CN111477985A - Method for recycling waste lithium ion batteries - Google Patents
Method for recycling waste lithium ion batteries Download PDFInfo
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- CN111477985A CN111477985A CN202010294915.3A CN202010294915A CN111477985A CN 111477985 A CN111477985 A CN 111477985A CN 202010294915 A CN202010294915 A CN 202010294915A CN 111477985 A CN111477985 A CN 111477985A
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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
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- 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 and discharging: step two, disassembling: step three, active substance separation: step four, drying and crushing: step five, leaching: step six, precipitation: step seven, primary ammonia distillation: and step eight, electrolysis. The method of the invention can not only prepare the transition metal in the waste lithium ion battery into the precursor of the anode material with high added value, but also recycle the lithium by lithium carbonate or lithium hydroxide; meanwhile, harmful electrolyte, binder and other organic components in the waste battery are recycled, and the organic solvent for extraction can be recycled; realizing closed circulation of a leaching agent, a complexing agent and a precipitator in the process flow; no waste water, waste residue and waste gas are discharged; the full utilization of valuable components in the waste lithium ion battery is realized, the environmental protection cost generated by wastewater treatment is obviously reduced, and the manufacturing cost of the whole process is obviously reduced.
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 warming and the exhaustion of non-renewable fossil energy compel people to develop and utilize renewable clean energy, at present, the utilization rate of clean energy such as solar energy, wind energy and the like gradually rises, and in order to solve the problem that solar energy and wind energy are discontinuous in time and space, the development of energy storage devices with excellent electrochemical performance is the current hotspot. 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 applied to hybrid electric vehicles and pure electric vehicles in large scale, and are gradually applied to large-scale energy storage power stations.
According to statistics, the new energy automobile keeping amount in China reaches 344 thousands of automobiles as the year 6 of 2019. 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 life quality of people; on the other hand, if the waste lithium ion battery cannot be effectively recycled, the problems of resource waste and environmental pollution caused by the decommissioning of the lithium ion battery will inevitably hinder the sustainable development of the society. The authorities expect that the accumulated rejection of only one power battery reaches 20 million tons by 2020 years, and the value of valuable metal in the power battery reaches 50 million yuan. Research shows that the recycling of lithium ion batteries can save 51.3% of natural resources, including 45.3% reduction of ore consumption and 57.2% reduction of fossil energy consumption. Therefore, the development of a waste lithium ion battery recovery technology with low cost, high valuable metal recovery rate and environmental protection is urgently needed.
Chinese patent document CN 106129511A discloses a method for comprehensively recovering valuable metals from waste lithium ion battery materials: the method is to use the waste lithium ion batteryMixing with a carbon reducing agent, roasting at 500-750 ℃, and soaking in carbonized water to obtain L i2CO3The product, the water leaching slag is further leached, extracted and separated to prepare sulfate solution containing nickel, cobalt and manganese, L i can be prepared by the patent method2CO3And low value-added products such as nickel sulfate, cobalt sulfate, manganese sulfate and the like, but the large-scale application of the method is greatly limited by the problems of high energy consumption, tail gas treatment and discharge, treatment of a large amount of wastewater generated by concentration and crystallization and the like in the high-temperature roasting process.
Further, Chinese patent document CN 1068470A discloses a method for recovering and preparing a ternary cathode material from a waste nickel-cobalt-manganese ternary lithium ion battery, which comprises the steps of carrying out two-stage roasting on the anode of the waste nickel-cobalt-manganese ternary lithium ion battery, wherein the first-stage roasting is carried out in the air (300-500 ℃), and the second-stage roasting is carried out in the chlorine or sulfur dioxide atmosphere (300-600 ℃), leaching to obtain a leaching solution containing L i, Ni, Co and Mn, adding an alkali metal hydroxide and a carbonate to form an NCM ternary material precursor, and finally roasting to obtain the ternary cathode material.
In order to overcome the disadvantages of the method for recovering valuable metals from waste lithium ion batteries by a pyrogenic process, chinese patent documents CN 107117661A, CN 106785177 a and CN 107326181 a disclose methods for recovering valuable metals from waste lithium ion batteries by a liquid phase method, which can effectively recover valuable metals such as Ni, Co, Mn, etc. from electrode materials, and simultaneously prepare a high value-added positive electrode material or a positive electrode material precursor. However, waste ammonia and waste water (containing sodium sulfate or sodium chloride) formed by introduced acid (sulfuric acid, hydrochloric acid, etc.) and alkali (sodium hydroxide, ammonia water) in the process are not effectively treated and recycled, so that the process has great risks of safety and environmental protection.
Disclosure of Invention
The invention provides a method for recycling waste lithium ion batteries, and aims to provide an economic and environment-friendly method 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, including the following steps:
step one, soaking and discharging:
soaking the waste lithium ion battery in dilute saline water for 7-14 days, and stirring once a day;
step two, disassembling:
drying the waste lithium ion battery after soaking discharge at low temperature, then disassembling and separating the shell to obtain a roll core of the waste lithium ion battery;
step three, active substance separation:
placing the roll core obtained in the step two in a closed reaction container, introducing a proper amount of organic solvent, stirring and heating at low temperature to strip the active substances from the current collector, then carrying out physical separation to obtain copper foil, aluminum foil and a diaphragm, carrying out solid-liquid separation to obtain positive and negative electrode powder materials, and processing the separated organic solvent system for recycling;
step four, drying and crushing:
and (4) drying the anode and cathode powder materials obtained in the step three at a low temperature, and crushing to obtain a raw material for leaching.
Step five, leaching:
adding a leaching agent by adopting an acid leaching method, leaching the metal elements in the raw material obtained in the step four into a liquid phase, and performing solid-liquid separation to obtain carbon negative electrode powder and a leachate containing the metal elements, wherein the carbon negative electrode powder is sintered to prepare the negative electrode material for the lithium ion battery;
step six, precipitation:
purifying and removing impurities from the leachate obtained in the step five, adjusting the proportion of transition metal elements and the concentration of transition metal ions in the leachate, and adding a precipitator and a complexing agent to obtain a precursor for the lithium ion battery anode material;
step seven, primary ammonia distillation:
performing primary ammonia distillation concentration on the wastewater obtained in the sixth step, and conveying the obtained ammonia water to the sixth step for recycling;
step eight, electrolysis:
and (4) performing membrane electrolysis on the wastewater subjected to the primary ammonia distillation concentration to generate acid and alkali, conveying the obtained acid to the fifth step for recycling, and conveying the obtained alkali to the sixth step for recycling.
Preferably, the anode material of the waste lithium ion battery is L iCoO2、LiMn2O4、LiNixCoyMnzO2And L iNiaCobAlcO2Wherein, 0<x<1，0<y<1，0<z<1, and x + y + z is 1; 0.5<a<1，0<b<0.5,0<c<0.1, and a + b + c is 1.
Preferably, in the first step, the dilute brine is 0.01-0.2 mol L-1Sodium sulfate solution.
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, ethyl methyl carbonate, propylene carbonate, dimethyl ether, methyl ethyl ether, N-methyl pyrrolidone 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 organic solvent and the adhesive which can be recycled are obtained after treatment.
Preferably, the heating temperature in the fourth step is 50-80 ℃.
Preferably, in the fifth step, the leaching agent is one or two of hydrochloric acid, sulfuric acid and hydrogen peroxide.
Preferably, in the sixth step, the precipitation process is carried out 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 interior of the reaction kettle is filled with dry inert gas.
Preferably, in the sixth step, the precipitator is one or two of sodium carbonate and 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 ions is 0.1-5 mol/L.
The scheme of the invention has the following beneficial effects:
(1) harmful electrolyte, binder and other organic components in the waste battery are recycled, and the organic solvent for extraction can be recycled;
(2) transition metals in the waste lithium ion batteries are prepared into a high value-added positive electrode material precursor, and lithium is recycled by lithium carbonate or lithium hydroxide;
(3) the closed circulation of the leaching agent, the complexing agent and the precipitating agent in the process flow is realized;
(4) no waste water, waste residue and waste gas are discharged;
(5) the full utilization of valuable components in the waste lithium ion battery is realized, and the environmental protection cost generated by wastewater treatment and the manufacturing cost of the whole process are obviously reduced.
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 of the present invention more apparent, the following detailed description is 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 a used lithium ion battery, including the following steps:
step one, soaking and discharging:
l iNi recovered0.5Co0.2Mn0.3O2Putting the waste/C lithium ion battery in 0.1 mol/L Na2SO4Soaking in dilute saline for 12 days, and stirring once a day;
step two, disassembling:
drying the waste lithium ion battery subjected to soaking discharge at 50 ℃, then disassembling and separating the shell to obtain a roll core of the waste lithium ion battery;
step three, active substance separation:
placing the roll core in a closed reaction container, introducing a proper amount of DMC solution, and stirring and heating at low temperature, wherein the heating temperature is 40 ℃, so that the active substance is stripped from the current collector; carrying out physical separation to obtain copper foil, aluminum foil and a diaphragm, carrying out solid-liquid separation to obtain a positive electrode powder material and a negative electrode powder material, and treating an organic solvent system obtained by the solid-liquid separation for cyclic utilization;
step four, drying and crushing:
and drying the anode and cathode powder material obtained in the step three at a low temperature of 60 ℃, and then further crushing to obtain a raw material for leaching.
Step five, leaching:
leaching L i, Ni, Co, Mn and other metal elements in the raw materials into a liquid phase by adopting a sulfuric acid leaching method, then carrying out solid-liquid separation to obtain carbon negative electrode powder and leachate containing L i, Ni, Co, Mn and other metal elements, and preparing the carbon negative electrode powder into a high-value negative electrode material for the lithium ion battery through subsequent sintering;
step six, precipitation:
further purifying the leachate, removing impurities, and passing through NiSO4、CoSO4And MnSO4Adjusting the proportion of transition metal elements in the leachate until the ratio of Ni to Co to Mn is 5:3:2, the concentration of transition metal ions is 2 mol/L, adding sodium hydroxide and ammonia water, wherein the concentration of the ammonia water is 0.5 mol/L, controlling the pH value to be 11.5, reacting at the temperature of 60 ℃, and preparing Ni in a closed reaction kettle filled with dry nitrogen0.5Co0.2Mn0.3(OH)2A precursor;
step seven, primary ammonia distillation:
concentrating the wastewater in the sixth step by primary ammonia distillation, and conveying the ammonia water to the sixth step for recycling
Step eight, electrolysis:
by means of a partitionElectrolyzing the sodium sulfate wastewater after primary ammonia distillation concentration by using a membrane electrolysis method, wherein a cationic membrane (H) is adopted+Membrane) and anionic membrane (OH)-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; high-purity hydrogen and oxygen are by-produced and can be sold for external use; 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.
By the method, the transition metal in the waste lithium ion battery can be prepared into the precursor of the anode material with high added value, and lithium is recycled by lithium carbonate or lithium hydroxide; meanwhile, harmful electrolyte, binder and other organic components in the waste battery are recycled, and the organic solvent for extraction can also be recycled; realizing closed circulation of a leaching agent, a complexing agent and a precipitator in the process flow; no waste water, waste residue and waste gas are discharged, and the requirements of modern industrial economy and environmental protection are met; the full utilization of valuable components in the waste lithium ion battery is realized, the environmental protection cost generated by wastewater treatment is obviously reduced, and the manufacturing cost of the whole process is obviously reduced.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for recycling waste lithium ion batteries is characterized by comprising the following steps:
step one, soaking and discharging:
soaking the waste lithium ion battery in dilute saline water for 7-14 days, and stirring once a day;
step two, disassembling:
drying the waste lithium ion battery after soaking discharge at low temperature, then disassembling and separating the shell to obtain a roll core of the waste lithium ion battery;
step three, active substance separation:
placing the roll core obtained in the step two in a closed reaction container, introducing a proper amount of organic solvent, stirring and heating at low temperature to strip the active substances from the current collector, then carrying out physical separation to obtain copper foil, aluminum foil and a diaphragm, carrying out solid-liquid separation to obtain positive and negative electrode powder materials, and processing the separated organic solvent system for recycling;
step four, drying and crushing:
drying the positive and negative electrode powder materials obtained in the step three at a low temperature and then crushing to obtain a raw material for leaching;
step five, leaching:
adding a leaching agent by adopting an acid leaching method, leaching the metal elements in the raw material obtained in the step four into a liquid phase, and performing solid-liquid separation to obtain carbon negative electrode powder and a leachate containing the metal elements, wherein the carbon negative electrode powder is sintered to prepare the negative electrode material for the lithium ion battery;
step six, precipitation:
purifying and removing impurities from the leachate obtained in the step five, adjusting the proportion of transition metal elements and the concentration of transition metal ions in the leachate, and adding a precipitator and a complexing agent to obtain a precursor for the lithium ion battery anode material;
step seven, primary ammonia distillation:
performing primary ammonia distillation concentration on the wastewater obtained in the sixth step, and conveying the obtained ammonia water to the sixth step for recycling;
step eight, electrolysis:
and (4) performing membrane electrolysis on the wastewater subjected to the primary ammonia distillation concentration to generate acid and alkali, conveying the obtained acid to the fifth step for recycling, and conveying the obtained alkali to the sixth step for recycling.
2. The method for recycling waste lithium ion batteries according to claim 1, wherein the anode material of the waste lithium ion batteries is L iCoO2、LiMn2O4、LiNixCoyMnzO2And L iNiaCobAlcO2One ofOr a plurality of them, wherein, 0<x<1，0<y<1，0<z<1, and x + y + z is 1; 0.5<a<1，0<b<0.5,0<c<0.1, and a + b + c is 1.
3. The method for recycling waste lithium ion batteries according to claim 2, wherein in the step one, the dilute brine is 0.01-0.2 mol L-1Sodium sulfate solution.
4. The method for recycling waste lithium ion batteries according to claim 3, wherein the drying temperature in the second step is 40-65 ℃.
5. The method for recycling the waste lithium ion batteries according to claim 4, wherein in the third step, the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, propylene carbonate, dimethyl ether, methyl ethyl ether, N-methyl pyrrolidone 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 organic solvent and the adhesive which can be recycled are obtained after treatment.
6. The method for recycling waste lithium ion batteries according to claim 5, wherein the heating temperature in the fourth step is 50-80 ℃.
7. The method for recycling waste lithium ion batteries according to claim 6, wherein in the fifth step, the leaching agent is one or two of hydrochloric acid, sulfuric acid and hydrogen peroxide.
8. The method for recycling the waste lithium ion batteries according to claim 7, wherein in the sixth step, 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 interior of the reaction kettle is filled with dry inert gas.
9. The method for recycling the waste lithium ion batteries according to claim 8, wherein in the sixth step, the precipitator is one or two of sodium carbonate or sodium hydroxide, the complexing agent is one or two of ammonium bicarbonate or ammonia water, and the concentration of the complexing agent is 0.1-1 mol/L.
10. The method for recycling waste lithium ion batteries according to claim 9, wherein in the sixth step, the concentration of the transition metal ions is 0.1-5 mol/L.
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Cited By (6)
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| CN113981226A (en) * | 2021-09-29 | 2022-01-28 | 贵州中伟资源循环产业发展有限公司 | Method for pretreating ternary positive plate to be recycled |
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| CN114665182A (en) * | 2022-04-25 | 2022-06-24 | 中国科学院青海盐湖研究所 | Method for separating and recovering current collector and negative electrode material in waste lithium ion battery negative electrode |
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| CN116116867A (en) * | 2022-09-07 | 2023-05-16 | 北京科技大学 | Cooperative treatment system and method for waste dry batteries and kitchen waste |
| CN116904762A (en) * | 2023-09-14 | 2023-10-20 | 中南大学 | Method for stripping and recovering aluminum from waste lithium battery powder positive electrode material and current collector |
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| CN116116867B (en) * | 2022-09-07 | 2023-10-13 | 北京科技大学 | Cooperative treatment system and method for waste dry batteries and kitchen waste |
| CN116904762A (en) * | 2023-09-14 | 2023-10-20 | 中南大学 | Method for stripping and recovering aluminum from waste lithium battery powder positive electrode material and current collector |
| CN116904762B (en) * | 2023-09-14 | 2023-12-08 | 中南大学 | Method for stripping and recovering aluminum from waste lithium battery powder positive electrode material and current collector |
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