CN104659438A - Method for preparing ternary positive electrode material precursor by virtue of waste batteries - Google Patents
Method for preparing ternary positive electrode material precursor by virtue of waste batteries Download PDFInfo
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- CN104659438A CN104659438A CN201510071447.2A CN201510071447A CN104659438A CN 104659438 A CN104659438 A CN 104659438A CN 201510071447 A CN201510071447 A CN 201510071447A CN 104659438 A CN104659438 A CN 104659438A
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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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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a method for preparing a ternary positive electrode material precursor by virtue of waste batteries. The method comprises the steps of detaching waste batteries, roasting the detached waste batteries and carrying out sulfuric acid dissolving to obtain a waste battery positive electrode material, then separating and removing metal impurities in the waste battery positive electrode material by virtue of an extraction method to obtain a sulfate solution, supplementing manganese or aluminum to prepare a mixed solution for preparing the ternary positive electrode material precursor, then sequentially adding ammonia water and a sodium hydroxide solution, reacting to generate ternary positive electrode material precursor precipitates, and finally washing and drying to obtain the ternary positive electrode material precursor. According to the method, the cyclic utilization of resources of nickel and cobalt in waste batteries is realized, and the environmental pollution caused by heavy metals is avoided; furthermore, a nickel-cobalt-aluminum precursor and a nickel-cobalt-manganese precursor are produced from the recycled waste batteries, so that the requirements on primary mineral resources are lowered, and the purchase costs of nickel and cobalt are lowered; the method adopts a simple technological process and is applicable to industrial large-scale production.
Description
Technical field
The present invention relates to the preparation method of ternary anode material precursor, specifically a kind of method utilizing refuse battery to prepare ternary anode material precursor.
Background technology
The recovery of old and useless battery and recycling are not only environmental protection and are opened up the needs of international Battery Market, and are the inevitable choices alleviated China's strategy metal resource scarcity situation, promote China's battery industry sustainable development.The heavy metal that the quantity that contains waste secondary battery does not wait or Determination of Rare-Expensive Elements are (as conventional lithium-ion battery contains cobalt 20%, copper 10%, aluminium 4.7%, iron 2.5% and lithium 0.1% etc.; Ni-MH battery containing the nickel of 30%, the cobalt of 4% and about 10% light rare earth metal), and China's cobalt, copper, nickel resources are short, domestic have a large amount of cell production companies, the secondary waste product of a certain amount of leftover pieces and 1 ~ 2% can be produced in usual Ni-MH battery and lithium ion battery production process, containing a large amount of nickel cobalt valuable metals, annual generation is thousands of metal tons, and these valuable metals, can to environment if do not recycled.Therefore recycling or harmless treatment must be carried out to refuse battery, to meet environmental protection and international Battery Market to the requirement of producer responsibility.The resource recycling of old and useless battery utilizes the difficult problem having become battery industry common concern.
Nickel-cobalt-manganternary ternary anode material is a kind of Olivine-type Cathode Material in Li-ion Batteries, have that capacity is high, Heat stability is good, the advantage such as cheap, compact lithium cell and lithium-ion-power cell can be widely used in, it is a kind of product being in close proximity to cobalt acid lithium, its cost performance is far above the sour lithium of cobalt, Capacity Ratio cobalt acid lithium is high by 10 ~ 20%, it is one of novel battery material most possibly replacing cobalt acid lithium, be called as third generation anode material for lithium-ion batteries, the domestic annual requirement of its positive electrode replaces cobalt acid lithium gradually with the annual growth rate of 20%.At present, the production of ternary anode material precursor adopts nickelous sulfate crystallization, cobaltous sulfate crystallization etc. to be primary raw material, and production cost is high.
By the nickel cobalt element that obtains of process refuse battery, production ternary anode material precursor can be used for.This had both been conducive to resource regeneration and environmental friendliness development, can reduce again the production cost of ternary anode material precursor.Process the process of nickel cobalt refuse material at present both at home and abroad, usual employing Metallurgic Chemical Process, its typical technological process has: first nickel cobalt refuse material passes through acidleach, nickel and cobalt containing is dissolved in acid solution at interior non-ferrous metal, by metallurgical purification means, its metallic element outside nickel cobalt is removed again, obtain the solution that nickel-to-cobalt ratio is purer.Finally adopt the metallurgical technology means of oxidationreduction, obtain the high nickel slag of comparision contents or cobalt slag respectively, then do further process.But Metallurgic Chemical Process complex process, extraction cost are high, very uneconomical, therefore also lack now the effective ways obtaining ternary anode material precursor by reclaiming refuse battery.
Summary of the invention
The object of this invention is to provide a kind of method effectively utilizing refuse battery to prepare ternary anode material precursor.
For achieving the above object, the present invention by the following technical solutions:
Utilize refuse battery to prepare a method for ternary anode material precursor, the steps include:
(1) split refuse battery, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) roasting refuse battery positive electrode, the organic substance in removing positive electrode;
(3) with the refuse battery positive electrode of sulfuric acid dissolution through roasting, refuse battery positive electrode solution is obtained;
(4) impurity in removing refuse battery positive electrode solution is separated by the method for extraction, obtain cobalt sulfate solution and nickel sulfate solution, then in nickel sulfate solution, cobaltous sulfate is added, and manganese supplement element or aluminium element, be made into the mixed liquor of production ternary anode material precursor;
(5) stir gained mixed liquor under normal temperature, add ammoniacal liquor simultaneously, then heat mixed liquor, add sodium hydroxide solution simultaneously, reaction generates ternary anode material precursor precipitation;
(6) ternary anode material precursor washing of precipitate, drying are obtained ternary anode material precursor.
Further, described refuse battery is one or more of used Li ion cell, waste Ni-Cd battery and waste nickel-hydrogen battery.
Further, described ternary anode material precursor is nickel cobalt aluminium presoma or nickel cobalt manganese presoma.
Further, the temperature of described step (2) roasting is 800 ~ 1000 DEG C.
Further, the concentration of described step (3) sulfuric acid is 4 ~ 8mol/L.
Further, in the refuse battery positive electrode solution of described step (3), the total content of nickel and cobalt reaches 3 ~ 4N.
Further, the refuse battery positive electrode solution oxidation-precipitation method removing iron tramp wherein described step (3) obtained, makes iron content≤10ppm.
Further, the extraction of described step (4) comprises the following steps:
1) with manganese, copper, calcium, the zinc impurity in P204 extraction removing refuse battery positive electrode solution, Fe content≤5ppm in solution is made, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
2) be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
3) by N290 extraction removing step 2) magnesium addition in nickel sulfate solution, make content of magnesium≤5ppm in nickel sulfate solution.
Further, described step (4) manganese supplement element is with manganese salt form manganese supplement element, such as manganese sulfate, and supplementary aluminium element refers to and supplements aluminium element, such as aluminum sulfate with aluminium salt form.
Further, the concentration of the ammoniacal liquor that described step (5) uses is 4.0 ~ 6.0mol/L, and the content adding ammonia in rear mixed liquor is 1.0mol/L.
Further, the temperature that described step (5) heats is 40 ~ 70 DEG C, and the concentration of the NaOH of use is 7.0 ~ 10.0mol/L, makes the pH value of mixed liquor be 11.0 ~ 12.5.
Oxidation-precipitation method deironing utilizes contact action, accelerates at a low price Fe forms speed and make it the method removed, being made up of aeration, oxidation reaction and filtration three step.The pH value of water is very large to ferrous oxidation reaction rate, removes part CO by aeration aerating
2, pH can bring up to more than 7.0, is conducive to ferrous oxidation reaction and ferric flocculation sediment, is then removed after filtration; By filtrate absorption deironing and catalytic oxidation, and the irony filter membrane with catalytic activity is progressively generated at filter material surface, irony active filter film plays again the effect of deironing further, catalytic oxidation deironing make use of the catalytic action of irony active filter film, thus greatly accelerate ferrous oxidation rate, more effectively except the iron in anhydrating.
P204 extraction is a kind of method for the preliminary removal of impurities of cobalt nickel, can remove a small amount of iron aluminium chromium calcium, a large amount of zinc-manganese and part copper.P204 is a kind of acidic phosphorus extractant, and the process of its extracting metals ion belongs to base exchange process.The order that P204 extracts each metal ion species is in an acidic solution: Fe
3+>Zn
2+>Cu
2+>Fe
2+>Mn
2+>Co
2+>Ni
2+>Mg
2+>ca
2+, control suitable acidity condition, can Fe be made
3+, Zn
2+, Cu
2+, Mn
2+, Ca
2+enter organic phase Deng impurity, thus realize removal of impurities.For maintaining the pH of extraction process, need before extraction first by P204 NaOH saponification.Extraction is carried out at 20 DEG C, and aqueous phase solution pH value controls about 3, and the volume ratio of organic phase and aqueous phase is the volume fraction of 1:1, P204 extractant is 15%.
P507 extraction is a kind of method be separated for cobalt nickel deep impurity-removing and cobalt nickel, and may be used for demagging.P507 is a kind of acidic organophosphorus extractant, has good extraction ability to some metal ion.The extraction order of P507 to each metal ion species is: Fe
3+>Zn
2+>Cu
2+, Mn
2+, Ca
2+>Co
2+>Mg
2+>Ni
2+, effective separation of nickel, cobalt therefore can be realized under certain pH value.For maintaining the pH of extraction process, need first by P507 NaOH saponification before extraction, saponification rate is 65%.With P507 extract and separate nickel cobalt, its volume fraction is generally 25%, and the volume ratio of organic phase and aqueous phase is 1:1, controls solution ph at about 4, Co
2+have higher extraction efficiency, major part enters organic phase, and Ni
2+extraction efficiency very low, the overwhelming majority is stayed in aqueous phase.Like this, by 3 ~ 5 extractions, substantially only containing Ni in aqueous phase
2+and not containing Co
2+, thus reach the object of nickel cobalt ions separation.Finally, in organic phase, add hydrochloric acid strip, Co
2+can be got back in aqueous phase by reextraction.
N290 extraction is a kind of method for demagging.N290 is a kind of acidic organophosphorus extractant, and the selectivity of separating nickel magnesium is far longer than P507, is 4 at balance pH, in organic phase, N290 volume fraction is 20%, when the volume ratio of organic phase and aqueous phase is 1:1, by 3 to 5 grades of extractions, in nickel sulfate solution, the content of magnesium can be reduced to below 5ppm.
The invention has the beneficial effects as follows:
1 present invention achieves recycling of the resource such as nickel, cobalt in refuse battery, improves resource utilization, avoids heavy metal and cause environmental pollution;
The added value of product that 2 the present invention obtain is high, nickel cobalt aluminium presoma and nickel cobalt manganese presoma are the quality materials producing anode, produce nickel cobalt aluminium presoma and nickel cobalt manganese presoma less to the demand of primary ore resource, the purchase cost of nickel cobalt can be reduced by reclaiming refuse battery;
3 recovery process flow processs of the present invention are simple, realize being separated of nickel and cobalt by other metal impurities in extracting process removing nickel and cobalt solution, do not need to adopt nickelous sulfate and cobaltous sulfate concentration and crystallization process, also avoid by metallurgical purification method removing impurity element, greatly reduce production cost, very the mass production method of suitability for industrialized;
4 the present invention do not produce secondary pollution, are conducive to protection of the environment and sustainable development utilizing refuse battery to prepare in the process of ternary anode material precursor;
The selectivity of 5 N290 extraction separating nickel magnesium of the present invention, far above conventional method, can make the content of magnesium in nickel sulfate solution be reduced to below 5ppm.
Embodiment
P204 extraction in following examples, P507 extraction, all to carry out according to relevant the describing of summary of the invention with N290 extraction, repeat no more.
embodiment 1
Refuse battery is utilized to prepare ternary anode material precursor according to following steps:
(1) split waste nickel-hydrogen battery, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) at 900 DEG C of roasting refuse battery positive electrodes, the organic substance in removing positive electrode;
(3) the refuse battery positive electrode of sulfuric acid dissolution through roasting of 4mol/L is used, obtain refuse battery positive electrode solution, this solution is based on nickelous sulfate, cobaltous sulfate, containing other metal impurities, the total content of nickel and cobalt reaches 3.5N, with the iron tramp in oxidation-precipitation method removing solution, make iron content≤10ppm;
(4) with manganese, copper, calcium, the zinc impurity in P204 extraction removing refuse battery positive electrode solution, Fe content≤5ppm in solution is made, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
(5) be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
(6) magnesium addition in the nickel sulfate solution after being separated with cobaltous sulfate with the removing of N290 extraction is above-mentioned, makes content of magnesium≤5ppm in nickel sulfate solution;
(7) in nickel sulfate solution, add cobalt sulfate solution, and add manganese sulfate, manganese supplement element, be made into the mixed liquor producing nickel cobalt manganese presoma;
(8) gained mixed liquor is stirred under normal temperature, add concentration is 5.0mol/L ammoniacal liquor simultaneously, the content adding ammonia in rear mixed liquor is 1.0mol/L, then mixed liquor to 50 DEG C is heated, add the sodium hydroxide solution that concentration is 8.0mol/L simultaneously, make the pH value of mixed liquor be 12, reaction generates ternary anode material precursor precipitation;
(9) ternary anode material precursor washing of precipitate, drying are obtained tertiary cathode material nickel cobalt manganese presoma.
embodiment 2
Refuse battery is utilized to prepare ternary anode material precursor according to following steps:
(1) split used Li ion cell, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) at 800 DEG C of roasting refuse battery positive electrodes, the organic substance in removing positive electrode;
(3) the refuse battery positive electrode of sulfuric acid dissolution through roasting of 6mol/L is used, obtain refuse battery positive electrode solution, this solution is based on nickelous sulfate, cobaltous sulfate, containing other metal impurities, the total content of nickel and cobalt reaches 3N, with the iron tramp in oxidation-precipitation method removing solution, make iron content≤10ppm;
(4) with manganese, copper, calcium, the zinc impurity in P204 extraction removing refuse battery positive electrode solution, Fe content≤5ppm in solution is made, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
(5) be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
(6) magnesium addition in the nickel sulfate solution after being separated with cobaltous sulfate with the removing of N290 extraction is above-mentioned, makes content of magnesium≤5ppm in nickel sulfate solution;
(7) in nickel sulfate solution, add cobalt sulfate solution, add aluminum sulfate, supplement aluminium element, be made into the mixed liquor producing nickel cobalt aluminium presoma;
(8) gained mixed liquor is stirred under normal temperature, add concentration is 4.0mol/L ammoniacal liquor simultaneously, the content adding ammonia in rear mixed liquor is 1.0mol/L, then mixed liquor to 40 DEG C is heated, add the sodium hydroxide solution that concentration is 7.0mol/L simultaneously, make the pH value of mixed liquor be 11.0, reaction generates ternary anode material precursor precipitation;
(9) ternary anode material precursor washing of precipitate, drying are obtained tertiary cathode material nickel cobalt aluminium presoma.
embodiment 3
Refuse battery is utilized to prepare ternary anode material precursor according to following steps:
(1) split waste Ni-Cd battery and used Li ion cell, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) at 1000 DEG C of roasting refuse battery positive electrodes, the organic substance in removing positive electrode;
(3) the refuse battery positive electrode of sulfuric acid dissolution through roasting of 8mol/L is used, obtain refuse battery positive electrode solution, this solution is based on nickelous sulfate, cobaltous sulfate, containing other metal impurities, the total content of nickel and cobalt reaches 4N, with the iron tramp in oxidation-precipitation method removing solution, make iron content≤10ppm;
(4) with manganese, copper, calcium, the zinc impurity in P204 extraction removing refuse battery positive electrode solution, Fe content≤5ppm in solution is made, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
(5) be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
(6) magnesium addition in the nickel sulfate solution after being separated with cobaltous sulfate with the removing of N290 extraction is above-mentioned, makes content of magnesium≤5ppm in nickel sulfate solution;
(7) in nickel sulfate solution, add cobalt sulfate solution, add manganese sulfate, manganese supplement element, be made into the mixed liquor producing nickel cobalt manganese presoma;
(8) gained mixed liquor is stirred under normal temperature, add concentration is 6.0mol/L ammoniacal liquor simultaneously, the content adding ammonia in rear mixed liquor is 1.0mol/L, then mixed liquor to 70 DEG C is heated, add the sodium hydroxide solution that concentration is 10.0mol/L simultaneously, make the pH value of mixed liquor be 12.5, reaction generates ternary anode material precursor precipitation;
(9) ternary anode material precursor washing of precipitate, drying are obtained tertiary cathode material nickel cobalt manganese presoma.
embodiment 4
Refuse battery is utilized to prepare ternary anode material precursor according to following steps:
(1) split used Li ion cell, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) at 900 DEG C of roasting refuse battery positive electrodes, the organic substance in removing positive electrode;
(3) the refuse battery positive electrode of sulfuric acid dissolution through roasting of 6mol/L is used, obtain refuse battery positive electrode solution, this solution is based on nickelous sulfate, cobaltous sulfate, containing other metal impurities, the total content of nickel and cobalt reaches 3.5N, with the iron tramp in oxidation-precipitation method removing solution, make iron content≤10ppm;
(4) with manganese, copper, calcium, the zinc impurity in P204 extraction removing refuse battery positive electrode solution, Fe content≤5ppm in solution is made, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
(5) be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
(6) magnesium addition in the nickel sulfate solution after being separated with cobaltous sulfate with the removing of N290 extraction is above-mentioned, makes content of magnesium≤5ppm in nickel sulfate solution;
(7) in nickel sulfate solution, add cobalt sulfate solution, add aluminum sulfate, supplement aluminium element, be made into the mixed liquor producing nickel cobalt aluminium presoma;
(8) gained mixed liquor is stirred under normal temperature, add concentration is 5.0mol/L ammoniacal liquor simultaneously, the content adding ammonia in rear mixed liquor is 1.0mol/L, then mixed liquor to 40 DEG C is heated, add the sodium hydroxide solution that concentration is 8.0mol/L simultaneously, make the pH value of mixed liquor be 12.0, reaction generates ternary anode material precursor precipitation;
(9) ternary anode material precursor washing of precipitate, drying are obtained tertiary cathode material nickel cobalt aluminium presoma.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly belongs to those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (10)
1. utilize refuse battery to prepare a method for ternary anode material precursor, it is characterized in that, the steps include:
(1) split refuse battery, remove packing material and battery cathode, obtain refuse battery positive electrode;
(2) roasting refuse battery positive electrode, the organic substance in removing positive electrode;
(3) with the refuse battery positive electrode of sulfuric acid dissolution through roasting, refuse battery positive electrode solution is obtained;
(4) impurity in removing refuse battery positive electrode solution is separated by the method for extraction, obtain cobalt sulfate solution and nickel sulfate solution, then in nickel sulfate solution, cobaltous sulfate is added, and manganese supplement element or aluminium element, be made into the mixed liquor of production ternary anode material precursor;
(5) stir gained mixed liquor under normal temperature, add ammoniacal liquor, then heat mixed liquor, and add sodium hydroxide solution, reaction generates ternary anode material precursor precipitation;
(6) ternary anode material precursor washing of precipitate, drying are obtained ternary anode material precursor.
2. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, described refuse battery is one or more of used Li ion cell, waste Ni-Cd battery and waste nickel-hydrogen battery.
3. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, described ternary anode material precursor is nickel cobalt aluminium presoma or nickel cobalt manganese presoma.
4. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, the temperature of described step (2) roasting is 800 ~ 1000 DEG C.
5. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, in the refuse battery positive electrode solution of described step (3), the total content of nickel and cobalt reaches 3 ~ 4N.
6. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, the refuse battery positive electrode solution oxidation-precipitation method removing iron tramp wherein described step (3) obtained, makes iron content≤10ppm.
7. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, the extraction of described step (4) comprises the following steps:
With manganese, copper, calcium, zinc impurity in P204 extraction removing refuse battery positive electrode solution, make Fe content≤5ppm in solution, copper content≤1ppm, calcium content≤5ppm, Zn content≤5ppm;
Be separated nickelous sulfate and cobaltous sulfate with P507 extraction, obtain nickel sulfate solution and cobalt sulfate solution respectively, make content of magnesium≤10ppm in cobalt sulfate solution;
By N290 extraction removing step 2) magnesium addition in nickel sulfate solution, make content of magnesium≤5ppm in nickel sulfate solution.
8. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, described step (4) manganese supplement element or aluminium element refer to supplementary manganese sulfate or aluminum sulfate.
9. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, is characterized in that, the concentration of the ammoniacal liquor that described step (5) uses is 4.0 ~ 6.0mol/L, and the content adding ammonia in rear mixed liquor is 1.0mol/L.
10. the method utilizing refuse battery to prepare ternary anode material precursor according to claim 1, it is characterized in that, the temperature that described step (5) heats is 40 ~ 70 DEG C, and the concentration of the NaOH of use is 7.0 ~ 10.0mol/L, makes the pH value of mixed liquor be 11.0 ~ 12.5.
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| CN105118990A (en) * | 2015-07-08 | 2015-12-02 | 陕西理工学院 | Technology for preparing nickel-cobalt-aluminum electrode material through recovering nickel from manganese-cobalt-nickel slag |
| CN106450370A (en) * | 2016-11-24 | 2017-02-22 | 张灿 | Dry battery recycling method |
| CN106654205A (en) * | 2016-12-19 | 2017-05-10 | 天齐锂业股份有限公司 | Method for preparing ternary cathode material precursor by using waste lithium battery material |
| CN106785173A (en) * | 2017-02-16 | 2017-05-31 | 盐城工学院 | One kind regeneration tertiary cathode material and preparation method thereof |
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| CN105118990A (en) * | 2015-07-08 | 2015-12-02 | 陕西理工学院 | Technology for preparing nickel-cobalt-aluminum electrode material through recovering nickel from manganese-cobalt-nickel slag |
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