CN112575203A - Method for recycling lithium in waste power lithium battery - Google Patents
Method for recycling lithium in waste power lithium battery Download PDFInfo
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- 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
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- 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
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention discloses a method for recovering lithium in waste power lithium batteries, which comprises the following steps: pretreatment: disassembling, crushing and sorting the waste power lithium battery under the protection of inert gas and in a closed state to obtain waste battery powder; high-temperature calcination: adding an additive into the waste battery powder for high-temperature calcination; mechanical activation and water immersion: adding an activating agent into the waste battery powder after high-temperature calcination, performing mechanical activation and water leaching, and performing solid-liquid separation to obtain a lithium-containing leachate; evaporation and crystallization: evaporating and crystallizing the obtained lithium-containing leaching solution to obtain a lithium hydroxide product. By adopting the method, the yield of the metal lithium in the whole treatment process reaches over 90 percent.
Description
Technical Field
The invention relates to the technical field of waste battery recovery, in particular to a method for recovering lithium in waste power lithium batteries.
Background
With the rapid development of new energy automobiles, large-scale retired power batteries will be brought in the future. The expected scrappage of lithium-ion power batteries will be 25Gwh, about 20 million tons, by 2020. The scrappage in 2023 years will reach 101Gwh, about 80 ten thousand tons. The overall battery recycling market size is predicted to reach 111 million yuan in 2020, wherein the echelon utilization is 69 million yuan, the recycling is 42 million yuan, and the overall market size reaches 150 million yuan by 2023. After a large amount of retired power storage batteries are not properly disposed and the value is maximized, the public safety is threatened, environmental pollution which is difficult to reverse is caused, and precious valuable metal resources are wasted.
At present, the recovery of lithium ion batteries in industry mainly focuses on the recovery and reuse of cobalt, nickel and other valuable metals, the extraction of lithium is not yet regarded as important, and the metal lithium is usually recovered and treated as waste residue or in the form of crude lithium carbonate at the end of a process. The lithium yield only reaches about 75 percent, and the problems of long wet recovery process, low lithium metal yield and the like exist.
Chinese patent CN107699692A discloses a method for recovering and regenerating a positive electrode material of a waste lithium ion battery, which comprises the following steps: discharging and disassembling the waste lithium ion battery, ventilating and drying a positive plate in a fume hood, cutting, soaking in a sodium hydroxide solution for 4-8 hours, filtering and washing, drying the obtained filter residue, calcining at 500-700 ℃ for 2-5 hours, and grinding to obtain a waste lithium ion battery positive material; mixing the waste lithium ion battery anode material with 0.2-4 mol/L of organic acid, stirring for 10-150 min at 25-90 ℃ when the organic acid is oxalic acid to obtain a solution containing Li + and a precipitate, and separating the solution containing Li + and the precipitate to obtain a lithium-containing solution. According to the method, the steps of grinding and organic acid leaching are adopted step by step for the calcined anode material, the treatment process is long, so that the lithium yield is influenced, and the method of organic acid leaching is high in cost and difficult to realize large-scale industrial application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for recovering lithium in waste power lithium batteries, which has high recovery rate and low cost.
The invention is realized by the following technical scheme.
A method for recycling lithium in waste power lithium batteries is characterized by comprising the following steps:
(1) pretreatment: disassembling, crushing and sorting the waste power lithium battery under the protection of inert gas and in a closed state to obtain waste battery powder;
(2) high-temperature calcination: adding an additive into the waste battery powder for high-temperature calcination;
(3) mechanical activation and water immersion: adding an activating agent into the waste battery powder after high-temperature calcination, performing mechanical activation and water leaching, and performing solid-liquid separation to obtain a lithium-containing leachate;
(4) evaporation and crystallization: evaporating and crystallizing the obtained lithium-containing leaching solution to obtain a lithium hydroxide product.
Further, in the step (1), the waste power lithium battery comprises one or more of a nickel-cobalt-manganese ternary lithium battery, a nickel-cobalt-aluminum lithium battery, a cobalt acid lithium battery, a manganese acid lithium battery and a iron phosphate lithium battery; the inert gas is any one of nitrogen, argon and carbon dioxide.
Furthermore, the particle size of the waste battery powder in the step (1) is 5-30 μm.
Further, in the step (2), the high-temperature calcination temperature is 200-600 ℃, and the calcination time is 30-120 min; the mass ratio of the waste battery powder to the additive is 1:0.5-2, and the additive is carbon powder or graphite.
Further, in the step (3), the mass ratio of the battery powder subjected to high-temperature calcination to the activating agent is 1:1-2, and the activating time is 30-120 min.
Further, in the step (3), the activating agent is zirconia, and the particle size is 20-80 mm.
Further, in the step (3), adding an activating agent into the battery powder after high-temperature calcination, slurrying the battery powder with deionized water, controlling the liquid-solid ratio of the deionized water to the battery powder after high-temperature calcination to be 1-3:1, controlling the mechanical activation and water immersion rotation speed to be 200-fold at 400r/min, and filtering the battery powder after mechanical activation and water immersion by using a Buchner funnel to obtain a lithium-containing leachate and filter residues containing the activating agent and nickel, cobalt and manganese.
Further, in the step (3), the filter residue obtained by filtering is screened and separated, the particle size of the screen is 8-40 mm, the separated activating agent is recycled in the steps of mechanical activation and water immersion in the step (3), and the nickel, cobalt and manganese in the filter residue are recycled in the wet method.
Further, in the step (3), the mechanical activation and the water immersion are carried out on a planetary type activation machine.
Further, in the step (4), the obtained lithium-containing leachate is subjected to evaporation crystallization on a rotary evaporator, the evaporation temperature is 73-86 ℃, the pressure is-0.075 MPa, and the lithium hydroxide product is obtained by centrifugal separation after the evaporation crystallization.
The invention has the beneficial technical effects that:
1. the method adopts a one-step method of mechanical activation and water leaching to further activate the calcined battery powder, improve the leaching rate of lithium, realize the high-efficiency separation of metal lithium and nickel-cobalt-manganese metal in the waste battery powder, transfer the metal lithium to the solution, and completely remove the metals such as nickel, cobalt, manganese and the like. The zirconium oxide activator is recycled for the steps of mechanical activation and water leaching, and the yield of the metal lithium in the whole treatment process is improved to more than 90 percent from about 75 percent at present in the industry. The method is easy to realize continuous, stable and large-scale industrial production, and accords with the green development concept of the waste power battery recovery industry.
2. The invention adopts a one-step completion method of mechanical activation and water immersion, combines mechanical, thermal and hydrometallurgy technologies, does not need heating in the mechanical activation process, converts mechanical energy into heat energy, ensures the system temperature and promotes the leaching of lithium.
3. The invention has wide application range, and the lithium in the lithium-containing solution is prepared into the lithium hydroxide product by a direct evaporation crystallization method, thereby avoiding the problems of low lithium yield and single product when the crude lithium carbonate is prepared by a precipitation method in the lithium recovery process. And simultaneously meets the market demand of the development of the current high-nickel anode material on lithium hydroxide. The invention fundamentally solves the problems of low yield of the metal lithium in the waste power lithium battery powder, long processing flow of the prepared lithium product and the like in the prior industry, really realizes the high-efficiency recovery and reutilization of the metal lithium, and has certain economic benefit and social benefit.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
(1) The method comprises the following steps of (1) preprocessing waste power lithium batteries (several mixed batteries of nickel-cobalt-manganese ternary lithium batteries, nickel-cobalt-aluminum lithium batteries and cobalt acid lithium batteries): 20kg of waste power lithium batteries are disassembled under the protection of inert gas (nitrogen) and in a closed state, and first-stage shredding, second-stage crushing, multi-stage sorting and screening are carried out to obtain waste battery powder, wherein the particle size of the battery powder is 8 microns.
(2) And (3) calcining the battery powder at high temperature: and adding 50g of carbon powder into 50g of waste power battery powder obtained by sorting, mixing, and putting into a box-type resistance furnace for high-temperature calcination. Calcination temperature 260 ℃, heat preservation time: and (4) 120min, and naturally cooling after calcining for later use.
(3) Mechanical activation and water immersion of battery powder: adding 100g of zirconia activator into 50g of calcined battery powder, wherein the grain size of the zirconia activator is 50mm, adding 75g of deionized water after preparation, sealing a planetary activating machine, adjusting the water immersion rotation speed to 250r/rmin, carrying out mechanical activation and water immersion for 90min, filtering the mixture by using a Buchner funnel after the mechanical activation and water immersion are finished to obtain a lithium-containing solution, a zirconia activator and nickel-cobalt-manganese slag, screening the slag by using a screen with the grain size of 30mm, and recycling the oversize product in the steps of mechanical activation and water immersion. The undersize is the slag containing nickel, cobalt and manganese, and directly enters the wet recovery process.
(4) And (3) evaporating and crystallizing: and pouring the obtained 500mL of lithium-containing leaching solution into a rotary evaporator, evaporating and crystallizing under a vacuum state at the evaporation temperature of 78 ℃ and the evaporation pressure of-0.075 MPa, and performing centrifugal separation after evaporation to obtain a lithium hydroxide product. The recovery rate of lithium reaches 91.2%.
Example 2
(1) The method comprises the following steps of (1) preprocessing a waste power lithium battery (nickel-cobalt-manganese ternary lithium battery): 50kg of waste power lithium batteries are disassembled under the protection of inert gas (argon) and in a closed state, and first-stage shredding, second-stage crushing, multi-stage sorting and screening are carried out to obtain waste battery powder, wherein the particle size of the battery powder is 18 microns.
(2) And (3) calcining the battery powder at high temperature: and adding 150g of graphite into 100g of the sorted waste power lithium ion battery powder, mixing, and putting into a box-type resistance furnace for high-temperature calcination. Calcining at 420 deg.C for 60min, and naturally cooling.
(3) Mechanical activation and water immersion of battery powder: adding 100g of zirconia activator into 100g of calcined battery powder, wherein the grain size of the zirconia activator is 20mm, adding 175g of deionized water after preparation, sealing an activator, carrying out water immersion at the rotation speed of 300r/min for 120min, carrying out mechanical activation and water immersion, filtering the mixture by using a Buchner funnel after the mechanical activation and the water immersion are finished, obtaining a lithium-containing solution, zirconium oxide-containing activator and nickel-cobalt-manganese slag, screening the slag by using a screen with the grain size of 10mm, and recycling the zirconium oxide activator in the steps of mechanical activation and water immersion. The undersize is the slag containing nickel, cobalt and manganese, and directly enters the wet recovery process.
(4) And (3) evaporating and crystallizing: and pouring 350mL of the obtained lithium-containing leaching solution into a rotary evaporator, evaporating and crystallizing under a vacuum state at 73 ℃ and-0.075 MPa, and performing centrifugal separation after evaporation to obtain a lithium hydroxide product. The recovery rate of lithium reaches 90.17%.
Example 3
(1) The method comprises the following steps of (1) preprocessing waste power lithium batteries (nickel-cobalt-manganese ternary lithium batteries, lithium manganate batteries and several mixed batteries of lithium iron phosphate batteries): 100kg of waste power lithium batteries are disassembled under the protection of inert gas carbon dioxide and in a closed state, and subjected to primary shredding, secondary crushing, multi-stage sorting and screening to obtain waste battery powder, wherein the particle size of the battery powder is 28 microns.
(2) And (3) calcining the battery powder at high temperature: and adding 150g of carbon powder into 75g of the sorted waste power lithium ion battery powder, mixing, and putting into a box-type resistance furnace for high-temperature calcination. Calcination temperature 580 ℃, heat preservation time: and (5) cooling naturally after calcining for 30min for later use.
(3) Mechanical activation and water immersion of battery powder: adding 75g of zirconium oxide activator into 50g of calcined battery powder, wherein the particle size of the zirconium oxide activator is 80mm, adding 150g of deionized water after preparation, sealing an activating machine, adjusting the rotating speed to 390r/min, and carrying out activation and water immersion for 30min, filtering the battery powder by using a Buchner funnel after mechanical activation and water immersion are finished to obtain a lithium-containing solution, zirconium oxide-containing activator and nickel-cobalt-manganese slag, screening the battery powder by using a screen with the particle size of 40mm, wherein oversize products are the zirconium oxide activator, and are recycled for the steps of mechanical activation and water immersion. The undersize is the slag containing nickel, cobalt and manganese, and directly enters the wet recovery process.
(4) And (3) evaporating and crystallizing: and (3) pouring 620mL of the obtained lithium-containing leaching solution into a rotary evaporator, evaporating and crystallizing under a vacuum state at the evaporation temperature of 84 ℃ and the evaporation pressure of-0.075 MPa, and performing centrifugal separation after evaporation to obtain a lithium hydroxide product. The recovery rate of lithium reaches 91.7%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (10)
1. A method for recycling lithium in waste power lithium batteries is characterized by comprising the following steps:
(1) pretreatment: disassembling, crushing and sorting the waste power lithium battery under the protection of inert gas and in a closed state to obtain waste battery powder;
(2) high-temperature calcination: adding an additive into the waste battery powder for high-temperature calcination;
(3) mechanical activation and water immersion: adding an activating agent into the waste battery powder after high-temperature calcination, performing mechanical activation and water leaching, and performing solid-liquid separation to obtain a lithium-containing leachate;
(4) evaporation and crystallization: evaporating and crystallizing the obtained lithium-containing leaching solution to obtain a lithium hydroxide product.
2. The method as claimed in claim 1, wherein in the step (1), the waste power lithium battery comprises one or more of a nickel-cobalt-manganese ternary lithium battery, a nickel-cobalt-aluminum lithium battery, a lithium cobaltate battery, a lithium manganate battery and a lithium iron phosphate battery; the inert gas is any one of nitrogen, argon and carbon dioxide.
3. The method according to any one of claims 1 or 2, wherein the particle size of the waste battery powder in the step (1) is 5 μm to 30 μm.
4. The method according to any one of claims 1 or 2, wherein in the step (2), the high-temperature calcination temperature is 200 ℃ to 600 ℃, and the calcination time is 30min to 120 min; the mass ratio of the waste battery powder to the additive is 1:0.5-2, and the additive is carbon powder or graphite.
5. The method according to any one of claims 1 or 2, wherein in the step (3), the mass ratio of the battery powder subjected to high-temperature calcination to the activator is 1:1-2, and the activation time is 30-120 min.
6. The method according to any one of claims 1 or 2, wherein in step (3), the activator is zirconia having a particle size of 20 to 80 mm.
7. The method according to any one of claims 1 or 2, wherein in the step (3), the battery powder after high-temperature calcination is added with an activating agent and then slurried with deionized water, the liquid-solid ratio of the deionized water to the battery powder after high-temperature calcination is 1-3:1, the mechanical activation and water immersion rotation speed is controlled to be 200-.
8. The method according to any one of claims 7, characterized in that in the step (3), the filter residue obtained by filtering is screened and separated, the particle size of a screen is 8mm-40mm, the separated activating agent is recycled in the steps of mechanical activation and water immersion in the step (3), and nickel, cobalt and manganese in the filter residue are recycled in the wet recovery process.
9. The method according to any one of claims 1 or 2, wherein in the step (3), the mechanical activation and the water immersion are carried out on a planetary type activation machine.
10. The method according to any one of claims 1 or 2, wherein in the step (4), the obtained lithium-containing leachate is subjected to evaporative crystallization on a rotary evaporator at the evaporation temperature of 73-86 ℃ and the pressure of-0.075 MPa, and the lithium hydroxide product is obtained by centrifugal separation after the evaporative crystallization.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113120930A (en) * | 2021-04-21 | 2021-07-16 | 中国科学院过程工程研究所 | Method for preparing lithium hydroxide by pyrolyzing waste lithium ion batteries |
| CN114899522A (en) * | 2022-07-11 | 2022-08-12 | 河北顺境环保科技有限公司 | Treatment method of waste ternary soft package lithium battery |
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| CN111170343A (en) * | 2019-12-23 | 2020-05-19 | 北京矿冶科技集团有限公司 | Method for recovering and producing lithium hydroxide from waste lithium ion battery |
| CN111313120A (en) * | 2020-02-20 | 2020-06-19 | 扬州大学 | Method for recovering cobalt and lithium metals in waste lithium ion battery |
| CN111333048A (en) * | 2020-03-10 | 2020-06-26 | 桑顿新能源科技(长沙)有限公司 | Method for preparing lithium manganese iron phosphate by using waste lithium iron phosphate and lithium manganate materials |
| CN111534697A (en) * | 2020-06-09 | 2020-08-14 | 中国恩菲工程技术有限公司 | Selection-smelting combined comprehensive recovery method and device for waste lithium ion batteries |
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| CN113120930A (en) * | 2021-04-21 | 2021-07-16 | 中国科学院过程工程研究所 | Method for preparing lithium hydroxide by pyrolyzing waste lithium ion batteries |
| CN114899522A (en) * | 2022-07-11 | 2022-08-12 | 河北顺境环保科技有限公司 | Treatment method of waste ternary soft package lithium battery |
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