CN107828966A - A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries - Google Patents
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries Download PDFInfo
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- CN107828966A CN107828966A CN201710948110.4A CN201710948110A CN107828966A CN 107828966 A CN107828966 A CN 107828966A CN 201710948110 A CN201710948110 A CN 201710948110A CN 107828966 A CN107828966 A CN 107828966A
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- 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
- C22B23/0476—Separation of nickel from cobalt
-
- 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
-
- 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
- C22B47/00—Obtaining manganese
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The invention discloses a kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, comprise the following steps:Ternary lithium ion cell positive powder is added to the water and carries out mashing and handles to obtain mashing liquid, the concentrated sulfuric acid and hydrogen peroxide stirring is subsequently added into, is filtrated to get pickle liquor A;Pickle liquor A is adjusted in acidity, excessive Fe powder is added to remove Cu impurity, reuses the iron aluminium impurity in halotrichite method removal solution, be filtrated to get filtered fluid B;Filtered fluid B is adjusted to alkalescence to precipitate nickel element, cobalt element, manganese element, is filtrated to get solution C and filter residue D;Solution C is concentrated, saturated sodium carbonate solution is added and obtains lithium carbonate precipitation;Filter residue D is dissolved to obtain solution E, solution E progress extract and separate is obtained into solution containing nickel, cobalt-carrying solution and manganese containing solution.Nickel cobalt manganese element is precipitated after the leaching removal of impurities of ternary lithium ion cell positive powder, separates elemental lithium first, realize the priority reclamation of lithium, improve the rate of recovery of elemental lithium by the present invention.
Description
Technical field
The present invention relates to lithium ion battery recovery technology field, more particularly to a kind of ternary anode material for lithium-ion batteries
Comprehensive recovering process.
Background technology
Within the coming years, the situation that supply falls short of demand, annual need will be presented in high-end ternary system dynamic lithium battery
The amount of asking reaches tens of thousands of tons, and the electric automobile using tesla's automobile as representative now, using ternary material lithium ion battery
Technology has progressively tended to be ripe.
At the same time, the processing recovery of ternary battery also gradually obtains everybody concern, the generation master of ternary battery waste
There are caused waste material in ternary battery production, ternary battery to scrap caused waste material.Due in ternary battery waste contain lithium,
The metals such as cobalt, nickel, manganese, and content is higher, so its recovery has higher economic value, while also has higher society's effect
Benefit.
Ternary powder handling process can be divided into three classes at present:Dry recovery technology, hydrometallurgic recovery technology and biological recovery
Technology.Wherein biological recovery technology is still immature, and part Li is had in Dry recovery technology and is entered in waste gas;Hydrometallurgic recovery skill
Art focuses on the recovery with Ni, Co and Mn, and Li recovery is placed on into technique least significant end, causes the Li rate of recovery relatively low.In lithium resource
It is increasingly rare, today of lithium salts price rapid growth, thus to develop the Li rate of recovery in a kind of raising old and useless battery powder
Recovery method.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of the comprehensive of ternary anode material for lithium-ion batteries
Recovery method is closed, the elemental lithium in advantage distillation ternary lithium ion cell positive powder, improves the rate of recovery of lithium.
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries proposed by the present invention, comprises the following steps:
S1, ternary lithium ion cell positive powder is added to the water carries out mashing and handle to obtain mashing liquid, be subsequently added into dense
Sulfuric acid and hydrogen peroxide stirring, are filtrated to get pickle liquor A;
S2, regulation pickle liquor A add excessive Fe powder to remove Cu impurity, it is molten to reuse the removal of halotrichite method in acidity
Iron aluminium impurity in liquid, is filtrated to get filtered fluid B;
S3, regulation filtered fluid B, to precipitate nickel element, cobalt element, manganese element, are filtrated to get solution C and filter residue D to alkalescence;
S4, solution C concentrated, add saturated sodium carbonate solution and obtain lithium carbonate precipitation;
S5, filter residue D dissolved to obtain solution E, solution E progress extract and separate is obtained into solution containing nickel, cobalt-carrying solution
And manganese containing solution.
Preferably, in S1, it is 1 to be beaten solid-liquid mass ratio in liquid:4-10.
Preferably, in S1, whipping temp is 60-95 DEG C, mixing time 0.5-3h.
Preferably, in S1, the amount volume ratio (mol/L) of the concentrated sulfuric acid and the material of mashing liquid is 1.5-5:1.
Preferably, in S1, the volume mass ratio (mL/g) of hydrogen peroxide and ternary lithium ion cell positive powder is 1-5:1.
Preferably, in S2, regulation pickle liquor A pH value is 2-2.5.
Preferably, in S3, regulation filtered fluid B pH value is 10-13.
Preferably, in S4, it is 10-20g/L that solution C is concentrated into elemental lithium concentration.
Preferably, in S4, the temperature of saturated solution of sodium carbonate is 85-95 DEG C.
Nickel cobalt manganese element is precipitated, divided first after the leaching removal of impurities of ternary lithium ion cell positive powder by the present invention
From elemental lithium, the priority reclamation of lithium is realized, improves the rate of recovery of elemental lithium.
Brief description of the drawings
Fig. 1 is that a kind of flow of comprehensive recovering process of ternary anode material for lithium-ion batteries proposed by the present invention is illustrated
Figure.
Embodiment
As shown in figure 1, Fig. 1 is a kind of comprehensive recovering process of ternary anode material for lithium-ion batteries proposed by the present invention
Schematic flow sheet.
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, comprises the following steps:
S1, ternary lithium ion cell positive powder is added to the water carries out mashing and handle to obtain mashing liquid, be beaten solid in liquid
Liquid mass ratio is 1:6, the concentrated sulfuric acid and hydrogen peroxide stirring 1.5h are subsequently added into, whipping temp is 70 DEG C, the concentrated sulfuric acid and mashing liquid
The amount volume ratio (mol/L) of material is 2:1, the volume mass ratio (mL/g) of hydrogen peroxide and ternary lithium ion cell positive powder is
2:1, it is filtrated to get pickle liquor A;
S2, regulation pickle liquor A add excessive Fe powder to remove Cu impurity, it is molten to reuse the removal of halotrichite method in acidity
Iron aluminium impurity in liquid, is filtrated to get filtered fluid B;
S3, regulation filtered fluid B, to precipitate nickel element, cobalt element, manganese element, are filtrated to get solution C and filter residue D to alkalescence;
S4, solution C is carried out being concentrated into elemental lithium concentration to be 12g/L, it is molten to add the saturated sodium carbonate that temperature is 88 DEG C
Liquid obtains lithium carbonate precipitation;
S5, filter residue D dissolved to obtain solution E, solution E progress extract and separate is obtained into solution containing nickel, cobalt-carrying solution
And manganese containing solution.
Embodiment 2
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, comprises the following steps:
S1, ternary lithium ion cell positive powder is added to the water carries out mashing and handle to obtain mashing liquid, be beaten solid in liquid
Liquid mass ratio is 1:8, the concentrated sulfuric acid and hydrogen peroxide stirring 2.5h are subsequently added into, whipping temp is 80 DEG C, the concentrated sulfuric acid and mashing liquid
The amount volume ratio (mol/L) of material is 4:1, the volume mass ratio (mL/g) of hydrogen peroxide and ternary lithium ion cell positive powder is
3:1, it is filtrated to get pickle liquor A;
S2, regulation pickle liquor A add excessive Fe powder to remove Cu impurity, it is molten to reuse the removal of halotrichite method in acidity
Iron aluminium impurity in liquid, is filtrated to get filtered fluid B;
S3, regulation filtered fluid B, to precipitate nickel element, cobalt element, manganese element, are filtrated to get solution C and filter residue D to alkalescence;
S4, solution C is carried out being concentrated into elemental lithium concentration to be 18g/L, it is molten to add the saturated sodium carbonate that temperature is 92 DEG C
Liquid obtains lithium carbonate precipitation;
S5, filter residue D dissolved to obtain solution E, solution E progress extract and separate is obtained into solution containing nickel, cobalt-carrying solution
And manganese containing solution.
Embodiment 3
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, comprises the following steps:
S1,1kg ternary lithium ion cell positives powder added in 4L deionized waters carry out mashing and handle to obtain mashing liquid,
The 20mol concentrated sulfuric acids and 1L hydrogen peroxide stirring 3h are subsequently added into, whipping temp is 60 DEG C, is filtrated to get pickle liquor A;
S2, regulation pickle liquor A pH value add excessive Fe powder to remove Cu impurity, add excessive sodium chlorate to 2
And sodium carbonate, regulation pH value to 2.5 remove the iron aluminium impurity in solution, are filtrated to get filtered fluid B;
S3, NaOH solids are added into filtered fluid B, regulation filtered fluid B's is first to precipitate nickel element, cobalt to pH value to 10
Element, manganese element, are filtrated to get solution C and filter residue D;
S4, solution C is carried out being concentrated into elemental lithium concentration to be 10g/L, it is molten to add the saturated sodium carbonate that temperature is 95 DEG C
Liquid obtains lithium carbonate precipitation, realizes the recovery of elemental lithium, and the rate of recovery of lithium is not less than 95%;
S5, will filter residue D add sulfuric acid in dissolving obtain solution E, by solution E progress extract and separate obtain nickel sulfate solution,
Cobalt sulfate solution and manganese sulfate solution, the rate of recovery of nickel cobalt manganese are not less than 95%.
Embodiment 4
A kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, comprises the following steps:
S1,1kg ternary lithium ion cell positives powder is added in 10L deionized waters carry out mashing and handle to be beaten
Liquid, the 15mol concentrated sulfuric acids and 5L hydrogen peroxide stirring 0.5h are subsequently added into, whipping temp is 95 DEG C, is filtrated to get pickle liquor A;
S2, regulation pickle liquor A pH value add excessive Fe powder to remove Cu impurity, add excessive chloric acid to 2.5
Sodium and sodium carbonate, regulation pH value to 3.0 remove the iron aluminium impurity in solution, are filtrated to get filtered fluid B;
S3, NaOH solids are added into filtered fluid B, regulation filtered fluid B's is first to precipitate nickel element, cobalt to pH value to 13
Element, manganese element, are filtrated to get solution C and filter residue D;
S4, solution C is carried out being concentrated into elemental lithium concentration to be 15g/L, it is molten to add the saturated sodium carbonate that temperature is 90 DEG C
Liquid obtains lithium carbonate precipitation, realizes the recovery of elemental lithium, and the rate of recovery of lithium is not less than 95%;
S5, will filter residue D add hydrochloric acid in dissolving obtain solution E, by solution E progress extract and separate obtain nickel chloride solution,
Cobalt chloride solution and manganese chloride solution, the rate of recovery of nickel cobalt manganese are not less than 95%.
Embodiment 5
A kind of reference picture 1, comprehensive recovering process of ternary anode material for lithium-ion batteries, comprises the following steps:
S1,1kg ternary lithium ion cell positives powder added in 6L deionized waters carry out mashing and handle to obtain mashing liquid,
The 18mol concentrated sulfuric acids and 3L hydrogen peroxide stirring 2h are subsequently added into, whipping temp is 85 DEG C, is filtrated to get pickle liquor A;
S2, regulation pickle liquor A pH value add excessive Fe powder to remove Cu impurity, add excessive chloric acid to 2.2
Sodium and sodium carbonate, regulation pH value to 3.5 remove the iron aluminium impurity in solution, are filtrated to get filtered fluid B;
S3, NaOH solids are added into filtered fluid B, regulation filtered fluid B's is first to precipitate nickel element, cobalt to pH value to 11.5
Element, manganese element, are filtrated to get solution C and filter residue D;
S4, solution C is carried out being concentrated into elemental lithium concentration to be 20g/L, it is molten to add the saturated sodium carbonate that temperature is 85 DEG C
Liquid obtains lithium carbonate precipitation, realizes the recovery of elemental lithium, and the rate of recovery of lithium is not less than 95%;
S5, will filter residue D add sulfuric acid in dissolving obtain solution E, by solution E progress extract and separate obtain nickel sulfate solution,
Cobalt sulfate solution and manganese sulfate solution, the rate of recovery of nickel cobalt manganese are not less than 95%.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (9)
1. a kind of comprehensive recovering process of ternary anode material for lithium-ion batteries, it is characterised in that comprise the following steps:
S1, ternary lithium ion cell positive powder is added to the water carries out mashing and handle to obtain mashing liquid, be subsequently added into the concentrated sulfuric acid
Stirred with hydrogen peroxide, be filtrated to get pickle liquor A;
S2, regulation pickle liquor A add excessive Fe powder to remove Cu impurity, reuse halotrichite method and remove in solution in acidity
Iron aluminium impurity, be filtrated to get filtered fluid B;
S3, regulation filtered fluid B, to precipitate nickel element, cobalt element, manganese element, are filtrated to get solution C and filter residue D to alkalescence;
S4, solution C concentrated, add saturated sodium carbonate solution and obtain lithium carbonate precipitation;
S5, filter residue D dissolved to obtain solution E, solution E progress extract and separate is obtained into solution containing nickel, cobalt-carrying solution and contained
Manganese solution.
2. the comprehensive recovering process of ternary anode material for lithium-ion batteries according to claim 1, it is characterised in that in S1,
It is 1 to be beaten solid-liquid mass ratio in liquid:4-10.
3. the comprehensive recovering process of ternary anode material for lithium-ion batteries according to claim 1 or claim 2, it is characterised in that S1
In, whipping temp is 60-95 DEG C, mixing time 0.5-3h.
4. according to the comprehensive recovering process of any one of the claim 1-3 ternary anode material for lithium-ion batteries, its feature exists
In in S1, the amount volume ratio (mol/L) of the concentrated sulfuric acid and the material of mashing liquid is 1.5-5:1.
5. according to the comprehensive recovering process of any one of the claim 1-4 ternary anode material for lithium-ion batteries, in S1, dioxygen
The volume mass ratio (mL/g) of water and ternary lithium ion cell positive powder is 1-5:1.
6. according to the comprehensive recovering process of any one of the claim 1-5 ternary anode material for lithium-ion batteries, its feature exists
In in S2, regulation pickle liquor A pH value is 2-2.5.
7. according to the comprehensive recovering process of any one of the claim 1-6 ternary anode material for lithium-ion batteries, its feature exists
In in S3, regulation filtered fluid B pH value is 10-13.
8. according to the comprehensive recovering process of any one of the claim 1-7 ternary anode material for lithium-ion batteries, its feature exists
In in S4, it is 10-20g/L that solution C is concentrated into elemental lithium concentration.
9. according to the comprehensive recovering process of any one of the claim 1-8 ternary anode material for lithium-ion batteries, its feature exists
In in S4, the temperature of saturated solution of sodium carbonate is 85-95 DEG C.
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CN109088116A (en) * | 2018-07-26 | 2018-12-25 | 合肥国轩高科动力能源有限公司 | A kind of recovery method of waste lithium ion cell anode powder |
CN109216821A (en) * | 2018-09-05 | 2019-01-15 | 合肥国轩高科动力能源有限公司 | A kind of recovery method of waste and old lithium titanate battery |
CN109722540A (en) * | 2019-03-01 | 2019-05-07 | 江西赣锋锂业股份有限公司 | A kind of method of tertiary cathode material pickle liquor separation and recovery lithium and nickel cobalt manganese |
CN110233304A (en) * | 2019-06-21 | 2019-09-13 | 广西大学 | The method of high efficiente callback mixing anode material for lithium-ion batteries |
CN110511015A (en) * | 2019-09-30 | 2019-11-29 | 山东凯通电子有限公司 | The preparation method of manganese-zinc ferrite |
CN110923453A (en) * | 2019-11-29 | 2020-03-27 | 中南大学 | Method for recovering lithium from waste lithium ion battery |
CN111082043A (en) * | 2019-11-26 | 2020-04-28 | 宁夏百川新材料有限公司 | Recycling method of waste nickel cobalt lithium manganate ternary battery positive electrode material |
CN111261967A (en) * | 2020-01-22 | 2020-06-09 | 宁波容百新能源科技股份有限公司 | Recovery method of waste lithium battery and battery-grade nickel-cobalt-manganese mixed crystal prepared by recovery |
CN111302408A (en) * | 2020-02-21 | 2020-06-19 | 北京蒙京石墨新材料科技研究院有限公司 | Method for recycling nickel, cobalt and manganese from scrapped lithium ion battery |
CN111825110A (en) * | 2020-05-12 | 2020-10-27 | 宁夏百川新材料有限公司 | Recycling method of waste lithium ion battery anode material |
CN112038722A (en) * | 2020-08-12 | 2020-12-04 | 中南大学 | Method for efficiently treating waste lithium iron phosphate positive plate |
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WO2021047352A1 (en) * | 2019-09-14 | 2021-03-18 | 湖南金源新材料股份有限公司 | Manganese-lithium separation and pre-extraction liquid preparation processes in comprehensive recovery of ternary battery waste, and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste |
CN112725621A (en) * | 2020-09-17 | 2021-04-30 | 湖北金泉新材料有限公司 | Method for separating nickel, cobalt and manganese from waste lithium battery based on carbonate solid-phase conversion method |
CN114427037A (en) * | 2022-01-06 | 2022-05-03 | 中国恩菲工程技术有限公司 | Method for continuously enriching nickel and cobalt from low-concentration nickel and cobalt solution |
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CN116837216A (en) * | 2023-09-01 | 2023-10-03 | 北京怀柔北珂新能源科技有限公司 | Impurity removal method for recycling positive electrode powder of lithium ion battery |
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CN109722540A (en) * | 2019-03-01 | 2019-05-07 | 江西赣锋锂业股份有限公司 | A kind of method of tertiary cathode material pickle liquor separation and recovery lithium and nickel cobalt manganese |
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JP7216945B2 (en) | 2019-09-14 | 2023-02-02 | 湖南金源新材料股▲ふん▼有限公司 | Manganese-lithium separation and pre-extraction solution preparation process in comprehensive recovery of ternary battery waste and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste |
JP2022539913A (en) * | 2019-09-14 | 2022-09-13 | 湖南金源新材料股▲ふん▼有限公司 | Manganese-lithium separation and pre-extraction solution preparation process in comprehensive recovery of ternary battery waste and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste |
WO2021047352A1 (en) * | 2019-09-14 | 2021-03-18 | 湖南金源新材料股份有限公司 | Manganese-lithium separation and pre-extraction liquid preparation processes in comprehensive recovery of ternary battery waste, and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste |
EP4030533A4 (en) * | 2019-09-14 | 2023-10-18 | Hunan Jin Yuan New Materials Joint Stock Company Limited | Manganese-lithium separation and pre-extraction liquid preparation processes in comprehensive recovery of ternary battery waste, and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste |
CN110511015A (en) * | 2019-09-30 | 2019-11-29 | 山东凯通电子有限公司 | The preparation method of manganese-zinc ferrite |
CN111082043A (en) * | 2019-11-26 | 2020-04-28 | 宁夏百川新材料有限公司 | Recycling method of waste nickel cobalt lithium manganate ternary battery positive electrode material |
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