CN109734107A - A kind of resource recycle method of the useless positive electrode of lithium battery - Google Patents
A kind of resource recycle method of the useless positive electrode of lithium battery Download PDFInfo
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- CN109734107A CN109734107A CN201811623549.0A CN201811623549A CN109734107A CN 109734107 A CN109734107 A CN 109734107A CN 201811623549 A CN201811623549 A CN 201811623549A CN 109734107 A CN109734107 A CN 109734107A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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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
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- 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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The present invention provides a kind of resource recycle method of useless positive electrode of lithium battery, includes the following steps: that 1) the useless positive electrode sulfuric acid of lithium battery and hydrogen peroxide restore acidleach, obtain the first solution after filters pressing;2) the first solution is adjusted into pH value, the second solution is obtained after filters pressing;3) the second solution is divided into the second solution I and the second solution II;4) the second solution I is concentrated by evaporation through MVR, centrifugation respectively obtains sulfuric acid crystalline lithium and the first centrifuge mother liquor water;5) the second solution II is added in the first centrifuge mother liquor water and is diluted, crystallisation by cooling, centrifugation respectively obtains a kind of and the second centrifuge mother liquor water in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol.A kind of crystal purity is high in the sulfuric acid crystalline lithium and nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol that resource recycle method of the present invention obtains, and is used separately as the raw material and production positive electrode material precursor raw material of production lithium carbonate or lithium hydroxide.
Description
Technical field
The invention belongs to technical fields of recycling used batteries, and in particular to the valuable gold of nickel, cobalt, aluminium, lithium into waste lithium cell
The method that the hydrometallurgic recovery of category utilizes.
Background technique
In recent years, the explosive growth of new-energy automobile has pushed flourishing for lithium battery industry.The lithium electricity produced every year
Pond just has several hundred million, and is increased with the speed for being more than 20%.The quantity of old and useless battery is also rapidly increasing simultaneously, it is contemplated that arrives
The year two thousand twenty, lithium battery learies reach 32GWH or more, about 500,000 tons of battery materials.
The positive electrode of lithium battery is mainly by LiFePO4, cobalt acid lithium, LiMn2O4, lithium nickelate, nickle cobalt lithium manganate etc. at present,
These lithium batteries usually contain nickel, cobalt, manganese, lithium and a small amount of iron, aluminium in obtained positive electrode after dismantling pretreatment
Deng.If cannot get safe disposal, heavy metal therein causes significant damage to environment, while will also result in the huge wave of resource
Take.Especially strategy metal cobalt and lithium, the in short supply metal resource current as China, the economic value recycled are very high.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of useless positive electrodes of lithium battery
Resource recycle method, include the following steps: 1) acidleach: the useless positive electrode sulfuric acid of lithium battery and hydrogen peroxide restore acidleach, pressure
The first solution is obtained after filter;2) clean: the first solution that step 1) is obtained adjusts pH value, and the second solution is obtained after filters pressing;3)
The second solution that step 2) is obtained is divided into the second solution I and the second solution II;4) MVR evaporative crystallization: step 3) is obtained
Second solution I is concentrated by evaporation through MVR, and centrifugation respectively obtains sulfuric acid crystalline lithium and the first centrifuge mother liquor water;5) it crystallisation by cooling: will walk
Rapid the second solution II 3) obtained, which is added in the first centrifuge mother liquor water that step 4) obtains, to be diluted, and crystallisation by cooling, centrifugation obtains respectively
To a kind of and the second centrifuge mother liquor water in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol.This hair
The sulfuric acid crystalline lithium and nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol that bright resource recycle method obtains
A kind of middle crystal purity is high, and sulfuric acid crystalline lithium is used as the raw material of production lithium carbonate or lithium hydroxide, nickel cobalt sulfate eutectic, nickel
A kind of crystal can be directly used as production positive electrode material precursor raw material in vitriol and cobalt vitriol, and the second centrifugation is female
Liquid water can return to MVR evaporative crystallization.The resource recycle method is simple, and investment is small, at low cost, is conducive to large-scale production.
In order to achieve the above objects and other related objects, the present invention is achieved by the following technical solutions:
The present invention provides a kind of resource recycle method of anode material of lithium battery, includes the following steps:
1) acidleach: the useless positive electrode sulfuric acid of lithium battery and hydrogen peroxide restore acidleach, and the first solution is obtained after filters pressing;
2) clean: the first solution that step 1) is obtained adjusts pH value, and the second solution is obtained after filters pressing;
3) the second solution for obtaining step 2) is divided into the second solution I and the second solution II;
4) MVR evaporative crystallization: the second solution I that step 3) is obtained is concentrated by evaporation through MVR, and centrifugation respectively obtains lithium sulfate
Crystal and the first centrifuge mother liquor water;
5) crystallisation by cooling: the second solution II that step 3) obtains is added dilute in the first centrifuge mother liquor water that step 4) obtains
It releases, crystallisation by cooling, centrifugation respectively obtains a kind of in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol
With the second centrifuge mother liquor water.
The useless positive electrode of lithium battery refers to lithium nickelate, cobalt acid lithium and nickel cobalt lithium aluminate that useless new energy anode dismantles
At least one of solid waste, the i.e. solid waste of nickel-and aluminum-containing lithium, cobalt and aluminium containing lithium or nickel and cobalt containing aluminium lithium metal ingredient, mainly
Ingredient is nickel 0-60wt%, cobalt 0-60wt%, aluminium 1-20wt%, lithium 2-20wt%, wherein the total content of nickel and cobalt is 2-
60wt%.
Preferably, the second centrifuge mother liquor water that step 5) obtains is back to step 4).
Preferably, in step 1), the reaction end pH value for restoring acidleach is 2-3, such as 2-2.3 or 2.3-3.
Preferably, in step 2), carbonate is added or hydroxide adjusts pH value to 4-6, such as 4-5 or 5-6.
It is highly preferred that the carbonate is at least one of carbonate and carbonate of cobalt of nickel, the hydroxide
For at least one of the hydroxide of nickel and hydroxide of cobalt.
Preferably, in step 4), it is 70-95 DEG C, such as 70-90 DEG C or 90-95 DEG C that MVR, which is concentrated by evaporation temperature,.
Preferably, in step 4), it is 1.52-1.57 that the second solution I that step 3) obtains, which is concentrated by evaporation through MVR to specific gravity,
After be centrifuged, as MVR be concentrated by evaporation to specific gravity be 1.52-1.53 or 1.53-1.57.
Preferably, in step 5), the first centrifuge mother liquor water that step 4) obtains controls specific gravity by the way that the second solution II is added
For 1.45-1.49, such as 1.45-1.47 or 1.47-1.49.
Preferably, in step 5), crystallisation by cooling temperature is 15-25 DEG C, such as 15-20 DEG C or 20-25 DEG C.
The present invention provides a kind of resource recycle method of useless positive electrode of lithium battery, just mainly for useless new energy battery
At least one of lithium nickelate, cobalt acid lithium and nickel cobalt lithium aluminate that pole dismantles solid waste, these positive electrodes provide at present
The problems such as that there are energy consumptions in sourceization recycling is high, long flow path, the present invention include the following steps: 1) acidleach: lithium battery gives up positive electrode
Acidleach is restored with sulfuric acid and hydrogen peroxide, the first solution is obtained after filters pressing;2) clean: the first solution that step 1) is obtained adjusts pH
Value, obtains the second solution after filters pressing;3) the second solution for obtaining step 2) is divided into the second solution I and the second solution II;4)MVR
Evaporative crystallization: the second solution I that step 3) is obtained is concentrated by evaporation through MVR, centrifugation respectively obtain sulfuric acid crystalline lithium and first from
Heart mother liquid coming;5) crystallisation by cooling: the second solution II that step 3) obtains is added in the first centrifuge mother liquor water that step 4) obtains
Dilution, crystallisation by cooling, centrifugation respectively obtain one in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol
Kind and the second centrifuge mother liquor water.The sulfuric acid crystalline lithium and nickel cobalt sulfate eutectic, nickel that resource recycle method of the present invention obtains
A kind of crystal purity is high in vitriol and cobalt vitriol, and sulfuric acid crystalline lithium is used as production lithium carbonate or lithium hydroxide
Raw material, a kind of crystal can be directly used as production anode in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol
Material precursor raw material, the second centrifuge mother liquor water can return to MVR evaporative crystallization.The resource recycle method is simple, and investment is small,
It is at low cost, be conducive to large-scale production.
Detailed description of the invention
Fig. 1 is the process flow chart of the resource recycle method of the useless positive electrode of lithium battery of the invention.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Disclosed content understands further advantage and effect of the invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Embodiment 1
A kind of resource recycle method of the useless positive electrode of lithium battery, as shown in Figure 1, including the following steps:
1) 3.1 tons of anode material of lithium battery are taken, wherein nickeliferous 927kg, cobalt 662kg, lithium 156kg, aluminium 113kg are added to
25m3Soft water in be beaten, sulfuric acid and hydrogen peroxide is added, the pH of solution reaches 2 after reaction 3 hours, and filters pressing obtains the first solution
21m3, wherein nickel cobalt manganese total concentration reaches 76g/l;
2) pH to 4 that the first solution is adjusted with nickelous carbonate, obtains the second solution, wherein aluminium ion concentration 7mg/l after filters pressing;
3) the second solution for obtaining step 2) is divided into 19m3Second solution I and 2m3Second solution II;
4) for the second solution I into MVR vapo(u)rization system, evaporating temperature is 70 DEG C, there is a large amount of sulfuric acid when being concentrated to specific gravity 1.52
Crystalline lithium respectively obtains sulfuric acid crystalline lithium and the first centrifuge mother liquor water after high temperature centrifugation, lithium content reaches into rotary process
10.6%, the purity of lithium sulfate reaches 96.9%, can use the raw material for doing lithium hydroxide or lithium carbonate production;
5) the first centrifuge mother liquor water is added the second solution II and is diluted to specific gravity 1.45, is cooled back to 25 DEG C of low temperature crystallizations, from
The nickel cobalt sulfate eutectic and the second centrifuge mother liquor water that the heart respectively obtains, nickel cobalt total content are 20.5%, and lithium content exists
0.05%, the raw material for doing production ternary precursor can be used.
Embodiment 2
A kind of resource recycle method of the useless positive electrode of lithium battery, as shown in Figure 1, including the following steps:
1) totally 3.3 tons of anode material of lithium battery, lithium cobaltate cathode material etc. are taken, wherein nickeliferous 1053kg, cobalt 960kg, lithium
191kg, aluminium 101kg, is added to 23m3Soft water in be beaten, sulfuric acid and hydrogen peroxide is added, the PH of solution reaches after reaction 5 hours
3, filters pressing obtains the first solution 20m3, wherein nickel cobalt manganese total concentration reaches 96g/l;
2) PH to 6 that the first solution is adjusted with nickelous carbonate, obtains the second solution, wherein aluminium ion concentration 5mg/l after filters pressing;
3) the second solution for obtaining step 2) is divided into 15m3Second solution I and 5m3Second solution II;
4) for the second solution I into MVR vapo(u)rization system, evaporating temperature is 95 DEG C, there is a large amount of sulfuric acid when being concentrated to specific gravity 1.57
Crystalline lithium respectively obtains sulfuric acid crystalline lithium and the first centrifuge mother liquor water after high temperature centrifugation, lithium content reaches into rotary process
10.5%, the purity of lithium sulfate reaches 96%, can use the raw material for doing lithium hydroxide or lithium carbonate production;
5) the first centrifuge mother liquor water is added the second solution II and is diluted to specific gravity 1.49, is cooled back to 15 DEG C of low temperature crystallizations, from
The nickel cobalt sulfate eutectic and the second centrifuge mother liquor water that the heart respectively obtains, nickel cobalt manganese total content are 20.1%, and lithium content exists
0.04%, the raw material for doing production ternary precursor can be used.
Embodiment 3
A kind of resource recycle method of the useless positive electrode of lithium battery, as shown in Figure 1, including the following steps:
1) totally 3.5 tons of lithium cobaltate cathode material, lithium nickelate positive electrode are taken, wherein nickeliferous 1122kg, cobalt 558kg, lithium
203kg, aluminium 81kg, is added to 23m3Soft water in be beaten, sulfuric acid and hydrogen peroxide is added, the PH of solution reaches after reaction 4 hours
2.3, filters pressing obtains the first solution 20.5m3, wherein nickel cobalt manganese total concentration reaches 82g/l;
2) PH to 5 that the first solution is adjusted with nickelous carbonate, obtains the second solution, wherein aluminium ion concentration 7mg/l after filters pressing;
3) the second solution for obtaining step 2) is divided into 16.5m3Second solution I and 4m3Second solution II;
4) for the second solution I into MVR vapo(u)rization system, evaporating temperature is 90 DEG C, there is a large amount of sulfuric acid when being concentrated to specific gravity 1.53
Crystalline lithium respectively obtains sulfuric acid crystalline lithium and the first centrifuge mother liquor water after high temperature centrifugation, lithium content reaches into rotary process
10.6%, the purity of lithium sulfate reaches 96.9%, can use the raw material for doing lithium hydroxide or lithium carbonate production;
5) the first centrifuge mother liquor water is added the second solution II and is diluted to specific gravity 1.47, is cooled back to 20 DEG C of low temperature crystallizations, from
The nickel cobalt sulfate eutectic and the second centrifuge mother liquor water that the heart respectively obtains, wherein nickel cobalt manganese total content is 20.3%, lithium content
0.05%, the raw material for doing production ternary precursor can be used.
The above, only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that under the premise of not departing from the method for the present invention, can also be made for those skilled in the art
Several improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are equivalent embodiment of the invention;Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution of any equivalent variations made by above-described embodiment, still fall within the range of technical solution of the present invention
It is interior.
Claims (9)
- The resource recycle method of positive electrode 1. a kind of lithium battery gives up, which comprises the steps of:1) acidleach: the useless positive electrode sulfuric acid of lithium battery and hydrogen peroxide restore acidleach, and the first solution is obtained after filters pressing;2) clean: the first solution that step 1) is obtained adjusts pH value, and the second solution is obtained after filters pressing;3) the second solution for obtaining step 2) is divided into the second solution I and the second solution II;4) MVR evaporative crystallization: the second solution I that step 3) is obtained is concentrated by evaporation through MVR, and centrifugation respectively obtains sulfuric acid crystalline lithium With the first centrifuge mother liquor water;5) crystallisation by cooling: the second solution II that step 3) obtains being added in the first centrifuge mother liquor water that step 4) obtains and is diluted, Crystallisation by cooling, centrifugation respectively obtain in nickel cobalt sulfate eutectic, nickel vitriol and cobalt vitriol it is a kind of and Second centrifuge mother liquor water.
- 2. resource recycle method as described in claim 1, which is characterized in that the second centrifuge mother liquor water that step 5) obtains returns It is back to step 4).
- 3. resource recycle method as described in claim 1, which is characterized in that in step 1), restore the reaction end of acidleach PH value is 2-3.
- 4. resource recycle method as described in claim 1, which is characterized in that in step 2), carbonate or hydrogen-oxygen is added Compound adjusts pH value to 4-6.
- 5. resource recycle method as claimed in claim 2, which is characterized in that the carbonate is the carbonate and cobalt of nickel At least one of carbonate, the hydroxide are at least one of hydroxide and hydroxide of cobalt of nickel.
- 6. resource recycle method as described in claim 1, which is characterized in that in step 4), MVR is concentrated by evaporation temperature and is 70-95℃。
- 7. resource recycle method as described in claim 1, which is characterized in that in step 4), step 3) is obtained second Solution I through MVR be concentrated by evaporation to specific gravity be 1.52-1.57 after be centrifuged.
- 8. resource recycle method as described in claim 1, which is characterized in that in step 5), step 4) obtain first from Heart mother liquid coming is 1.45-1.49 by the way that the second solution II is added to control specific gravity.
- 9. resource recycle method as described in claim 1, which is characterized in that in step 5), crystallisation by cooling temperature is 15-25 ℃。
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Cited By (8)
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CN111036651A (en) * | 2019-12-26 | 2020-04-21 | 甘肃睿思科新材料有限公司 | Recovery system of positive electrode waste slurry of lithium battery |
US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
CN112939315A (en) * | 2021-02-07 | 2021-06-11 | 阳江市联邦金属化工有限公司 | Treatment process for realizing zero discharge of cobalt-nickel industrial wastewater |
CN113258158A (en) * | 2021-04-27 | 2021-08-13 | 湖北金泉新材料有限公司 | Treatment method for recycling waste lithium ion batteries |
WO2022032344A1 (en) * | 2020-08-12 | 2022-02-17 | Resource Conservation and Recycling Corporation Pty Ltd | Process for recovering metal values from process liquors |
WO2023286684A1 (en) * | 2021-07-16 | 2023-01-19 | 戸田工業株式会社 | Method for producing lithium sulfate and transition metal sulfate |
WO2023286683A1 (en) * | 2021-07-16 | 2023-01-19 | 戸田工業株式会社 | Method for manufacturing high-purity nickel sulfate |
WO2023006826A1 (en) * | 2021-07-29 | 2023-02-02 | Umicore | Crystallization process for the separation of metals |
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CN111036651A (en) * | 2019-12-26 | 2020-04-21 | 甘肃睿思科新材料有限公司 | Recovery system of positive electrode waste slurry of lithium battery |
US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
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WO2022032344A1 (en) * | 2020-08-12 | 2022-02-17 | Resource Conservation and Recycling Corporation Pty Ltd | Process for recovering metal values from process liquors |
CN112939315A (en) * | 2021-02-07 | 2021-06-11 | 阳江市联邦金属化工有限公司 | Treatment process for realizing zero discharge of cobalt-nickel industrial wastewater |
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