CN111961857A - Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries - Google Patents
Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries Download PDFInfo
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- CN111961857A CN111961857A CN202010799019.2A CN202010799019A CN111961857A CN 111961857 A CN111961857 A CN 111961857A CN 202010799019 A CN202010799019 A CN 202010799019A CN 111961857 A CN111961857 A CN 111961857A
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- leaching
- electrode powder
- sulfuric acid
- lithium ion
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps: pretreating a waste lithium ion battery to obtain electrode powder, uniformly mixing the electrode powder with water and concentrated sulfuric acid, curing at 50-200 ℃ for 1.0-24.0 h, adding a leaching agent into the cured material for leaching after curing, and filtering after leaching to obtain the valuable metal leaching solution with low fluorine content. The method organically combines the removal of fluorine in the electrode powder with the leaching of valuable metals, and a curing and defluorination step is added before the acid leaching of the electrode powder, namely, the electrode powder is firstly added with partial concentrated sulfuric acid for curing and defluorination, the electrode powder after defluorination is added with partial sulfuric acid for leaching, and the electrode powder are tightly connected; compared with the conventional acid leaching process, the method has the advantages of no increase of acid consumption, low process cost, strong operability, low fluorine content of the obtained valuable metal leaching solution and easy realization of industrial production.
Description
Technical Field
The invention belongs to the technical field of waste lithium ion battery resource recovery, and particularly relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries.
Background
Lithium ion batteries have the advantages of large capacity, high energy density, no memory, small self-discharge and the like, are rapidly developed since the advent, and are successively applied to portable consumer electronics markets such as mobile phones, notebook computers and mobile power supplies and the industry of new energy automobiles in large quantities. At present, China becomes the biggest lithium ion battery producing country in the world.
After the lithium ion battery is charged and discharged for a certain number of times, the active material is deactivated and scrapped due to structural change, and the service life of the lithium ion battery is generally 3-5 years. In recent years, with the rapid development of new energy automobile industry, the scrappage of power batteries is also getting larger and larger, and the scrappage of the power batteries for automobiles in China is expected to reach 32GWh (about 50 million tons) in 2020; by 2030, the scrappage of the power battery for the vehicle can reach 101GWh, about 116 ten thousand tons. The scrapped lithium ion battery contains various harmful substances, such as heavy metals, organic and inorganic toxic compounds and the like, and if the waste lithium ion battery is not treated in time, the environment is easily polluted; meanwhile, the lithium ion battery contains rare and precious metals such as cobalt, nickel, manganese, lithium and the like and fluorine-containing electrolyte, particularly metallic cobalt, which is an internationally recognized strategic substance, and valuable metals are timely recovered, so that the potential environmental problem can be solved, the regeneration of resources such as nickel, cobalt, manganese, lithium and the like can be realized, and the sustainable development of new energy industry is facilitated.
At present, the recovery and utilization of waste lithium ion batteries mainly aim at the recovery and utilization of valuable metals in positive active materials, and two processes of fire smelting and wet smelting in the recovery process are most typical, and the wet smelting process is mainly used. The wet process is that the lithium ion battery is first pre-treated through overdischarge, disassembly, crushing, sorting, roasting, etc. to obtain electrode powder, and then proper amount of inorganic acid or organic acid is used to dissolve the valuable metal, and finally the corresponding metal and metal compound are obtained through precipitation, extraction, ion exchange, etc. However, in the process of recycling and utilizing the lithium ion battery, the lithium hexafluorophosphate as the electrolyte is in contact with acid, alkali and water or can be decomposed and hydrolyzed under heating, so that fluorine-containing compounds are generated and remained in the electrode powder, the PVDF as the binder can also be decomposed in the pretreatment roasting process to generate fluorides and remain in the electrode powder, and the fluorine-containing compounds remained in the electrode powder can enter a leachate along with valuable metals in the acid leaching process, thereby having adverse effects on the subsequent separation process requiring low fluorine content.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries comprises the following steps: pretreating a waste lithium ion battery to obtain electrode powder (comprising anode powder and cathode powder), uniformly mixing the electrode powder with water and concentrated sulfuric acid, curing, controlling the temperature of the curing at 50-200 ℃ for 1.0-24.0 h, removing anhydrous hydrogen fluoride generated by reaction of concentrated sulfuric acid and fluoride in the curing process through volatilization, dissolving part of metals and oxides thereof to form sulfate, adding a leaching agent into the cured material after curing, leaching, and filtering to obtain valuable metal leachate with low fluorine content. The parameters of the curing treatment need to be controlled within the scope of the invention, if the parameters exceed the scope of the invention, the energy consumption is increased, the water can be volatilized too fast, and the concentrated sulfuric acid can not fully react with the electrode powder; if the amount is less than the range of the present invention, the number of active molecules in the aging reaction decreases, and the reaction proceeds slowly or incompletely.
In the above method, preferably, the mass ratio of the concentrated sulfuric acid to the electrode powder is (0.1-0.5): 1, the mass concentration of the concentrated sulfuric acid is more than 60%. The adding amount of the concentrated sulfuric acid needs to be controlled within the range of the invention, the mixture becomes sticky due to excessive adding amount, the reaction is not facilitated, and the curing reaction can not be completely carried out due to too little adding amount.
In the above method, preferably, the mass ratio of the water to the electrode powder is (0.1 to 0.3): 1. the surface of solid particles of the electrode powder can be soaked by adding water, so that the sulfuric acid and the electrode powder can be fully mixed and serve as a medium for ions between concentrated sulfuric acid and the solid particles to enter and exit; the addition amount of water is too small, so that electrode powder cannot be fully wetted, the concentrated sulfuric acid and the electrode powder are not uniformly mixed, and the addition amount of water is too large, so that the concentration of sulfuric acid is reduced, and the defluorination efficiency is reduced.
In the method, preferably, the leaching temperature is 50-100 ℃ and the leaching time is 1.0-5.0 h. Leaching parameters need to be controlled within the scope of the invention, and if the leaching parameters exceed the scope of the invention, not only energy consumption is increased, but also the decomposition speed or the oxidation speed of the reducing agent is increased due to the temperature rise, so that metal can not be leached completely, or the dosage of the reducing agent is increased; if the temperature is lower than the range of the invention, the activation temperature required for the acid dissolution and reduction of the nickel-cobalt-manganese metal oxide can not be reached, and the reaction can not be completely carried out.
In the above method, preferably, the leaching agent is a mixture of sulfuric acid, water and a reducing agent, and in order to avoid bringing new impurities, the reducing agent is at least one of hydrogen peroxide, sodium sulfite, sodium thiosulfate, ferrous sulfate, sulfur dioxide and ascorbic acid.
In the method, preferably, in order to reduce the amount of neutralizing agent and extracting agent used in the subsequent valuable metal separation process and improve the leaching rate of valuable metals, the mass ratio of concentrated sulfuric acid to electrode powder in the leaching agent is (1-2): 1, the liquid-solid ratio of the mixed liquid of water and concentrated sulfuric acid in the leaching agent to the electrode powder is (5-10): 1, the ratio is expressed in L/kg. In order to improve the leaching rate of valuable metals, the addition amount of the reducing agent is 1.5-5.0 times of the theoretical amount required for reducing the high-valence nickel, cobalt and manganese in the electrode powder into bivalent metal.
In the method, the pretreatment preferably includes discharging, dismantling, crushing, sorting and removing organic matters.
In the above method, preferably, the removal of organic matters means that organic matters contained in the sorted materials are removed by a cracking method, an oxidizing roasting method or an organic solvent dissolving method.
In the method, the fluorine content in the valuable metal leaching solution is preferably less than 0.25 g/L.
Compared with the prior art, the invention has the advantages that:
according to the method, the removal of fluorine in the electrode powder and the leaching of valuable metals are organically combined, a curing and defluorination step is added before the acid leaching of the electrode powder, namely, part of concentrated sulfuric acid is firstly added into the electrode powder for curing and defluorination, part of sulfuric acid is added into the electrode powder after defluorination for leaching, and the electrode powder are tightly connected; compared with the conventional acid leaching process, the method has the advantages of no increase of acid consumption, low process cost, strong operability, low fluorine content of the obtained valuable metal leaching solution and easy realization of industrial production.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps:
firstly, discharging a ternary lithium ion battery monomer, then removing a shell, volatilizing electrolyte, then taking out an inner core for crushing, then sorting to obtain a positive-negative electrode mixed material, carrying out vacuum cracking on the mixed material at 400 ℃, and further removing organic matters such as the electrolyte, a binder and the like to obtain electrode powder. The main components of the electrode powder are Ni 33.49%, Co 12.36%, Mn 14.22%, Li 7.45% and F3.89%.
Taking 100.0g of electrode powder, adding 15.0ml of water and 27.7ml of 98% sulfuric acid, uniformly mixing, then putting into a drying oven, preserving heat and curing for 3.0h at 120 ℃, adding 55.5ml of 98% sulfuric acid, 850ml of water and 40.0ml of 30% hydrogen peroxide into a cured material after curing is finished, stirring and leaching for 2.0h at 60 ℃, and then filtering to obtain 995ml of valuable metal leaching solution with low fluorine content. The valuable metal leaching solution with low fluorine content mainly comprises 33.50g/L, Co 12.40.40 g/L, Mn 14.25.25 g/L, Li 7.09.09 g/L, F0.19.19 g/L of Ni, and the removal rate of F is 95.14%.
Comparative example 1;
a method for leaching valuable metals from waste lithium ion batteries comprises the following steps:
100.0g of the electrode powder pretreated in example 1 was weighed, added with 84.0ml of 98% sulfuric acid, 850ml of water and 40.0ml of 30% hydrogen peroxide, stirred and leached at 60 ℃ for 2.0 hours, and then filtered to obtain 1000ml of valuable metal leaching solution. The main component of the valuable metal leaching solution is Ni 33.39g/L, Co 12.40.40 g/L, Mn 14.15.15 g/L, Li 6.99.99 g/L, F3.85.85 g/L, and the removal rate of F is only 1.03%.
Example 2:
the invention relates to a method for synchronously defluorinating valuable metals leached from waste lithium ion batteries, which comprises the following steps:
firstly, discharging, disassembling, crushing and sorting a 18650 type lithium cobalt oxide battery to obtain a positive-negative electrode mixed material, oxidizing and roasting the mixed material at 600 ℃, and removing organic matters such as electrolyte, a binder and the like to obtain electrode powder. The main components of the electrode powder are Co 20.13, Li 3.87% and F4.58%.
Taking 100.0g of electrode powder, adding 10.0ml of water and 18.0ml of 90% sulfuric acid, uniformly mixing, then putting into a drying oven, preserving heat and curing for 5.0h at 150 ℃, adding 78.0ml of 90% sulfuric acid, 650ml of water and 50.0ml of 30% hydrogen peroxide into a cured material after curing is finished, stirring and leaching for 3.0h at 80 ℃, and then filtering to obtain 795ml of valuable metal leaching solution with low fluorine content. The valuable metal leaching solution with low fluorine content mainly comprises Co25.30g/L, Li 4.79.79 g/L, F0.23.23 g/L, and the removal rate of F is 96.01%.
Comparative example 2:
a method for leaching valuable metals from waste lithium ion batteries comprises the following steps:
100.0g of the electrode powder pretreated in example 2 was weighed, 96.0ml of 90% sulfuric acid, 650ml of water and 50.0ml of 30% hydrogen peroxide were added, stirred and leached at 80 ℃ for 3.0 hours, and then filtered to obtain 800ml of valuable metal leachate, the main component of which is Co 25.00g/L, Li 4.75.75 g/L, F5.76.76 g/L, and the removal rate of F is only 0.96%.
Claims (10)
1. A method for synchronously defluorinating valuable metals leached from waste lithium ion batteries is characterized by comprising the following steps: pretreating a waste lithium ion battery to obtain electrode powder, uniformly mixing the electrode powder with water and concentrated sulfuric acid, curing at 50-200 ℃ for 1.0-24.0 h, adding a leaching agent into the cured material for leaching after curing, and filtering after leaching to obtain the valuable metal leaching solution with low fluorine content.
2. The method according to claim 1, wherein the mass ratio of the concentrated sulfuric acid to the electrode powder is (0.1-0.5): 1; the mass concentration of the concentrated sulfuric acid is more than 60%.
3. The method according to claim 1 or 2, wherein the mass ratio of the water to the electrode powder is (0.1-0.3): 1.
4. the method according to claim 1 or 2, wherein the leaching temperature is 50-100 ℃ and the leaching time is 1.0-5.0 h.
5. A method according to claim 1 or 2, characterized in that the leaching agent is a mixture of concentrated sulphuric acid, water and a reducing agent.
6. The method of claim 5, wherein the reducing agent is at least one of hydrogen peroxide, sodium sulfite, sodium thiosulfate, ferrous sulfate, sulfur dioxide, and ascorbic acid.
7. The method according to claim 6, wherein the mass ratio of concentrated sulfuric acid to electrode powder in the leaching agent is (1-2): 1; the liquid-solid ratio of the mixed liquid of water and concentrated sulfuric acid in the leaching agent to the electrode powder is (5-10): 1, the unit of the ratio is L/kg; the addition amount of the reducing agent is 1.5-5.0 times of the theoretical amount required for reducing the high-valence nickel, cobalt and manganese in the electrode powder into bivalent nickel.
8. The method according to claim 1 or 2, wherein the pre-treatment comprises electrical discharge, dismantling, crushing, sorting, removal of organic matter.
9. The method according to claim 8, wherein the removing of the organic substances is removing the organic substances contained in the sorted materials by a cracking method, an oxidizing roasting method or an organic solvent dissolving method.
10. The method according to claim 1 or 2, wherein the level of fluorine in the value metal leach solution is less than 0.25 g/L.
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| CN113415813A (en) * | 2021-06-22 | 2021-09-21 | 四川长虹格润环保科技股份有限公司 | Method for recovering lithium nickel cobalt manganese from waste ternary battery material |
| CN113621800A (en) * | 2021-08-11 | 2021-11-09 | 郑州大学 | Method for treating acid leaching solution containing fluorine |
| CN113846224A (en) * | 2021-10-25 | 2021-12-28 | 贵州中伟资源循环产业发展有限公司 | Method for recovering valuable metal from positive electrode material containing binder and valuable metal |
| CN113897490A (en) * | 2021-12-13 | 2022-01-07 | 矿冶科技集团有限公司 | Defluorination method and application of lithium ion battery anode material leaching solution |
| CN115986251A (en) * | 2023-01-09 | 2023-04-18 | 深圳市新昊青科技有限公司 | Method for removing fluorine in lithium ion battery powder |
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