lithium ion batteries are required for power supply from mobile phones, notebook computers to electric automobiles, and a lot of waste caused after the use is over is increasing at a remarkable speed. Meanwhile, the shortage of lithium ion battery raw materials also causes the trend of reutilization of waste materials to generate more critical urgent sense. If the waste battery is not well solved, the cost of enterprises is increased, the natural ecological environment is destroyed, and the waste battery is harmful to the healthy development of human beings. The data show that if the waste lithium batteries can be fully recovered, 240 tons of cobalt can be recovered each year, and the value can reach more than 4000 ten thousand yuan; if the mobile phone battery is abandoned on the land, 1 square kilometer land can be polluted for about 50 years by 1 mobile phone battery of 20 g. Therefore, the recycling of the waste lithium batteries is not only in view of the environmental protection requirement, but also meets the requirements of the concept of recycling economy and sustainable development.
At present, after the pretreatment such as disassembly and crushing of the waste batteries, the recovery method of the positive electrode powder of the lithium batteries generally comprises three technologies of pyrometallurgy, hydrometallurgy and bioleaching. The pyrometallurgical technology has the advantages of high energy consumption, serious pollution and high process cost, and a lot of valuable components can be lost in the treatment process, and toxic and harmful gases are generated; the biological leaching technology has long leaching period, difficult strain culture, poor treatment effect and low efficiency. Compared with other technologies, hydrometallurgy has the advantages of small pollution, low energy consumption, high leaching efficiency and the like, and is widely applied to the field of metal recovery. Wherein the wet recovery process includes a physical process portion and a chemical process portion. The physical process comprises discharging, disassembling and pulverizing of lithium batteryCrushing and sieving. The chemical process mainly involves alkaline leaching, acid leaching, precipitation, extraction, etc., wherein the leaching process is the key of wet recovery. In the acid leaching process, a large amount of acid liquor is required, and in the traditional leaching process, inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid and the like is mainly used as a leaching agent, and Cl is released in the leaching process 2 、SO 3 、NO x And harmful gases, such as pollution to the environment and harm to human health. In recent years, organic acid leaching gradually replaces inorganic acid leaching, and becomes a new research hot spot. Such as citric acid, malic acid, oxalic acid, succinic acid, tartaric acid, ascorbic acid, etc., the organic acid is mostly extracted from plants or foods, no dirty acid is generated in the leaching process, and the organic acid can be recycled.
At present, the most widely used reducing agent is hydrogen peroxide, and the hydrogen peroxide is used as the reducing agent and cannot introduce impurity ions in the reaction process. However, hydrogen peroxide is unstable, is easy to decompose in the heating leaching process, has severe reduction reaction and releases oxygen, so that the hydrogen peroxide utilization rate is low and the controllability of the leaching process is low. Also by NaHSO 3 Or Na (or) 2 SO 3 As a reducing agent, but SO is easily released during the reaction 2 Gas, causing atmospheric pollution. In summary, the selection of the leaching acid and the reducing agent is an extremely important link in the wet recovery process of valuable metals in the waste lithium batteries.
The invention directly adopts the organic acid system with reducibility to realize the leaching of valuable metals in the waste lithium batteries, which has not been reported at home and abroad. Compared with the currently reported leaching system and leaching method, the method has the advantages of environmental protection, safe and controllable leaching process, convenient and fast medicament transportation, obvious innovation, and better industrial application prospect.
Disclosure of Invention
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for preparing battery raw materials by taking waste lithium ion batteries as raw materials comprises the following steps:
s01, discharging, disassembling and classifying the waste lithium batteries to obtain pole piece mixed powder, wherein the pole piece mixed powder consists of positive and negative electrode materials, a small amount of current collector and binder electrolyte;
s02, sintering the pole piece mixed powder obtained in the step S01, and removing the binder electrolyte and acetylene black of the pole piece mixed powder;
s03, washing the sintered powder in the step S02 with water to remove lithium, thereby obtaining a lithium-containing aqueous solution;
s04, placing the washed lithium powder in the step S03 into an alkali solution to remove aluminum iron impurities, and performing suction filtration separation;
s05, placing filter residues obtained in the step S04 into pickle liquor for leaching;
s06, further removing impurities from the metal leaching solution obtained in the step S05 to obtain a high-purity solution containing nickel, cobalt and manganese, and obtaining the raw material for preparing the new battery.
In one embodiment, in step S02, the calcination temperature is 400 ℃ to 800 ℃ and the calcination time is 2 to 8 hours.
In one embodiment, in step S03, the water wash temperature is 40 ℃ to 90 ℃.
In one embodiment, in step S04, the alkali solution is one or more of sodium hydroxide or potassium hydroxide, the concentration of the alkali solution is 0.5mol/L to 5mol/L, the reaction time is 1 to 4 hours, and the reaction temperature is 40 ℃ to 70 ℃.
In one embodiment, in step S05, the pickling solution is selected from two or more of ascorbic acid, citric acid, malic acid, formic acid, sulfonic acid and tartaric acid, wherein the concentration of the pickling solution is 1mol/L-8mol/L, the reaction time is 2-6h, and the reaction temperature is 40-90 ℃.
In one embodiment, in step S06, the metal leach solution is one or more of bis (2-ethylhexyl) phosphate, 2-ethylhexyl phosphate mono, copper extractant M5640.
An application of waste lithium ion battery as raw material in preparing battery raw material for preparing battery anode material.
The beneficial effects of the invention are that
The invention has reasonable design, in the treatment process of the waste lithium ion battery, the traditional acid leaching step mainly uses inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid and the like as a leaching agent, and meanwhile, the leaching rate is improved by matching with a reducing agent, but the inorganic acid has strong corrosiveness, and has certain danger in both transportation and storage. A large amount of harmful gas is released in the reaction process, which causes harm to human body, environment and the like. The use of reducing agents also causes some harm and increases costs. The invention uses the organic acid with reducibility to leach, the leaching process is safe and controllable, the environment is friendly, the danger of drug transportation and storage is greatly reduced, and the invention has good industrial prospect.
Drawings
FIG. 1 is a process flow diagram of a process for preparing a battery raw material from waste lithium ions;
FIG. 2 is a graph showing experimental leaching content data of a specific example of a battery raw material prepared from waste lithium ions;
FIG. 3 is a graph showing experimental leaching rate data for a specific example of a battery raw material prepared from waste lithium ions;
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods described in the examples of the present invention are conventional methods unless otherwise specified.
Example 1
A method for preparing battery raw materials by taking waste lithium ion batteries as raw materials comprises the following steps:
step S01, disassembling the waste lithium battery after discharging, and removing the shell and the diaphragm to obtain anode-cathode mixed black powder;
step S02, sintering the mixed black powder at the high temperature of 400 ℃ for 2 hours, wherein the binder electrolyte and acetylene black in the mixed black powder are removed in the whole calcination process;
step S03, grinding and crushing the powder sintered in the step S02, washing the ground powder with water at 40 ℃ to remove lithium, and carrying out suction filtration to obtain a lithium-containing aqueous solution and filter residues, wherein the filter residues are subjected to the next treatment;
step S04, carrying out alkaline leaching on the filter residue obtained in the step S03 to remove impurities such as iron and aluminum, wherein the alkaline leaching solution is 0.5mol/L sodium hydroxide solution, the alkaline leaching reaction temperature is 40 ℃, the reaction time is 1h, then carrying out suction filtration on the solution, separating the filter residue from filtrate, and carrying out next utilization on the filter residue;
step S05, carrying out acid leaching on the filter residues in the step S04, wherein the acid leaching solution is a combination of two or more organic acids such as ascorbic acid, citric acid, malic acid, formic acid, sulfonic acid, tartaric acid and the like, the concentration of the acid leaching solution is 1mol/L, the acid leaching reaction time is 2h, the reaction temperature is 40 ℃, and the ion solution containing nickel-cobalt-manganese-lithium valuable metals is obtained through suction filtration;
step S06, the metal leaching solution obtained in step S05 is subjected to further impurity removal (P204, P507 and M5640 extraction impurity removal) to obtain a high-purity solution containing nickel, cobalt and manganese, and the high-purity solution can be used as a raw material for preparing a new battery.
Example 2
A method for preparing battery raw materials by taking waste lithium ion batteries as raw materials comprises the following steps:
step S01, disassembling the waste lithium battery after discharging, and removing the shell and the diaphragm to obtain anode-cathode mixed black powder;
step S02, sintering the mixed black powder at the high temperature of 600 ℃ for 4 hours, wherein the binder electrolyte and acetylene black in the mixed black powder are removed in the whole calcination process;
step S03, grinding and crushing the powder sintered in the step S02, washing the ground powder with water at 70 ℃ to remove lithium, and carrying out suction filtration to obtain a lithium-containing aqueous solution and filter residues, wherein the filter residues are subjected to the next treatment;
step S04, carrying out alkaline leaching on the filter residue treated in the step S03 to remove impurities such as iron and aluminum, wherein the alkaline leaching solution is a sodium hydroxide solution with the concentration of 2mol/L, the alkaline leaching reaction temperature is 50 ℃, the reaction time is 2 hours, carrying out suction filtration, separating the filter residue from filtrate, and carrying out next utilization on the filter residue;
step S05, carrying out acid leaching on the filter residues in the step S04, wherein the acid leaching solution is a combination of two or more organic acids such as ascorbic acid, citric acid, malic acid, formic acid, sulfonic acid, tartaric acid and the like, the concentration of the acid leaching solution is 4mol/L, the acid leaching reaction time is 4 hours, the reaction temperature is 60 ℃, and the ion solution containing nickel-cobalt-manganese-lithium valuable metals is obtained through suction filtration;
step S06, the metal leaching solution obtained in step S05 is subjected to further impurity removal (P204, P507 and M5640 extraction impurity removal) to obtain a high-purity solution containing nickel, cobalt and manganese, and the high-purity solution can be used as a raw material for preparing a new battery.
Example 3
A method for preparing battery raw materials by taking waste lithium ion batteries as raw materials comprises the following steps:
step S01, disassembling the waste lithium battery after discharging, removing a shell, a diaphragm and the like to obtain anode-cathode mixed black powder;
step S02, sintering the mixed black powder at a high temperature of 800 ℃ for 6 hours, wherein the binder electrolyte and acetylene black in the mixed black powder are removed in the whole calcination process;
step S03, grinding and crushing the powder sintered in the step S02, washing the ground powder with water at 90 ℃ to remove lithium to obtain a lithium-containing aqueous solution, and carrying out the next treatment on filter residues;
step S04, carrying out alkaline leaching on the filter residue treated in the step S03 to remove impurities such as iron and aluminum, wherein the alkaline leaching solution is 5mol/L sodium hydroxide solution, the reaction temperature is 70 ℃, the reaction time is 4 hours, carrying out suction filtration, separating the filter residue from filtrate, and carrying out next utilization on the filter residue;
step S05, carrying out acid leaching on the filter residues in the step S04, wherein the acid leaching solution is a combination of two or more organic acids such as ascorbic acid, citric acid, malic acid, formic acid, sulfonic acid, tartaric acid and the like, the concentration of the acid leaching solution is 8mol/L, the reaction time is 6h, the reaction temperature is 90 ℃, and the ion solution containing nickel-cobalt-manganese-lithium valuable metals is obtained through suction filtration;
step S06, the metal leaching solution obtained in step S05 is subjected to further impurity removal (P204, P507 and M5640 extraction impurity removal) to obtain a high-purity solution containing nickel, cobalt and manganese, and the high-purity solution can be used as a raw material for preparing a new battery.

Claims (7)

1. The method for preparing the battery raw material by taking the waste lithium ion battery as the raw material is characterized by comprising the following steps:
s01, discharging, disassembling and classifying the waste lithium batteries to obtain pole piece mixed powder, wherein the pole piece mixed powder consists of positive and negative electrode materials, a small amount of current collector and binder electrolyte;
s02, sintering the pole piece mixed powder obtained in the step S01, and removing the binder electrolyte and acetylene black of the pole piece mixed powder;
s03, washing the sintered powder in the step S02 with water to remove lithium, thereby obtaining a lithium-containing aqueous solution;
s04, placing the washed lithium powder in the step S03 into an alkali solution to remove aluminum iron impurities, and performing suction filtration separation;
s05, placing filter residues obtained in the step S04 into pickle liquor for leaching;
s06, further removing impurities from the metal leaching solution obtained in the step S05 to obtain a high-purity solution containing nickel, cobalt and manganese, and obtaining the raw material for preparing the new battery.
2. The method for preparing a battery raw material from waste lithium ion batteries according to claim 1, wherein in step S02, the calcination temperature is 400-800 ℃ and the calcination time is 2-8 hours.
3. The method for producing a battery raw material from a waste lithium ion battery according to claim 1, wherein in step S03, the water washing temperature is 40 ℃ to 90 ℃.
4. The method for preparing the battery raw material by taking the waste lithium ion battery as the raw material according to claim 1, wherein in the step S04, the alkali solution is one or more of sodium hydroxide and potassium hydroxide, the concentration of the alkali solution is 0.5mol/L-5mol/L, the reaction time is 1-4h, and the reaction temperature is 40-70 ℃.
5. The method for preparing the battery raw material by taking the waste lithium ion battery as the raw material according to claim 1, wherein in the step S05, the pickling solution is a combination of two or more of ascorbic acid, citric acid, malic acid, formic acid, sulfonic acid and tartaric acid, the concentration of the pickling solution is 1mol/L-8mol/L, the reaction time is 2-6h, and the reaction temperature is 40-90 ℃.
6. The method for preparing a battery raw material from waste lithium ion batteries according to claim 1, wherein in step S06, the metal leaching solution is one or more of bis (2-ethylhexyl) phosphate, 2-ethylhexyl phosphate, and copper extractant M5640.
7. Use of a waste lithium ion battery as a raw material for preparing a battery positive electrode material according to any one of claims 1 to 6.
CN202310644626.5A 2023-06-01 2023-06-01 Method for preparing battery raw material by taking waste lithium ion battery as raw material and application Pending CN117154270A (en)

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CN202310644626.5A CN117154270A (en) 2023-06-01 2023-06-01 Method for preparing battery raw material by taking waste lithium ion battery as raw material and application

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CN202310644626.5A CN117154270A (en) 2023-06-01 2023-06-01 Method for preparing battery raw material by taking waste lithium ion battery as raw material and application

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