CN103199230B - A kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation - Google Patents
A kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation Download PDFInfo
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- CN103199230B CN103199230B CN201310089509.3A CN201310089509A CN103199230B CN 103199230 B CN103199230 B CN 103199230B CN 201310089509 A CN201310089509 A CN 201310089509A CN 103199230 B CN103199230 B CN 103199230B
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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
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- 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
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Abstract
The invention discloses a kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, comprise the following steps: the battery anode slice that (1) gets waste and old lithium ion battery carries out pretreatment acquisition positive powder; (2) described positive powder is dissolved in inorganic acid, removal of impurities, obtains the mixed solution that contains nickel and manganese; (3) in described mixed solution, add Huo Meng source, nickel source; (4) add acetate complexing agent, adjust the ratio of acetate concentration and metal ion total concentration; (5) mixed solution is placed in to electrolytic cell and carries out electrolysis, Ni, Mn oxide is deposited on titanium sheet; (6) stop passing into direct current, take out titanium sheet, the Ni, Mn oxide on separating titanium sheet, dry, obtain Ni, Mn oxide powder; (7) Ni, Mn oxide powder mixes with lithium source, then carries out calcination processing, obtains nickel LiMn2O4. This technique can, by waste battery by reverse reclamation technique, obtain the reconstituted product identical with original product performance, realizes recycling.
Description
Technical field
The present invention relates to nickel LiMn2O4 preparation technology, relate in particular to a kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation.
Background technology
Along with the development of digital product industry, people increase day by day to the demand of battery. Nickel LiMn2O4 is a kind of important anode material of lithium battery, produces and uses increasingly extensively, and market demand is larger. When lithium battery is flourish, can predict, in the near future, after battery stops, can enter the stage of scrapping, can calculate that with the quantity of current lithium battery its learies is also huge on an equal basis.
Waste lithium cell positive electrode is nickel LiMn2O4 etc., can reclaim and be utilized, and makes metal powder, metal oxide, chemical industry salt etc. But best mode still reclaims nickel LiMn2O4 by reverse reclamation technique, is prepared into battery material, realizes recycling.
At present, reclaiming the technique of nickel lithium manganate battery material, is generally in the purification of metals liquid of battery material, to add precipitating reagent to make nickel manganese precipitated metal out, is then prepared into nickel manganese presoma through high-temperature calcination, then mixes lithium source and prepare nickel LiMn2O4. The precipitating reagent using can be solids of sedimentation agent, as carbonate; Also can be liquid precipitation agent, as ammoniacal liquor. But the cost compare that feeds intake is high, if ammoniacal liquor is made precipitating reagent, can produce ammonia nitrogen waste water, neither environmental protection, also increases cost for wastewater treatment.
Electrodeposition process is a kind of current method that reclaims metal simple-substance, still, because the deposition potential of nickel, manganese element is larger, easily separates out separately nickel oxide and manganese oxide when electro-deposition apart, and more difficult generation codeposition obtains Ni, Mn oxide; And in reaction system, ratio and the total concentration of nickel, manganese ion concentration is larger on the appearance structure impact of Ni, Mn oxide, therefore not it was reported that at present best nickel, the manganese ion concentration of bright electric deposition nickel Mn oxide.
Summary of the invention
Object of the present invention provides a kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, and this technique can, by waste battery by reverse reclamation technique, obtain the reconstituted product identical with original product performance, realizes recycling.
The object of the invention is to be achieved through the following technical solutions: a kind of technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, comprises the following steps:
(1) battery anode slice of getting waste and old lithium ion battery carries out pretreatment acquisition positive powder;
(2) described positive powder is dissolved in inorganic acid, removal of impurities, obtains the mixed solution that contains nickel and manganese;
(3) in described mixed solution, add Huo Meng source, nickel source, in adjusting mixed solution, the molar concentration rate of nickel and manganese is (0.5-2) ﹕ 1, and metal ion total concentration is 1-5mol/L;
(4) add acetate complexing agent, the ratio of acetate concentration and metal ion total concentration is 1 ~ 2 ﹕ 1;
(5) mixed solution is placed in to electrolytic cell, is heated to 85 ~ 95 DEG C, constant temperature 10 ~ 15min, then taking titanium sheet as negative electrode, graphite rod is anode, passes into constant current direct current, controls current density at 100 ~ 500A/m2, maintain 2 ~ 5h, Ni, Mn oxide is deposited on titanium sheet;
(6) stop passing into direct current, take out titanium sheet, the Ni, Mn oxide on separating titanium sheet, dry, obtain Ni, Mn oxide powder;
(7) Ni, Mn oxide powder mixes with lithium source, then carries out calcination processing, obtains nickel LiMn2O4.
In the present invention, the impact on crystal nucleation speed and size according to the concentration of current density, temperature and solution. Under other condition same cases, adopt high current density, can make crystal nucleation fast, nucleus is many, and size is large, and the oversize chemical property that is unfavorable for nickel LiMn2O4, therefore highest current density is no more than 500A/m2; Adopt low current density, nucleation is slow, and nucleus is few, and size is little, but can reduce production efficiency, therefore minimum current density is not less than 100A/m2. Under other condition same cases, adopt high temperature, can accelerate system reaction speed, but excess Temperature can make water solution system seethe with excitement or closely boil, and makes reaction system unstable, therefore maximum temperature is no more than 95 DEG C; Adopt low temperature, can make stable reaction, be conducive to crystal and evenly grow, structure is consistent, but the too low meeting of temperature production efficiency, therefore minimum temperature is not less than 85 DEG C. Under other condition same cases, adopt highly concentrated solution, can increase product output, but excessive concentration can make crystal growth exceed substrate volume, reunites, and is unfavorable for the chemical property of nickel LiMn2O4, therefore the highest total concentration of metal ion is no more than 5mol/L; Adopt low concentration solution, can ensure crystal growing space, but the too low meeting of concentration makes output lower, waste resource, therefore the highest total concentration of metal ion is not less than 1mol/L.
The pretreatment of step of the present invention (1), is that battery cell is disassembled, and takes out positive plate, then by positive plate fragmentation, pyrolysis, vibrosieve, makes positive powder and other materials physical separation;
The nickel source of step of the present invention (2) is the one in nickel chloride, nickelous sulfate, nickel nitrate, described manganese source is the one in manganese chloride, manganese sulfate, manganese nitrate, described inorganic acid is the one in hydrochloric acid, nitric acid and sulfuric acid, wherein preferably adopt nitric acid, the oxidisability of nitric acid is to dissolve for front end, also be for electro deposition oxidation nickel manganese, can have saved feed intake step and the cost of oxidant.
Step of the present invention (2) removal of impurities is to be purified and only contained the acid solution of nickel, two kinds of metallic elements of manganese by extraction mode.
As an embodiment of the invention, described extraction detailed process is: controlling acid solution pH is 2 ~ 3, the P that to add by volume fraction be 30%204With the extractant that the volume fraction sulfonated kerosene that is 70% forms, the volume ratio of extractant and acid solution is 2 ﹕ 1, and equilibration time is 15 ~ 30min, then uses the back extraction of 2mol/L inorganic acid, and equilibration time is 15 ~ 30min, obtains mixed solution nickeliferous, manganese.
The acetate complexing agent of step of the present invention (4) is sodium acetate or potassium acetate.
It is that Ni, Mn oxide departs from titanium sheet that step of the present invention (6) adopts sonic oscillation, and duration of oscillation is preferably 10 ~ 15min. Described dry employing pressure-filteration drying, carries out press filtration by the Ni, Mn oxide suspension after sonic oscillation, and filter residue is placed in to heating furnace, is heated to 100 DEG C, dry 30min.
The mass ratio in the described Ni, Mn oxide of step of the present invention (7) and lithium source is 3 ~ 5:1. The program of described calcination processing is for to be warming up to 200 DEG C with 2 DEG C/min speed, constant temperature 4h, then be warming up to 500 ~ 600 DEG C, constant temperature 10 ~ 12h.
Described step (7) lithium source is lithium carbonate or lithium hydroxide.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention first synthesizes Ni, Mn oxide by old and useless battery positive electrode, more synthetic new nickel manganate cathode material for lithium, can, by waste battery by reverse reclamation technique, obtain the reconstituted product identical with original product performance, realizes recycling.
(2) in the step of the synthetic Ni, Mn oxide of the present invention, can control by controlling the concentration of current density, temperature and solution speed and the size of crystal growth, be conducive to regulate and control character and the performance of synthetic material.
(3) the present invention is that from solution, electrodeposition is out by Ni, Mn oxide, compared with the traditional precipitation method, save the link of adding solids of sedimentation agent or ammoniacal liquor, save the cost of auxiliary material, and process do not produce ammonia nitrogen waste water pollute, reduced cost for wastewater treatment.
(4) ratio and the total concentration of nickel ion and manganese ion in control reaction system of the present invention, it is the Ni, Mn oxide that homogeneous is spherical that electro-deposition obtains pattern, the synthesizing formula that provides a kind of prior art not have.
(5) the present invention uses acetate for complexing agent, utilize acetate can with the character of nickel, manganese ion complexing, the deposition potential of the nickel that furthers, manganese element, makes nickel, manganese element be easy to occur codeposition, solve nickel, manganese element because of deposition potential apart from each other, separately the problem of deposition.
Brief description of the drawings
Fig. 1 is the SEM figure of the embodiment of the present invention one gained Ni, Mn oxide.
Fig. 2 is the SEM figure of contrast experiment's one gained Ni, Mn oxide.
Fig. 3 is the SEM figure of contrast experiment's two gained Ni, Mn oxides.
Detailed description of the invention
Embodiment mono-:
(1) battery cell is disassembled, taken out positive plate; Positive plate is pulverized, and pyrolysis, adopts 60 object standard screens to sieve under vibration, obtains anodal powder 1846g.
(2) anodal powder is dissolved in 10L nitric acid, insoluble matter removes by filter, and controlling filtrate pH is 2, adds 20L extractant, and the component of extractant is that volume fraction is 30% P204With the sulfonated kerosene that volume fraction is 70%, equilibration time is 15min, then strips with 10L2mol/L nitric acid, equilibration time is 15min, obtain the mixed solution that solution is nickel nitrate and manganese nitrate, recording nickel ion concentration in solution is 0.60mol/L, and manganese ion concentration is 0.63mol/L.
(3) in the mixed solution of step (2), add 54.84g nickel nitrate, making nickel ion and manganese ion concentration ratio is 1 ﹕ 1.
(4) add 1033.2g sodium acetate, the ratio of acetate concentration and metal ion total concentration is 1 ﹕ 1.
(5) pour above-mentioned solution into electrolytic cell, be heated to 85 DEG C, constant temperature 10min. Insert titanium sheet and graphite rod, taking titanium sheet as negative electrode, taking graphite rod as anode, be communicated with galvanostat, pass into constant current direct current, control current density is 100A/m2, maintain 2h, Ni, Mn oxide is deposited on titanium sheet;
(6) stop passing into direct current, take out titanium sheet, be placed in water, sonic oscillation 5min, Ni, Mn oxide departs from titanium sheet, and the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min, obtains Ni, Mn oxide powder 942.22g;
(7) add 242.75g lithium carbonate toward Ni, Mn oxide powder, mix, be placed in calcining furnace, be warming up to 200 DEG C with 2 DEG C/min speed, constant temperature 4h, then be warming up to 500 DEG C, constant temperature 10h, obtains 1120.32g nickel LiMn2O4. The microstructure of Ni, Mn oxide as shown in Figure 1, this Ni, Mn oxide is spherical in shape, and structure is consistent, and particle diameter is even.
Embodiment bis-:
(1) battery cell is disassembled, taken out positive plate; Positive plate is pulverized, and pyrolysis, adopts 60 object standard screens to sieve under vibration, obtains anodal powder 1950g.
(2) anodal powder is dissolved in 10L hydrochloric acid, insoluble matter removes by filter, controlling filtrate pH is 2, adds 20L extractant, and the component of extractant is that volume fraction is the sulfonated kerosene that 30% P204 and volume fraction are 70%, equilibration time is 20min, strip with 10L2mol/L hydrochloric acid, equilibration time is 20min, obtains the mixed solution that solution is nickel chloride and manganese chloride again, recording nickel ion concentration in solution is 1.25mol/L, and manganese ion concentration is 2.2mol/L.
(3) in the mixed solution of step (2), add 390g manganese chloride, making nickel ion and manganese ion concentration ratio is 0.5 ﹕ 1.
(4) add 3075g sodium acetate, the ratio of acetate concentration and metal ion total concentration is 1 ﹕ 1.
(5) pour above-mentioned solution into electrolytic cell, be heated to 90 DEG C, constant temperature 10min. Insert titanium sheet and graphite rod, taking titanium sheet as negative electrode, taking graphite rod as anode, be communicated with galvanostat, pass into constant current direct current, control current density is 200A/m2, maintain 3h, Ni, Mn oxide is deposited on titanium sheet.
(6) stop passing into direct current, take out titanium sheet, be placed in water, sonic oscillation 5min, Ni, Mn oxide departs from titanium sheet, and the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min, obtains Ni, Mn oxide powder 3412.5g.
(7) add 1387.5g lithium carbonate toward Ni, Mn oxide powder, mix, be placed in calcining furnace, be warming up to 200 DEG C with 2 DEG C/min speed, constant temperature 4h, then be warming up to 500 DEG C, constant temperature 10h, obtains 3675g nickel LiMn2O4.
Embodiment tri-:
(1) battery cell is disassembled, taken out positive plate; Positive plate is pulverized, and pyrolysis, adopts 60 object standard screens to sieve under vibration, obtains anodal powder 1872g.
(2) anodal powder is dissolved in 10L sulfuric acid, insoluble matter removes by filter, controlling filtrate pH is 3, adds 20L extractant, and the component of extractant is that volume fraction is the sulfonated kerosene that 30% P204 and volume fraction are 70%, equilibration time is 30min, strip with 10L2mol/L sulfuric acid, equilibration time is 30min, obtains the mixed solution that solution is nickelous sulfate and manganese sulfate again, recording nickel ion concentration in solution is 1.2mol/L, and manganese ion concentration is 1mol/L.
(3) in the mixed solution of step (2), add 1240g nickelous sulfate, making nickel ion and manganese ion concentration ratio is 2 ﹕ 1.
(4) add 2940g sodium acetate, the ratio of acetate concentration and metal ion total concentration is 1 ﹕ 1.
(5) pour above-mentioned solution into electrolytic cell, be heated to 95 DEG C, constant temperature 10min. Insert titanium sheet and graphite rod, taking titanium sheet as negative electrode, taking graphite rod as anode, be communicated with galvanostat, pass into constant current direct current, control current density is 500A/m2, maintain 5h, Ni, Mn oxide is deposited on titanium sheet.
(6) stop passing into direct current, take out titanium sheet, be placed in water, sonic oscillation 5min, Ni, Mn oxide departs from titanium sheet, and the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min, obtains Ni, Mn oxide powder 2730g;
(7) add 1110g lithium carbonate toward Ni, Mn oxide powder, mix, be placed in calcining furnace, be warming up to 200 DEG C with 2 DEG C/min speed, constant temperature 4h, then be warming up to 500 DEG C, constant temperature 10h, obtains 2940g nickel LiMn2O4.
Contrast experiment one:
Formulation components is that nickel nitrate concentration is 0.63mol/L, and manganese nitrate concentration is 0.21mol/L, the solution 10L that sodium acetate concentration is 0.84mol/L, and nickel ion is 3 ﹕ 1 with manganese ion concentration ratio; Pour above-mentioned solution into electrolytic cell, be heated to 85 DEG C, constant temperature 10min; Insert titanium sheet and graphite rod, taking titanium sheet as negative electrode, taking graphite rod as anode, be communicated with galvanostat, pass into constant current direct current, control current density is 100A/m2, maintain 2h, Ni, Mn oxide is deposited on titanium sheet; Stop passing into direct current, take out titanium sheet, be placed in water, sonic oscillation 5min, Ni, Mn oxide departs from titanium sheet, and the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min, obtains Ni, Mn oxide powder. The microstructure of Ni, Mn oxide as shown in Figure 2, the not moulding of this Ni, Mn oxide, shape differs, without fixed dimension.
Contrast experiment two:
Formulation components is that nickel nitrate concentration is 0.21mol/L, and manganese nitrate concentration is 0.63mol/L, the solution 10L that sodium acetate concentration is 0.84mol/L, and nickel ion is 1 ﹕ 3 with manganese ion concentration ratio; Pour above-mentioned solution into electrolytic cell, be heated to 85 DEG C, constant temperature 10min; Insert titanium sheet and graphite rod, taking titanium sheet as negative electrode, taking graphite rod as anode, be communicated with galvanostat, pass into constant current direct current, control current density is 100A/m2, maintain 2h, Ni, Mn oxide is deposited on titanium sheet; Stop passing into direct current, take out titanium sheet, be placed in water, sonic oscillation 5min, Ni, Mn oxide departs from titanium sheet, and the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min, obtains Ni, Mn oxide powder. The microstructure of Ni, Mn oxide as shown in Figure 3, it is irregular spherical that this Ni, Mn oxide is, and reunites mutually, without fixed dimension.
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character. Above-mentioned embodiment of the present invention all can only be thought explanation of the present invention instead of restriction, therefore every foundation essence technology of the present invention is done above embodiment any trickle amendment, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (8)
1. a technique of preparing nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, is characterized in that, comprises the following steps:
(1) battery anode slice of getting waste and old lithium ion battery carries out pretreatment acquisition positive powder;
(2) described positive powder is dissolved in inorganic acid, controlling acid solution pH is 2 ~ 3, the P that to add by volume fraction be 30%204With the extractant that the volume fraction sulfonated kerosene that is 70% forms, the volume ratio of extractant and acid solution is 2 ﹕ 1, and equilibration time is 15 ~ 30min, then uses the back extraction of 2mol/L inorganic acid, and equilibration time is 15 ~ 30min, obtains the mixed solution that contains nickel and manganese;
(3) in described mixed solution, add Huo Meng source, nickel source, in adjusting mixed solution, the molar concentration rate of nickel and manganese is 0.5 ~ 2 ﹕ 1, and metal ion total concentration is 1 ~ 5mol/L;
(4) add acetate complexing agent, the ratio of acetate concentration and metal ion total concentration is 1 ~ 2 ﹕ 1;
(5) mixed solution is placed in to electrolytic cell, is heated to 85 ~ 95 DEG C, constant temperature 10 ~ 15min, then taking titanium sheet as negative electrode, graphite rod is anode, passes into constant current direct current, controls current density at 100 ~ 500A/m2, maintain 2 ~ 5h, Ni, Mn oxide is deposited on titanium sheet;
(6) stop passing into direct current, take out titanium sheet, the Ni, Mn oxide on separating titanium sheet, dry, obtain Ni, Mn oxide powder;
(7) Ni, Mn oxide powder mixes with lithium source, then carries out calcination processing, obtains nickel LiMn2O4.
2. prepare according to claim 1 the technique of nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, the pretreatment of described step (1) is that battery cell is disassembled, take out positive plate, again by positive plate fragmentation, pyrolysis, vibrosieve, makes positive powder and other materials physical separation.
3. prepare according to claim 1 the technique of nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, the nickel source of described step (2) is the one in nickel chloride, nickelous sulfate and nickel nitrate, described manganese source is the one in manganese chloride, manganese sulfate and manganese nitrate, and described inorganic acid is the one in hydrochloric acid, nitric acid and sulfuric acid.
4. according to the technique of preparing nickel LiMn2O4 described in claim 1 or 3 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, the acetate complexing agent of described step (4) is sodium acetate or potassium acetate.
5. the technique of preparing according to claim 4 nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, is characterized in that, it is that Ni, Mn oxide departs from titanium sheet that described step (6) adopts sonic oscillation, and duration of oscillation is preferably 10 ~ 15min; Described dry employing pressure-filteration drying.
6. prepare according to claim 5 the technique of nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, described pressure-filteration drying is that the Ni, Mn oxide suspension after sonic oscillation is carried out to press filtration, and filter residue is placed in to heating furnace, be heated to 100 DEG C, dry 30min.
7. prepare according to claim 1 the technique of nickel LiMn2O4 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, the mass ratio in the described Ni, Mn oxide of described step (7) and lithium source is 3 ~ 5:1, the program of described calcination processing is for to be warming up to 200 DEG C with 2 DEG C/min speed, constant temperature 4h, be warming up to again 500 ~ 600 DEG C, constant temperature 10 ~ 12h.
8. according to the technique of preparing nickel LiMn2O4 described in claim 1 or 7 taking waste lithium cell as raw material reverse reclamation, it is characterized in that, described step (7) lithium source is lithium carbonate or lithium hydroxide.
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| CN103400965B (en) * | 2013-07-24 | 2015-05-13 | 广东邦普循环科技有限公司 | Process for reserve recycling and preparation of lithium nickel cobaltate from waste lithium battery as raw material |
| CN103633392B (en) * | 2013-12-04 | 2015-10-07 | 广东邦普循环科技有限公司 | A kind of method being prepared nickel manganese hydroxide by waste and old electrokinetic cell directed circulation |
| CN104600284B (en) * | 2015-01-15 | 2017-01-11 | 兰州理工大学 | Method for regenerating positive active material in spent lithium manganate lithium ion battery |
| CN106785174B (en) * | 2017-02-24 | 2020-04-21 | 中南大学 | Method for leaching and recovering metal from lithium ion battery anode waste based on electrochemical method |
| CN106916955A (en) * | 2017-03-31 | 2017-07-04 | 广东佳纳能源科技有限公司 | A kind of method of valuable metal in selective recovery lithium ion cell anode waste |
| CN107968198B (en) * | 2017-11-24 | 2021-03-12 | 中国科学院过程工程研究所 | Nickel-cobalt lithium manganate precursor with core-shell structure, preparation method thereof and application of precursor in lithium ion battery |
| CN108306071A (en) * | 2018-01-16 | 2018-07-20 | 深圳市比克电池有限公司 | A kind of waste lithium ion cell anode material recovery technique |
| CN108565419A (en) * | 2018-03-30 | 2018-09-21 | 华南师范大学 | A kind of regenerative lithium ion anode material and preparation method thereof |
| CN109755539A (en) * | 2019-02-21 | 2019-05-14 | 湖南邦普循环科技有限公司 | Utilize the method for lithium ion cell anode waste production aluminium doping ternary precursor |
| CN110247129B (en) * | 2019-06-14 | 2021-11-30 | 广西师范大学 | Method for recycling positive active substances of waste lithium ion batteries |
| CN112582601A (en) * | 2020-12-14 | 2021-03-30 | 中钢集团南京新材料研究院有限公司 | Method for preparing lithium nickel manganese oxide by utilizing waste lithium manganese oxide and lithium nickel manganese oxide |
| CN114759285B (en) * | 2022-04-11 | 2024-06-04 | 中南大学 | Treatment method of waste lithium ion battery leaching liquid |
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