CN107293820A - A kind of method that metal is reclaimed from waste and old lithium ion battery - Google Patents
A kind of method that metal is reclaimed from waste and old lithium ion battery Download PDFInfo
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- CN107293820A CN107293820A CN201710648304.2A CN201710648304A CN107293820A CN 107293820 A CN107293820 A CN 107293820A CN 201710648304 A CN201710648304 A CN 201710648304A CN 107293820 A CN107293820 A CN 107293820A
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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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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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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- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to waste lithium cell recovery technology field, specifically a kind of method that metal is reclaimed from waste and old lithium ion battery comprises the following steps:(1) anode waste of lithium ion battery is reclaimed, and electrode slice is made in anode waste;(2) using above-mentioned electrode slice as negative electrode, inert electrode is, to electrode, to be electrochemically reacted in acidic electrolysis bath, metal is leached, obtain the solution containing metal ion;(3) it is 9~10 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5 benzene tertacarbonic acids added in supernatant, 5~12h of hydro-thermal reaction, obtains metal organic composite material at 100~160 DEG C;The metal is nickel and/or cobalt, is leached the metal in positive electrode by the method for electrochemistry, it is ensured that the completeness of leaching;Meanwhile, the metal leached and organic matter are subjected to complexation reaction, they are that the valuable metal in anode waste opens a new application direction as the application of new lithium battery anode or supercapacitor positive electrode.
Description
Technical field
The present invention relates to waste lithium cell recovery technology field, specifically one kind is reclaimed from waste and old lithium ion battery
The method of metal.
Background technology
In recent years, because environmental pollution and problem of energy crisis become increasingly conspicuous, new-energy automobile and power accumulator are obtained
The development advanced by leaps and bounds, power accumulator includes lead-acid accumulator, Ni-MH power cell and lithium-ion-power cell, wherein have
There is the lithium-ion-power cell of high-energy-density and cycle characteristics, be described as the optimum growth direction of following power accumulator, with
The continuous renewal replacement and the continuous lifting of new-energy automobile volume of production and marketing of electric equipment products, waste lithium cell will be caused
Quantity sharply increase, in waste lithium cell contain substantial amounts of lithium metal and cobalt, because lithium belongs to rare metal, cobalt is defined as
Strategy metal, if these scarce resources are not recycled, will certainly cause the huge waste of resource, therefore useless old lithium
The recycling in pond turns into study hotspot in recent years.
Positive electrode includes the metals such as cobalt, nickel, manganese, lithium, iron, aluminium, with higher recovery value, therefore useless old lithium
The positive electrode recovery in pond is the core that lithium battery is reclaimed, and lithium battery positive pole active substance is bonded in aluminium foil by bonding agent
Surface, each element in separation aluminium foil and active material and separating active substances is core and difficulty in whole removal process
Point, the recovery of waste lithium cell positive electrode mainly includes mechanical milling method, chemical precipitation method, salting out method, solvent extraction.And
Above method, which more or less can all exist, extracts incomplete phenomenon, or can not obtain pure product, and material is reclaimed to postorder
Application cause difficulty.
The content of the invention
For the problems of the prior art, added it is an object of the invention to provide a kind of efficiently quick, purpose product
The high method that metal is reclaimed from waste and old lithium ion battery of value.
To achieve these goals, the present invention is achieved using following technical scheme:
A kind of method that metal is reclaimed from waste and old lithium ion battery, comprises the following steps:
(1) anode waste of lithium ion battery is reclaimed, and electrode slice is made in anode waste;
(2) using above-mentioned electrode slice as negative electrode, inert electrode is, to electrode, to be electrochemically reacted in acidic electrolysis bath,
Metal is leached, the solution containing metal ion is obtained;
(3) it is 9~10 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2 is added in supernatant,
4,5- benzene tertacarbonic acids, 5~12h of hydro-thermal reaction, obtains metal organic composite material at 100~160 DEG C;
The metal is nickel and/or cobalt.
The key of the present invention is the method using electrochemistry, can be realized by adjusting the current density of electrochemical reaction
It is electrolysed out rare metallic element completely from anode waste, then using 1,2,4,5- benzene tertacarbonic acids are led to as organic ligand
Hydro-thermal reaction is crossed, Coordinate self-assembly is carried out with metal ion nickel and cobalt, obtains the Porous coordination polymer of metal organic framework, it is real
The effective recycling of nickel and cobalt in anode waste is showed, obtained metal organic composite material can be as new lithium battery just
Applied on pole material or supercapacitor positive electrode.
Further, according to the present invention, heretofore described inert electrode is graphite, titanium plate or platinum sheet.
Further, according to the present invention, the acidic electrolysis bath in the present invention in step (2) includes following material:Mx+, it is organic
Acid, inorganic acid, surfactant, reducing agent;
In order to promote nickel and cobalt in anode waste to be efficiently leached, described Mx+For Na+、K+、Zn2+、Fe2+、Mg2 +、Al3+At least one of, further, described Mx+Concentration be 0.1-0.6mol/L, Mx+Concentration electrolyte is led
Electrical property has a very big impact, when concentration is too low, and electrolytic speed can be extremely slow.
Further, according to the present invention, heretofore described organic acid is in citric acid, formic acid, acetic acid, malic acid
At least one, the inorganic acid is at least one of hydrochloric acid, nitric acid, sulfuric acid.
The effect that heretofore described surfactant was soaked, and permeated and reduced surface tension in the electrolytic solution is true
Protect cell reaction efficiently, thoroughly to carry out, surfactant well-known to those skilled in the art can be used, Ke Yiju
Go out as stearic acid, neopelex, quaternary ammonium compound, lecithin, amino acid pattern, alkyl glucoside, fatty glyceride,
At least one of fatty acid sorbitan, polysorbate.
Further, according to the present invention, heretofore described reducing agent is in ascorbic acid, hydroxylamine hydrochloride, hydrazine hydrate
It is at least one.
According to the present invention, the current density of heretofore described electrochemical reaction is 5~30mA/cm2, potential window is
0.2~0.5V.
Further, according to the present invention, thickness and the compacted density of electrode slice have close pass for the efficiency of electrolysis
System, compacted density is too low, is compacted not blocking, it is difficult to used as electrolysis pole piece, and the thickness of heretofore described electrode slice is 0.2
~3cm, compacted density is 3~10g/cm3。
Further, the temperature of the hydro-thermal reaction is 120~150 DEG C, and the time is 6~10h.
According to the present invention, the recovery method of heretofore described anode waste comprises the following steps:
(1.1) lithium ion battery scrapped that collection comes is positioned over to 0.1~0.5mol/L sodium hydroxide at room temperature
The discharge process of progress 3~6 hours in the aqueous solution;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, obtained
Positive plate, negative plate, barrier film and battery case, lug;
(1.2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 500 DEG C~600 DEG C;Forge
Residue after burning is handled using 1mol/L NaOH solution, and metal is obtained through filtering, washing, drying, grinding after processing
Composite powder.
Compared with prior art, the present invention has the following technical effect that:By the method for electrochemistry by positive electrode
Metal is leached, and valuable metal is fast and efficiently entered in electrolyte, it is ensured that the completeness of leaching;Meanwhile, by what is leached
Metal carries out complexation reaction with organic matter, is that the valuable metal in anode waste opens a new application direction, as new
Lithium battery anode or supercapacitor positive electrode application, it is to avoid the not clear embarrassment of application direction after valuable metal is extracted, separately
Outside, the Rapid Leaching of rare metal can be both realized at normal temperatures, and condition is coincide, compared to the leaching of traditional acid+reducing agent,
More save, saved the consumption of acid.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is furture elucidated.
Embodiment 1
A kind of method that metallic nickel is reclaimed from waste and old lithium ion battery, comprises the following steps:
(1) the next lithium ion battery scrapped will be collected to be positioned in 0.2mol/L sodium hydrate aqueous solution at room temperature
The discharge process of progress 4 hours;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, positive plate, negative pole is obtained
Piece, barrier film and battery case, lug;
(2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 500 DEG C;Remnants after calcining
Thing is handled using 1mol/L NaOH solution, and metal composite powder is obtained through filtering, washing, drying, grinding after processing,
Then the metal composite powder is pressed into electrode slice, the thickness of described electrode slice is 1cm, and compacted density is 6g/cm3;
(3) using above-mentioned electrode slice as negative electrode, graphite is, to electrode, to be electrochemically reacted in acidic electrolysis bath, described
Acidic electrolysis bath include 0.4mol/L Na+, citric acid, hydrochloric acid, ascorbic acid and stearic acid surface activating agent, adjusting PH is
5.2, electric current is that density is 20mA/cm2, potential window is 0.4V, and metallic nickel is leached, and obtains the solution containing nickel ion;
(4) it is 9 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5- is added in supernatant
Benzene tertacarbonic acid, the hydro-thermal reaction 8h at 130 DEG C, obtains metallic nickel organic composite material.
Embodiment 2
A kind of method that metallic cobalt is reclaimed from waste and old lithium ion battery, comprises the following steps:
(1) the next lithium ion battery scrapped will be collected to be positioned in 0.3mol/L sodium hydrate aqueous solution at room temperature
The discharge process of progress 5 hours;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, positive plate, negative pole is obtained
Piece, barrier film and battery case, lug;
(2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 550 DEG C;Remnants after calcining
Thing is handled using 1mol/L NaOH solution, and metal composite powder is obtained through filtering, washing, drying, grinding after processing,
Then the metal composite powder is pressed into electrode slice, the thickness of described electrode slice is 2cm, and compacted density is 6g/cm3;
(3) using above-mentioned electrode slice as negative electrode, titanium plate is, to electrode, to be electrochemically reacted in acidic electrolysis bath, described
Acidic electrolysis bath include 0.3mol/L K+, formic acid, nitric acid, hydroxylamine hydrochloride and neopelex surfactant,
It is 5.5 to adjust PH, and electric current is that density is 22mA/cm2, potential window is 0.3V, and metallic nickel is leached, obtained containing nickel ion
Solution;
(4) it is 9 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5- is added in supernatant
Benzene tertacarbonic acid, the hydro-thermal reaction 7h at 110 DEG C, obtains metallic cobalt organic composite material.
Embodiment 3
A kind of method that metallic nickel is reclaimed from waste and old lithium ion battery, comprises the following steps:
(1) the next lithium ion battery scrapped will be collected to be positioned in 0.1mol/L sodium hydrate aqueous solution at room temperature
The discharge process of progress 6 hours;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, positive plate, negative pole is obtained
Piece, barrier film and battery case, lug;
(2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 600 DEG C;Remnants after calcining
Thing is handled using 1mol/L NaOH solution, and metal composite powder is obtained through filtering, washing, drying, grinding after processing,
Then the metal composite powder is pressed into electrode slice, the thickness of described electrode slice is 0.8cm, and compacted density is 9g/
cm3;
(3) using above-mentioned electrode slice as negative electrode, platinum sheet is, to electrode, to be electrochemically reacted in acidic electrolysis bath, described
Acidic electrolysis bath include 0.5mol/L Zn2+, acetic acid, sulfuric acid, ascorbic acid and fatty acid glycerine ester surfactant, regulation
PH is 4.8, and electric current is that density is 10mA/cm2, potential window is 0.3V, and metallic nickel is leached, obtained containing the molten of nickel ion
Liquid;
(4) it is 10 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5- is added in supernatant
Benzene tertacarbonic acid, the hydro-thermal reaction 12h at 100 DEG C, obtains metallic nickel organic composite material.
Embodiment 4
A kind of method that metallic cobalt is reclaimed from waste and old lithium ion battery, comprises the following steps:
(1) the next lithium ion battery scrapped will be collected to be positioned in 0.5mol/L sodium hydrate aqueous solution at room temperature
The discharge process of progress 3 hours;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, positive plate, negative pole is obtained
Piece, barrier film and battery case, lug;
(2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 520 DEG C;Remnants after calcining
Thing is handled using 1mol/L NaOH solution, and metal composite powder is obtained through filtering, washing, drying, grinding after processing,
Then the metal composite powder is pressed into electrode slice, the thickness of described electrode slice is 0.8cm, and compacted density is 6g/
cm3;
(3) using above-mentioned electrode slice as negative electrode, graphite is, to electrode, to be electrochemically reacted in acidic electrolysis bath, described
Acidic electrolysis bath include 0.2mol/L Mg2+, malic acid, hydrochloric acid, ascorbic acid and fatty acid sorbitan surfactant are adjusted
It is 5.4 to save PH, and electric current is that density is 25mA/cm2, potential window is 0.4V, and metallic nickel is leached, obtained containing the molten of nickel ion
Liquid;
(4) it is 10 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5- is added in supernatant
Benzene tertacarbonic acid, the hydro-thermal reaction 5h at 160 DEG C, obtains metallic cobalt organic composite material.
The method that metallic nickel and metallic cobalt are reclaimed from waste and old lithium ion battery that the present invention is provided, it is simple efficient, and will
The nickel or cobalt of recovery and organic matter complexation reaction, obtain metal organic composite material, improve rare gold in waste and old positive electrode
The added value of category.
General principle, principal character and the features of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement is both fallen within the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (8)
1. a kind of method that metal is reclaimed from waste and old lithium ion battery, it is characterised in that:Comprise the following steps:
(1) anode waste of lithium ion battery is reclaimed, and electrode slice is made in anode waste;
(2) using above-mentioned electrode slice as negative electrode, inert electrode is, to electrode, to be electrochemically reacted in acidic electrolysis bath, by gold
Category is leached, and obtains the solution containing metal ion;
(3) it is 9~10 to adjust above-mentioned pH value of solution, after being sufficiently stirred for, and centrifugation takes supernatant, 1,2,4,5- is added in supernatant
Benzene tertacarbonic acid, 5~12h of hydro-thermal reaction, obtains metal organic composite material at 100~160 DEG C;
The metal is nickel and/or cobalt.
2. the method according to claim 1 that metal is reclaimed from waste and old lithium ion battery, wherein, in the step (2)
Acidic electrolysis bath include following material:Mx+, organic acid, inorganic acid, surfactant, reducing agent;
Wherein, the Mx+For Na+、K+、Zn2+、Fe2+、Mg2+、Al3+At least one of;And/or
The Mx+Concentration be 0.1~0.6mol/L.
3. the method according to claim 2 that metal is reclaimed from waste and old lithium ion battery, wherein, the organic acid is lemon
At least one of lemon acid, formic acid, acetic acid, malic acid;And/or
The inorganic acid is at least one of hydrochloric acid, nitric acid, sulfuric acid.
4. the method according to claim 2 that metal is reclaimed from waste and old lithium ion battery, wherein, the reducing agent is anti-
At least one of bad hematic acid, hydroxylamine hydrochloride, hydrazine hydrate.
5. the method according to claim 1 that metal is reclaimed from waste and old lithium ion battery, wherein, the electrochemical reaction
Current density be 5~30mA/cm2, potential window is 0.2~0.5V.
6. the method according to claim 1 that metal is reclaimed from waste and old lithium ion battery, wherein, the thickness of the electrode slice
Spend for 0.2~3cm, compacted density is 3~10g/cm3。
7. the method according to claim 1 that metal is reclaimed from waste and old lithium ion battery, wherein, in step (3), institute
The temperature for stating hydro-thermal reaction is 120~150 DEG C, and the time is 6~10h.
8. the method according to claim 1 that metal is reclaimed from waste and old lithium ion battery, wherein, the anode waste
Recovery method comprises the following steps:
(1.1) sodium hydroxide for the lithium ion battery scrapped that collection comes being positioned over into 0.1~0.5mol/L at room temperature is water-soluble
The discharge process of progress 3~6 hours in liquid;After discharge process, the lithium ion battery scrapped is carried out to disassemble by hand, positive pole is obtained
Piece, negative plate, barrier film and battery case, lug;
(1.2) useless positive plate shearing obtained in the previous step is crushed, then calcined 2 hours at 500 DEG C~600 DEG C;After calcining
Residue handled using 1mol/L NaOH solution, obtain metal composite through filtering, washing, drying, grinding after processing
Thing powder.
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Cited By (11)
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CN107910611A (en) * | 2017-11-17 | 2018-04-13 | 成都新柯力化工科技有限公司 | A kind of method using sodium sulfite recycling lithium battery copper current collector |
CN108075203A (en) * | 2017-12-28 | 2018-05-25 | 中南大学 | A kind of method that valuable metal component recycles in waste and old lithium ion battery material |
CN108270045A (en) * | 2018-01-05 | 2018-07-10 | 昆明理工大学 | A kind of electrochemical leaching method of waste lithium cell positive electrode |
CN109103534A (en) * | 2018-08-08 | 2018-12-28 | 广东佳纳能源科技有限公司 | A kind of recovery method of waste and old lithium ion battery |
CN110453071A (en) * | 2018-08-06 | 2019-11-15 | 南方科技大学 | The method and device thereof of metal are recycled from waste lithium cell |
CN111048862A (en) * | 2019-11-25 | 2020-04-21 | 万华化学集团股份有限公司 | Method for efficiently recovering lithium ion battery anode and cathode materials as supercapacitor electrode materials |
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CN114583306A (en) * | 2022-03-01 | 2022-06-03 | 西安交通大学 | Method for recycling all elements of waste lithium iron phosphate batteries and preparing iron-based MOFs (metal-organic frameworks) material by organic acid integrated two-in-one double-effect |
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CN107910611A (en) * | 2017-11-17 | 2018-04-13 | 成都新柯力化工科技有限公司 | A kind of method using sodium sulfite recycling lithium battery copper current collector |
CN108075203A (en) * | 2017-12-28 | 2018-05-25 | 中南大学 | A kind of method that valuable metal component recycles in waste and old lithium ion battery material |
CN108270045A (en) * | 2018-01-05 | 2018-07-10 | 昆明理工大学 | A kind of electrochemical leaching method of waste lithium cell positive electrode |
CN110453071B (en) * | 2018-08-06 | 2021-06-11 | 南方科技大学 | Method and device for recovering metal from waste lithium battery |
CN110453071A (en) * | 2018-08-06 | 2019-11-15 | 南方科技大学 | The method and device thereof of metal are recycled from waste lithium cell |
CN109103534B (en) * | 2018-08-08 | 2020-05-29 | 广东佳纳能源科技有限公司 | Recovery method of waste cobalt-containing lithium ion battery |
CN109103534A (en) * | 2018-08-08 | 2018-12-28 | 广东佳纳能源科技有限公司 | A kind of recovery method of waste and old lithium ion battery |
CN111048862A (en) * | 2019-11-25 | 2020-04-21 | 万华化学集团股份有限公司 | Method for efficiently recovering lithium ion battery anode and cathode materials as supercapacitor electrode materials |
CN112510282A (en) * | 2020-12-01 | 2021-03-16 | 北京理工大学前沿技术研究院 | Method for preparing MOF-based nano material based on waste lithium ion battery leachate |
CN114204152A (en) * | 2021-12-16 | 2022-03-18 | 恩施市致纯电子材料有限公司 | Recovery process of waste ternary lithium ion battery anode material |
WO2023108854A1 (en) * | 2021-12-16 | 2023-06-22 | 恩施市致纯电子材料有限公司 | Recovery process for positive electrode material of waste ternary lithium-ion battery |
CN114204152B (en) * | 2021-12-16 | 2024-05-24 | 深圳甦鑫科技有限公司 | Recycling process of waste ternary lithium ion battery anode material |
CN114583306A (en) * | 2022-03-01 | 2022-06-03 | 西安交通大学 | Method for recycling all elements of waste lithium iron phosphate batteries and preparing iron-based MOFs (metal-organic frameworks) material by organic acid integrated two-in-one double-effect |
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