CN111088428A - Leaching system and leaching method for recovering valuable metals of waste lithium cobalt oxide batteries - Google Patents

Leaching system and leaching method for recovering valuable metals of waste lithium cobalt oxide batteries Download PDF

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Publication number
CN111088428A
CN111088428A CN201911167662.7A CN201911167662A CN111088428A CN 111088428 A CN111088428 A CN 111088428A CN 201911167662 A CN201911167662 A CN 201911167662A CN 111088428 A CN111088428 A CN 111088428A
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leaching
waste lithium
lithium cobaltate
valuable metals
recovering valuable
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张佳峰
李东民
李鹏飞
欧星
张宝
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Central South University
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0446—Leaching processes with an ammoniacal liquor or with a hydroxide of an alkali or alkaline-earth metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A leaching system and a leaching method for recovering valuable metals of waste lithium cobaltate batteries. The leaching system of the invention is a mixed aqueous solution comprising ammonia, sodium sulfite and ammonium chloride. The leaching method comprises the following steps: (1) discharging, crushing and separating the waste lithium cobaltate battery to obtain anode powder; (2) heating the leaching system, adding anode powder into the leaching system, carrying out leaching reaction under the stirring condition, and obtaining Li-containing material after the reaction is finished+、Co(NH3)n 2+The leachate of (2). The leaching system does not need acid liquor, does not generate harmful gas, is capable of leaching at normal pressure in one step, is green and environment-friendly, and does not have secondary pollution; book (I)The leaching method is safe and controllable, has low cost and industrial application prospect.

Description

Leaching system and leaching method for recovering valuable metals of waste lithium cobalt oxide batteries
Technical Field
The invention relates to the field of waste battery resource recovery, in particular to a leaching system and a leaching method for recovering valuable metals of waste lithium cobalt oxide batteries.
Background
The lithium ion battery has the excellent characteristics of high working voltage, high theoretical specific capacity, no memory effect, light weight and the like, and is widely applied to portable equipment and electric automobiles. Accordingly, the scrap amount of lithium ion batteries is also increasing greatly. According to prediction, the scrappage of the lithium ion battery in China reaches 50 ten thousand tons by 2020.
Lithium cobaltate is the first and most successful commercial product of lithium ion battery positive electrode material for portable electronic devices. Therefore, the number of used lithium cobalt oxide batteries is also the largest. The waste lithium cobalt oxide batteries contain valuable metals of lithium and cobalt, and belong to secondary resources with extremely high metal content compared with the traditional ore resources. If the waste lithium cobaltate battery is discarded at will, the cobalt and lithium contained in the waste lithium cobaltate battery can pollute water sources, atmosphere and soil, and the heavy metal cobalt has an accumulation effect and can seriously threaten human health after entering a food chain. Therefore, the waste lithium cobalt oxide batteries are recycled, and the sustainable development of human and ecological environment is facilitated from the economic and environmental protection perspectives.
Generally, the process flow for recycling the waste lithium cobalt oxide battery comprises a physical process and a chemical process. Physical processes include mechanical separation, thermal treatment, mechanochemical, and dissolution processes, and chemical processes include pyrometallurgical, hydrometallurgical, bioleaching, and the like. The pyrometallurgical energy consumption is high, the resource waste is serious, and harmful gas can be generated to cause atmospheric pollution; the biological leaching efficiency is low, the period is long, and the leaching effect is not good; the hydrometallurgy method is widely applied to separating and recovering valuable metals, and has the characteristics of high treatment efficiency, controllable operation, low energy consumption and the like.
The leaching process is an important step of hydrometallurgical recovery, and the traditional leaching method is to use an acid-reducing agent system for leaching, wherein the acid is divided into inorganic acid and organic acid, the inorganic acid comprises sulfuric acid, hydrochloric acid, nitric acid and the like, and the organic acid comprises citric acid, ascorbic acid, oxalic acid and the like. When the acid leaching is used, a large amount of acid waste gas, acid waste liquid and the like are generated in the leaching process, and secondary pollution to the environment is caused.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel leaching system and a leaching method for recovering valuable metals of waste lithium formate batteries, wherein the leaching system does not need acid liquor, does not generate harmful gases, is green and environment-friendly, does not cause secondary pollution, and the leaching method is safe and controllable, has low cost and has industrial application prospect.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a leaching system for recovering valuable metals of waste lithium cobaltate batteries is a mixed aqueous solution containing ammonia, sulfite and ammonium chloride.
Preferably, the ammonia concentration of the mixed solution is 1-5 mol/L. More preferably, the ammonia concentration is 3.5-4.5 mol/L. Within this range, the leaching rate can reach more than 70%.
Preferably, the concentration of the sodium sulfite is 0.2-3 mol/L. More preferably, the concentration of the sodium sulfite is 0.4 to 1.0mol/L, and still more preferably 0.5 mol/L. The sulfite is mainly used as a reducing agent to reduce trivalent cobalt into divalent cobalt, thereby being beneficial to leaching cobalt.
Preferably, the sulfite is sodium sulfite, potassium sulfite or ammonium sulfite.
Preferably, the concentration of the ammonium chloride is 1-5 mol/L, and more preferably, the concentration of the ammonium chloride is 1.2-2.0 mol/L; further preferably 1.5 mol/L.
A leaching method for recovering valuable metals of waste lithium cobaltate batteries comprises the following steps:
(1) discharging, crushing and separating the waste lithium cobaltate battery to obtain anode powder;
(2) subjecting the leaching system to additionHeating, adding anode powder, stirring, leaching to obtain Li-containing material+、Co(NH3)n 2+The leachate of (2).
Preferably, in the step (2), the temperature of the leaching reaction is 50-90 ℃, and more preferably 75-85 ℃; further preferably 80 ℃.
Preferably, in the step (2), the adding amount of the cathode material is 5-20 g/L, more preferably, the adding amount of the cathode material is 8-12 g/L, and further preferably 10 g/L.
Preferably, in the step (2), the leaching reaction time is 1-60 h, more preferably, the leaching reaction time is 40-55 h, and even more preferably 50 h.
Preferably, in the step (2), the stirring speed is more than or equal to 500 rpm.
The invention has the beneficial effects that:
(1) according to the invention, normal-pressure ammonia-sodium sulfite-ammonium chloride is adopted to leach lithium cobaltate in one step, so that the limitations of a large amount of waste gas generated by the traditional inorganic acid leaching, environmental pollution caused by acid liquor, high cost of organic acid and the like are overcome; in the leaching process, the pH value of the leaching solution is close to neutral, and the property is mild; less toxic and harmful waste gas is generated, and the method is environment-friendly; compared with the method of selecting hydrogen peroxide as a reducing agent, sodium sulfite is used as the reducing agent, so that the reaction is safe and controllable.
(2) Compared with the traditional pickle liquor, the leaching system disclosed by the invention adopts normal-pressure ammonia-sodium sulfite-ammonium chloride to leach lithium cobaltate in one step, so that the leaching system has no corrosion effect on instruments; no pressure reaction is needed, and the equipment is simple; the cost of the chemical reagent and the equipment is low, and the operation is safe.
Drawings
FIG. 1 is an XRD pattern of the anode material powder of a waste lithium cobaltate battery used in examples 1 to 4 of the present invention;
FIG. 2 is a graph showing the effect of leaching time on the leaching rate and the lithium and cobalt in the anode powder of the waste lithium cobaltate battery in example 1 of the present invention.
FIG. 3 is a graph showing the effect of leaching systems with different ammonia concentrations on the leaching rate of lithium and cobalt in the anode powder of the waste lithium cobalt oxide battery in example 2 of the present invention.
FIG. 4 is a graph showing the effect of leaching systems with different sodium sulfite concentrations on the leaching rate of lithium and cobalt in the anode powder of the waste lithium cobalt oxide battery in example 3 of the present invention.
FIG. 5 is a graph showing the effect of leaching systems with different ammonium chloride concentrations on the leaching rate of lithium and cobalt in the anode powder of the waste lithium cobalt oxide battery in example 4 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
Example 1
A leaching method for recovering valuable metals of waste lithium cobaltate batteries comprises the following steps:
(1) separating and crushing the waste lithium cobalt oxide battery, and separating out anode material powder, wherein the anode material powder contains Li7.39% and Co 60.23%, and mainly exists in the form of lithium cobalt oxide (see figure 1);
(2) preparing a leaching system for recovering valuable metals of the waste lithium cobaltate battery, namely a mixed aqueous solution of ammonia, sodium sulfite and ammonium chloride, wherein the ammonia concentration is 4mol/L, the sodium sulfite concentration is 0.5mol/L, and the ammonium chloride concentration is 1.5 mol/L;
(3) adding 300mL of the leaching system in the step (2) into a 500mL three-neck flask, installing a condensing device, heating to 80 ℃, adding 3g of the anode powder obtained in the step (1), carrying out leaching reaction under the magnetic stirring of 500rpm for 50h to obtain a solution containing Li+、Co(NH3)n 2+Leaching the liquid.
At different leaching reaction time points, Li in the leaching solution is added+And Co (NH)3)n 2+The measurement was performed, and a curve showing the change in the leaching rate of lithium and cobalt in the positive electrode powder was plotted in terms of the leaching rate, as shown in fig. 2.
Example 2
A leaching method for recovering valuable metals of waste lithium cobaltate batteries comprises the following steps:
(1) separating out anode material powder after the pretreatment of splitting, crushing and the like of the waste lithium cobaltate battery;
(2) preparing a leaching system for recovering valuable metals of the waste lithium cobaltate batteries with different ammonia concentrations, namely a mixed aqueous solution of ammonia, sodium sulfite and ammonium chloride, wherein the ammonia concentrations are respectively 0, 1, 2, 3, 4 and 5mol/L, the sodium sulfite concentration is 0.5mol/L, and the ammonium chloride concentration is 1.5 mol/L.
(3) Respectively adding 300mL of the leaching system with different ammonia concentrations in the step (2) into a 500mL three-neck flask, installing a condensing device, heating to 80 ℃, respectively adding 3g of the anode powder obtained in the step (1), carrying out leaching reaction under the magnetic stirring of 500rpm, and reacting for 50h to obtain the Li-containing anode powder+、Co(NH3)n 2+Leaching the liquid.
Measurement of Li in the leachate+、Co(NH3)n 2+The leaching rate was calculated, and a graph showing the influence of the ammonia concentration of the leaching system on the leaching rate was drawn, as shown in fig. 3.
Example 3
A leaching method for recovering valuable metals of waste lithium cobaltate batteries comprises the following steps:
(1) separating out anode material powder after the pretreatment of splitting, crushing and the like of the waste lithium cobaltate battery;
(2) preparing a leaching system for recovering valuable metals of the waste lithium cobaltate batteries with different sodium sulfite concentrations, namely a mixed aqueous solution of ammonia, sodium sulfite and ammonium chloride, wherein the ammonia concentration is 4mol/L, the sodium sulfite concentrations are respectively 0, 0.1, 0.2, 0.4, 0.5, 1.0, 2.0 and 3.0mol/L, and the ammonium chloride concentration is 1.5 mol/L.
(3) Adding 300mL of leaching systems with different sulfurous acid concentrations in the step (2) into 500mL three-neck flasks respectively, installing a condensing device, heating to 80 ℃, adding 3g of the anode powder obtained in the step (1) respectively, carrying out leaching reaction under the magnetic stirring of 500rpm for 50h to obtain a solution containing Li+、Co(NH3)n 2+Leaching the liquid.
Measurement of Li in leachate+And Co (NH)3)n 2+The concentration, converted to the leaching rate, was plotted as a graph showing the effect of the sodium sulfite concentration of the leaching system on the leaching rate, as shown in fig. 4.
Example 4
A leaching method for recovering valuable metals of waste lithium cobaltate batteries comprises the following steps:
(1) separating out anode material powder after the pretreatment of splitting, crushing and the like of the waste lithium cobaltate battery;
(2) preparing a leaching system for recovering valuable metals of the waste lithium cobaltate batteries with different ammonium chloride concentrations, namely a mixed aqueous solution of ammonia-sodium sulfite-ammonium chloride, wherein the ammonia concentration is 4mol/L, the sodium sulfite concentration is 0.5mol/L, and the ammonium chloride concentrations are respectively 0, 0.5, 1.0, 1.5, 2.0, 3.0, 4.0 and 5.0 mol/L.
(3) Adding 300mL of leaching systems with different ammonium chloride concentrations in the step (2) into 500mL three-neck flasks respectively, installing a condensing device, heating to 80 ℃, adding 3g of the anode powder obtained in the step (1) respectively, carrying out leaching reaction under the magnetic stirring of 500rpm for 50h, and obtaining Li-containing materials respectively+、Co(NH3)n 2+Leaching the liquid.
Measurement of Li in leachate+And Co (NH)3)n 2+The concentration was converted to the leaching rate, and a graph showing the effect of the ammonium chloride concentration in the leaching system on the leaching rate was drawn, as shown in fig. 5.

Claims (10)

1. A leaching system for recovering valuable metals of waste lithium cobaltate batteries is characterized by comprising a mixed aqueous solution of ammonia, sulfite and ammonium chloride.
2. The leaching system for recycling valuable metals from waste lithium cobaltate batteries according to claim 1, wherein the ammonia concentration in the mixed aqueous solution is 1-5 mol/L, preferably 3.5-4.5 mol/L.
3. The leaching system for recycling valuable metals of waste lithium cobaltate batteries according to claim 1 or 2, wherein the concentration of the sulfite is 0.2-3 mol/L, preferably 0.4-1.0 mol/L.
4. The leaching system for recovering valuable metals from waste lithium cobaltate batteries according to claim 1, 2 or 3, wherein the concentration of the ammonium chloride is 1-5 mol/L, preferably 1.2-2.0 mol/L.
5. A leaching method for recovering valuable metals of waste lithium cobaltate batteries is characterized by comprising the following steps:
(1) discharging, crushing and separating the waste lithium cobaltate battery to obtain anode powder;
(2) heating the leaching system of any one of claims 1 to 4, adding the positive electrode powder obtained in the step (1), and performing leaching reaction under stirring to obtain a Li-containing solution after the reaction is completed+、Co(NH3)n 2+The leachate of (2).
6. The leaching method for recovering valuable metals from waste lithium cobaltate batteries according to claim 5, wherein in the step (2), the temperature of the leaching reaction is 50-90 ℃; preferably 75 to 85 ℃.
7. The leaching method for recycling valuable metals of waste lithium cobaltate batteries according to claim 5 or 6, wherein in the step (2), the adding amount of the positive electrode material is 5-20 g/L.
8. The leaching method for recovering valuable metals of waste lithium cobaltate batteries according to any one of claims 5 to 7, wherein the adding amount of the positive electrode material is 8-12 g/L.
9. The leaching method for recovering valuable metals from waste lithium cobaltate batteries according to any one of claims 4 to 7, wherein in the step (2), the leaching reaction time is 1-60 hours, preferably 45-55 hours.
10. The leaching method for recovering valuable metals from waste lithium cobaltate batteries according to any one of claims 4 to 7, wherein in the step (2), the stirring speed is not less than 500 rpm.
CN201911167662.7A 2019-11-25 2019-11-25 Leaching system and leaching method for recovering valuable metals of waste lithium cobalt oxide batteries Pending CN111088428A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112374550A (en) * 2020-11-09 2021-02-19 贵州红星电子材料有限公司 Comprehensive recovery method for waste lithium iron phosphate and nickel cobalt lithium manganate lithium battery anode material
WO2022170399A1 (en) * 2021-02-12 2022-08-18 Renewable Metals Company Pty Ltd Recovery of metals
CN116845410A (en) * 2023-07-25 2023-10-03 湖南德景源科技有限公司 Method for recycling valuable metals from waste ternary lithium battery

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107230811A (en) * 2016-03-25 2017-10-03 中国科学院过程工程研究所 The Selectively leaching agent of metal component and recovery method in a kind of positive electrode

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107230811A (en) * 2016-03-25 2017-10-03 中国科学院过程工程研究所 The Selectively leaching agent of metal component and recovery method in a kind of positive electrode

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112374550A (en) * 2020-11-09 2021-02-19 贵州红星电子材料有限公司 Comprehensive recovery method for waste lithium iron phosphate and nickel cobalt lithium manganate lithium battery anode material
WO2022170399A1 (en) * 2021-02-12 2022-08-18 Renewable Metals Company Pty Ltd Recovery of metals
CN116845410A (en) * 2023-07-25 2023-10-03 湖南德景源科技有限公司 Method for recycling valuable metals from waste ternary lithium battery
CN116845410B (en) * 2023-07-25 2024-03-15 湖南德景源科技有限公司 Method for recycling valuable metals from waste ternary lithium battery

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