CN111477985B - Method for recycling waste lithium ion batteries - Google Patents
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- CN111477985B CN111477985B CN202010294915.3A CN202010294915A CN111477985B CN 111477985 B CN111477985 B CN 111477985B CN 202010294915 A CN202010294915 A CN 202010294915A CN 111477985 B CN111477985 B CN 111477985B
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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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- 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
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Abstract
The invention provides a method for recycling waste lithium ion batteries, which comprises the following steps: step one, soaking discharge: step two, disassembling: step three, active substance separation: step four, drying and crushing: leaching: step six, precipitation: step seven, preliminary ammonia distillation: and step eight, electrolysis. The method can prepare the transition metal in the waste lithium ion battery into a positive electrode material precursor with high added value, and lithium is recycled by lithium carbonate or lithium hydroxide; meanwhile, the harmful electrolyte, binder and other organic components in the waste batteries are recycled, and the organic solvent for leaching can be recycled; realizing the closed cycle of the leaching agent, the complexing agent and the precipitant in the process flow; no waste water, waste residue and waste gas are discharged; the method realizes the full utilization of valuable components in the waste lithium ion batteries, and remarkably reduces the environmental protection cost generated by wastewater treatment and the manufacturing cost of the whole process.
Description
Technical Field
The invention relates to the field of battery recovery, in particular to a method for recovering waste lithium ion batteries.
Background
The global climate is warmed, the depletion of non-renewable fossil energy forces people to develop and utilize renewable clean energy, and currently, the utilization rate of clean energy such as solar energy, wind energy and the like is gradually increased, so that the development of an energy storage device with excellent electrochemical performance is a current hot spot for solving the problem that solar energy and wind energy are discontinuous in time and space. The lithium ion battery has the advantages of high energy density, long cycle life, environmental friendliness and the like, and is widely applied to portable mobile electronic products such as mobile phones, cameras, notebooks and the like. In recent years, with the rise of the national new energy automobile industry, lithium ion batteries have been widely applied to hybrid electric vehicles and pure electric vehicles in batches, and gradually applied to large-scale energy storage power stations.
According to statistics, the new energy automobiles in China have 344 thousands of energy automobiles by 2019 and 6 months. On one hand, the application of the lithium ion battery greatly improves the utilization rate of clean energy, changes the life style of people, and greatly improves the living environment and the living quality of people; on the other hand, if the waste lithium ion battery cannot be effectively recycled, the problem of resource waste and environmental pollution caused by the retirement of the lithium ion battery is likely to prevent the sustainable development of society. Authorities expect that by the year 2020, only one power cell will have a cumulative scrap of 20 ten thousand tons, with a valuable metal value of up to 50 gigabytes. Studies have shown that recycling lithium ion batteries can save 51.3% of natural resources, including 45.3% ore consumption and 57.2% fossil energy consumption. Therefore, development of a waste lithium ion battery recycling technology with low cost, high valuable metal recycling rate and environmental protection is needed.
Chinese patent document CN106129511 a discloses a method for comprehensively recovering valuable metals from waste lithium ion battery materials: the method mixes waste lithium ion batteries with a carbon reducing agent, roasting the mixture at 500-750 ℃ and obtaining Li after carbonization water leaching 2 CO 3 The product, water leaching slag is further leached, extracted and separated to prepare sulfate solution containing nickel, cobalt and manganese. Li can be prepared by the method 2 CO 3 And low added value products such as nickel sulfate, cobalt sulfate, manganese sulfate and the like, but the problems of high energy consumption, tail gas treatment, emission, large amount of wastewater treatment generated by concentration and crystallization and the like in the high-temperature roasting process greatly limit the large-scale application of the method.
Further, chinese patent document CN106848470 a discloses a method for recovering and preparing ternary cathode material from waste nickel-cobalt-manganese ternary lithium ion battery: the method comprises the steps of carrying out secondary roasting on the anode of the waste nickel-cobalt-manganese lithium ion battery, wherein the primary roasting is carried out in air (300-500 ℃), and the secondary roasting is carried out in chlorine or sulfur dioxide atmosphere (300-600 ℃); leaching to obtain leaching solution containing Li, ni, co, mn, adding alkali metal hydroxide and carbonate to form NCM ternary material precursor, and finally roasting to obtain ternary positive electrode material. According to the method, li, ni, co, mn valuable metals in the waste lithium ion batteries are effectively recycled, and the ternary positive electrode material with high added value is prepared. However, the problems of strong corrosive acidic atmosphere and tail gas treatment in the roasting process, waste water treatment in the hydroxide precipitation process and the like are not solved, and the method is contrary to the concept of realizing green economy and sustainable development in China.
In order to solve the defects of the method for recycling valuable metals in the waste lithium ion batteries by the fire method, chinese patent documents CN 107117661A, CN 106785177A and CN 107326181A disclose methods for recycling valuable metals in the waste lithium ion batteries by a liquid phase method, and the methods can be used for effectively recycling valuable metals such as Ni, co, mn and the like in electrode materials, and simultaneously preparing a positive electrode material or a positive electrode material precursor with high added value. However, waste ammonia and waste water (sodium sulfate or sodium chloride) formed by acid (sulfuric acid, hydrochloric acid, etc.) and alkali (sodium hydroxide, ammonia water) introduced in the process are not treated and recycled effectively, so that the risk of safety and environmental protection is high.
Disclosure of Invention
The invention provides a method for recycling waste lithium ion batteries, and aims to provide a method which is economical, environment-friendly and capable of efficiently recycling valuable components in the waste lithium ion batteries.
In order to achieve the above object, an embodiment of the present invention provides a method for recycling waste lithium ion batteries, comprising the steps of:
step one, soaking discharge:
soaking the waste lithium ion battery in dilute brine for 7-14 days, and stirring once a day;
step two, disassembling:
drying the soaked and discharged waste lithium ion batteries at a low temperature, then disassembling and separating the shell to obtain a winding core of the waste lithium ion batteries;
step three, active substance separation:
placing the winding core obtained in the second step in a closed reaction container, introducing a proper amount of organic solvent, stirring and heating at a low temperature to strip active substances from a current collector, then physically separating to obtain copper foil, aluminum foil and a diaphragm, performing solid-liquid separation to obtain anode and cathode powder materials, and treating and recycling the separated organic solvent system;
step four, drying and crushing:
and (3) drying the anode and cathode powder material obtained in the step (III) at a low temperature, and crushing to obtain the raw material for leaching.
Leaching:
leaching the metal elements in the raw materials obtained in the step four into a liquid phase by adopting an acid leaching method, and obtaining carbon negative electrode powder and leaching liquid containing the metal elements after solid-liquid separation, wherein the carbon negative electrode powder is sintered to prepare a negative electrode material for a lithium ion battery;
step six, precipitation:
step five, purifying and removing impurities from the leaching solution, adjusting the proportion of transition metal elements and the concentration of transition metal ions in the leaching solution, and adding a precipitator and a complexing agent to obtain a precursor for the lithium ion battery anode material;
step seven, preliminary ammonia distillation:
carrying out preliminary ammonia distillation and concentration on the wastewater obtained in the step six, and conveying the obtained ammonia water to the step six for recycling;
step eight, electrolysis:
and (3) carrying out membrane electrolysis on the wastewater subjected to preliminary ammonia distillation and concentration to generate acid and alkali, conveying the obtained acid to a step five for recycling, and conveying the obtained alkali to a step six for recycling.
Preferably, the waste lithium ion batteryThe positive electrode material is LiCoO 2 、LiMn 2 O 4 、LiNi x Co y Mn z O 2 And LiNi a Co b Al c O 2 One or more of them, wherein 0<x<1，0<y<1，0<z<1, and x+y+z=1; 0.5<a<1，0<b<0.5,0<c<0.1, and a+b+c=1.
Preferably, in the first step, the diluted saline is 0.01-0.2 mol L -1 Sodium sulfate solution of (2).
Preferably, the drying temperature in the second step is 40-65 ℃.
Preferably, in the third step, the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, methylethyl carbonate, propylene carbonate, dimethyl ether, methylethyl ether, N-methylpyrrolidone and ethanol; the heating temperature is 30-50 ℃; the organic solvent system treatment method comprises the following steps: vacuum distillation or fractional distillation, and the recyclable organic solvent and binder are obtained after treatment.
Preferably, the heating temperature in the fourth step is 50 to 80 ℃.
Preferably, in the fifth step, the leaching agent is one or two of hydrochloric acid, sulfuric acid and hydrogen peroxide.
Preferably, in the step six, the precipitation process is performed in a closed reaction kettle, wherein the pH value is 10.5-12.0; the reaction temperature is 40-85 ℃, the reaction kettle is sealed, and the inside is filled with dry inert gas.
Preferably, in the sixth step, the precipitating agent is one or two of sodium carbonate or sodium hydroxide; the complexing agent is one or two of ammonium bicarbonate and ammonia water, and the concentration of the complexing agent is 0.1-1 mol/L.
Preferably, in the sixth step, the concentration of the transition metal ion is 0.1 to 5mol/L.
The scheme of the invention has the following beneficial effects:
(1) The harmful electrolyte, binder and other organic components in the waste batteries are recycled, and the organic solvent for leaching can be recycled;
(2) Preparing a positive electrode material precursor with high added value from transition metal in the waste lithium ion battery, wherein lithium is recycled by using lithium carbonate or lithium hydroxide;
(3) Realizing the closed cycle of the leaching agent, the complexing agent and the precipitant in the process flow;
(4) No waste water, waste residue and waste gas are discharged;
(5) The method realizes the full utilization of valuable components in the waste lithium ion batteries, and remarkably reduces the environmental protection cost generated by wastewater treatment and the manufacturing cost of the whole process.
Drawings
FIG. 1 is a process diagram of one embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, an embodiment of the present invention provides a method for recycling waste lithium ion batteries, including the following steps:
step one, soaking discharge:
to be recovered LiNi 0.5 Co 0.2 Mn 0.3 O 2 the/C waste lithium ion battery is placed in Na with 0.1mol/L 2 SO 4 Soaking in dilute saline for 12 days, and stirring once a day;
step two, disassembling:
drying the waste lithium ion battery after soaking and discharging at 50 ℃, then disassembling and separating the shell to obtain a winding core of the waste lithium ion battery;
step three, active substance separation:
placing the coiled core in a closed reaction container, introducing a proper amount of DMC solution, stirring and heating at a low temperature of 40 ℃ to strip active substances from a current collector; the copper foil, the aluminum foil and the diaphragm are obtained through physical separation, the anode and cathode powder materials are obtained after solid-liquid separation, and the organic solvent system obtained through solid-liquid separation is recycled after treatment;
step four, drying and crushing:
and step three, drying the anode and cathode powder material at a low temperature of 60 ℃ and then further crushing to obtain a raw material for leaching.
Leaching:
leaching Li, ni, co, mn and other metal elements in the raw materials into a liquid phase by adopting a sulfuric acid leaching method, and then carrying out solid-liquid separation to obtain carbon negative electrode powder and a leaching liquid containing Li, ni, co, mn and other metal elements, wherein the carbon negative electrode powder can be prepared into a high-value negative electrode material for a lithium ion battery through subsequent sintering;
step six, precipitation:
purifying the leaching solution, removing impurities, and passing through NiSO 4 、CoSO 4 And MnSO 4 Adjusting the proportion of transition metal elements in the leaching solution to Ni:Co:Mn=5:3:2, wherein the concentration of transition metal ions is 2mol/L, adding sodium hydroxide and ammonia water, wherein the concentration of ammonia water is 0.5mol/L, controlling the pH value to be 11.5, reacting at 60 ℃, and preparing Ni in a closed reaction kettle filled with dry nitrogen gas 0.5 Co 0.2 Mn 0.3 (OH) 2 A precursor;
step seven, preliminary ammonia distillation:
concentrating the wastewater in the step six through preliminary ammonia distillation, and conveying the ammonia water to the step six for recycling
Step eight, electrolysis:
the sodium sulfate wastewater after preliminary ammonia distillation and concentration is electrolyzed by a diaphragm electrolysis method, wherein a cation membrane (H + Membrane) and anionic membrane (OH - A membrane) separates the cathode chamber from the liquid inlet chamber and the anode chamber from the liquid inlet chamber, respectively. Respectively generating sulfuric acid and sodium hydroxide after electrolysis, and respectively returning the obtained sulfuric acid and sodium hydroxide to the fifth step and the sixth step for recycling; the byproduct high-purity hydrogen and oxygen can be sold; the ammonia water in the wastewater is further concentrated and returned to the step six, and the sodium sulfate dilute brine which is not fully electrolyzed is returned to the step one.
The method can prepare the transition metal in the waste lithium ion battery into a positive electrode material precursor with high added value, and lithium is recycled by lithium carbonate or lithium hydroxide; meanwhile, the harmful electrolyte, binder and other organic components in the waste batteries are recycled, and the organic solvent for leaching can also be recycled; realizing the closed cycle of the leaching agent, the complexing agent and the precipitant in the process flow; no waste water, waste residue and waste gas are discharged, and the requirements of current industrial economy and environmental protection are met; the method realizes the full utilization of valuable components in the waste lithium ion batteries, and remarkably reduces the environmental protection cost generated by wastewater treatment and the manufacturing cost of the whole process.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The method for recycling the waste lithium ion battery is characterized by comprising the following steps of:
step one, soaking discharge:
soaking the waste lithium ion battery in dilute brine for 7-14 days, and stirring once a day; the positive electrode material of the waste lithium ion battery is LiCoO 2 、LiMn 2 O 4 、LiNi x Co y Mn z O 2 And LiNi a Co b Al c O 2 One or more of them, wherein 0<x<1，0<y<1，0<z<1, and x+y+z=1; 0.5<a<1，0<b<0.5,0<c<0.1, and a+b+c=1; the diluted salt water is 0.01 to 0.2mol L -1 Sodium sulfate solution of (2);
step two, disassembling:
drying the soaked and discharged waste lithium ion batteries at a low temperature, then disassembling and separating the shell to obtain a winding core of the waste lithium ion batteries;
step three, active substance separation:
placing the winding core obtained in the second step in a closed reaction container, introducing a proper amount of organic solvent, stirring and heating at a low temperature to strip active substances from a current collector, then physically separating to obtain copper foil, aluminum foil and a diaphragm, performing solid-liquid separation to obtain anode and cathode powder materials, and treating and recycling the separated organic solvent system;
step four, drying and crushing:
drying the anode and cathode powder material obtained in the step three at a low temperature, and crushing to obtain a raw material for leaching;
leaching:
leaching the metal elements in the raw materials obtained in the step four into a liquid phase by adopting an acid leaching method, and obtaining carbon negative electrode powder and leaching liquid containing the metal elements after solid-liquid separation, wherein the carbon negative electrode powder is sintered to prepare a negative electrode material for a lithium ion battery;
step six, precipitation:
step five, purifying and removing impurities from the leaching solution, adjusting the proportion of transition metal elements and the concentration of transition metal ions in the leaching solution, and adding a precipitator and a complexing agent to obtain a precursor for the lithium ion battery anode material; the precipitant is one or two of sodium carbonate or sodium hydroxide; the complexing agent is one or two of ammonium bicarbonate and ammonia water, and the concentration of the complexing agent is 0.1-1 mol/L;
step seven, preliminary ammonia distillation:
carrying out preliminary ammonia distillation and concentration on the wastewater obtained in the step six, and conveying the obtained ammonia water to the step six for recycling;
step eight, electrolysis:
and (3) carrying out membrane electrolysis on the wastewater subjected to preliminary ammonia distillation and concentration to generate acid and alkali, conveying the obtained acid to a step five for recycling, and conveying the obtained alkali to a step six for recycling.
2. The method for recycling waste lithium ion batteries according to claim 1, wherein the drying temperature in the second step is 40-65 ℃.
3. The method for recycling waste lithium ion batteries according to claim 2, wherein in the third step, the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, methylethyl carbonate, propylene carbonate, dimethyl ether, methylethyl ether, N-methylpyrrolidone and ethanol; the heating temperature is 30-50 ℃; the organic solvent system treatment method comprises the following steps: vacuum distillation or fractional distillation, and the recyclable organic solvent and binder are obtained after treatment.
4. The method for recycling waste lithium ion batteries according to claim 3, wherein the heating temperature in the fourth step is 50-80 ℃.
5. The method for recycling waste lithium ion batteries according to claim 4, wherein in the fifth step, the leaching agent is one or two of hydrochloric acid, sulfuric acid and hydrogen peroxide.
6. The method for recycling waste lithium ion batteries according to claim 5, wherein in the step six, the precipitation process is performed in a closed reaction kettle, wherein the pH value is 10.5-12.0; the reaction temperature is 40-85 ℃, the reaction kettle is sealed, and the inside is filled with dry inert gas.
7. The method for recycling waste lithium ion batteries according to claim 1, wherein in the sixth step, the concentration of the transition metal ions is 0.1-5 mol/L.
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| KR20230044147A (en) * | 2021-04-13 | 2023-04-03 | 워세스터 폴리테크닉 인스티튜트 | Lithium recovery method |
| CN113981226B (en) * | 2021-09-29 | 2023-09-05 | 贵州中伟资源循环产业发展有限公司 | Method for preprocessing ternary positive plate to be recycled |
| CN114649598B (en) * | 2022-02-17 | 2024-09-06 | 广东邦普循环科技有限公司 | Method for desorbing recovered active material of waste battery |
| CN114665182B (en) * | 2022-04-25 | 2024-04-30 | 中国科学院青海盐湖研究所 | Method for separating and recycling current collector and negative electrode material in negative electrode of waste lithium ion battery |
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| WO2024173935A1 (en) * | 2023-02-17 | 2024-08-22 | The Trustees Of Indiana University | Methods of recovering electrode active materials from lithium-ion batteries and electrodes thereof |
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