CN108767351A - A kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery - Google Patents
A kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery Download PDFInfo
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- CN108767351A CN108767351A CN201810353291.0A CN201810353291A CN108767351A CN 108767351 A CN108767351 A CN 108767351A CN 201810353291 A CN201810353291 A CN 201810353291A CN 108767351 A CN108767351 A CN 108767351A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery, the method is that will obtain positive electrode after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；The mixed solution of lithium, nickel, cobalt, manganese is obtained after leaching positive active material jointly using citric acid and carbohydrate；Citric acid content in the ratio of each ion and mixed liquor is adjusted in mixed solution, and adjusts after pH value of solution heating water bath to forming gel；High-temperature calcination obtains nickel-cobalt-manganese ternary anode material of lithium battery presoma after gel is dried in vacuo.The advantage of the invention is that：Compared with the prior art, using citric acid and carbohydrate as leaching agent, secondary pollution is not will produce in leaching process, it is more environmentally-friendly, and leach advantage of lower cost.Effects of ion ratio is adjusted using citrate or acetate, any other ion will not be introduced in processing procedure, after high-temperature calcination, factory's use can be directly returned without foreign ion substantially in the persursor material of preparation.
Description
Technical field
The present invention relates to nickel-cobalt-manganternary ternary anode material regeneration methods, belong to old and useless battery recovery technology field.
Background technology
It is excellent that nickel-cobalt-manganese ternary lithium ion battery is high with its operating voltage, specific capacity is high, has extended cycle life, has a safety feature etc.
Point is widely used in the numerous areas such as digital product, aerospace, new-energy automobile.Nickel-cobalt-manganese ternary lithium ion battery is just
Pole material is LiNi1-x-yCoxMnyO2The mixture of active material, conductive agent and adhesive is applied in aluminum foil current collector, wherein
The metallic elements recovery value such as cobalt, nickel, lithium is quite high.
At present it has been reported that nickel-cobalt-manganternary ternary anode material regeneration method be usually put to waste lithium cell
Anode is obtained after electricity, dismantling, sorting, then by obtaining the mixed solution of cobalt, manganese, nickel, lithium after pre-processing and restoring acidleach, finally
Nickel-cobalt-manganternary ternary anode material is regenerated using solid-phase synthesis, coprecipitation, hydro-thermal method, sol-gal process.Such as patent publication No.
A kind of nickel-cobalt-manganternary ternary anode material regeneration based on solid-phase synthesis is proposed for the Chinese patent literature of CN104538695A
Method.This method does not remove the elements such as the iron, copper, potassium that may be mingled in positive electrode, and solid-phase synthesis can not be by nickel
Cobalt manganic acid lithium is sufficiently mixed with carbonate.For another example patent publication No. is that the Chinese patent literature of CN103606651 proposes one kind
The use of citric acid is leaching agent, the method for being used in combination Sol-Hydrothermal coupled method to prepare nickel-cobalt lithium manganate cathode material again.This method
Complex process adjusts ion ratio using sulfate, may introduce impurity during hydrothermal reaction coupling, influence regrown material
Chemical property.
Therefore, it is necessary to provide a kind of simple for process, at low cost, environmental-friendly, and it can ensure the freshly prepd material of weight
The regeneration method of the preferable nickel-cobalt-manganternary ternary anode material of chemical property.
Invention content
It is an object of the invention to overcome the shortcomings of above-mentioned technology, a kind of more economical, more environmentally-friendly, technique is provided more
Add a kind of simple regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery.
A kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery, innovative point are：The method uses
Citric acid and recuding sugars make leaching agent, adjust ion ratio and citric acid content using acetate or citrate, colloidal sol is solidifying
Glue method prepares nickel-cobalt-manganternary ternary anode material again, and foreign ion is not introduced in regenerative process.
Further, the method specifically includes following steps：
Step 1：Positive electrode will be obtained after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；
Step 2：Positive electrode material mixture and aluminium foil are obtained after positive electrode is ultrasonically treated；
Step 3：Positive-active mixture is leached using citric acid and carbohydrate, the mixing of lithium, nickel, cobalt, manganese is obtained after filtering
Solution and insoluble matter；
Step 4：The metal ion ratio in mixed solution is adjusted, the ratio of each ion in mixed solution is adjusted and is mixed
Citric acid content in liquid is closed, pH value of solution is adjusted, heating water bath is to forming gel；
Step 5：High-temperature calcination obtains nickel-cobalt-manganese ternary anode material of lithium battery presoma after gel is dried in vacuo.
Further, carbohydrate is lactose, sucrose, maltose, fructose, glucose, at least one of galactolipin in step 3,
Concentration of saccharide is 0.1~1wt.%, and citric acid concentration is 0.1~2.5mol/L, and extraction temperature is 50~90 DEG C, and mixing speed is
0~600rpm, solid-to-liquid ratio are 10~50g/L, and extraction time is 30~180min；Preferably, concentration of saccharide be 0.6~
0.8wt.%, citric acid concentration are 1~2mol/L, and extraction temperature is 80~90 DEG C.
Further, in step 4 adjust metal ion ratio lithium salts be at least one of lithium acetate and lithium citrate,
Nickel salt is at least one of nickel acetate and citric acid nickel, and cobalt salt is at least one of cobalt acetate and citric acid cobalt, and manganese salt is acetic acid
At least one of manganese and manganese citrate, lithium in mixed solution, nickel, cobalt, manganese molar ratio be 1: 0.5: 0.2: 0.3, pH be 6~
10, bath temperature is 70~90 DEG C；Preferably, pH is 6.5~8.5, and bath temperature is 75~85 DEG C.
Further, in step 5 vacuum drying temperature be 80~120 DEG C, drying time be 12~for 24 hours, calcined temperature
It it is 300~400 DEG C, calcination temperature is 800~950 DEG C, and calcination time is 8~16h；Preferably, drying temperature is 85~95 DEG C,
Calcination temperature is 850~900 DEG C, and calcination time is 12~14h.
The present invention proposes a kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery, with prior art phase
Than having the following advantages that：
Compared with the prior art, the present invention uses citric acid and carbohydrate as leaching agent, not will produce two in leaching process
Secondary pollution, it is more environmentally-friendly, and leach advantage of lower cost.Effects of ion ratio is adjusted using citrate or acetate,
Any other ion will not be introduced in processing procedure, after high-temperature calcination, in the persursor material of preparation substantially without impurity from
Son can directly return factory's use.
Description of the drawings
Fig. 1 is the process flow chart of the regenerating waste used nickel cobalt manganese anode material of the present invention.
Fig. 2 is the XRD spectrum of nickel-cobalt-manganternary ternary anode material made from the embodiment of the present invention 1.
Specific implementation mode
In order to better understand the present invention, the present invention is further described With reference to embodiment.
Embodiment 1：Positive electrode will be obtained after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；By positive electrode
At 200Hz, positive electrode material mixture and aluminium foil are obtained after being ultrasonically treated 0.5h；Positive-active is leached using citric acid and lactose
Mixture, concentration of saccharide 0.1wt.%, citric acid concentration 0.1mol/L, extraction temperature are 50 DEG C, and mixing speed is
100rpm, solid-to-liquid ratio 10g/L, extraction time 30min obtain the mixed solution and insoluble matter of lithium, nickel, cobalt, manganese after filtering；
Molar ratio using cobalt acetate, manganese acetate, nickel acetate, lithium acetate adjusting lithium, nickel, cobalt, manganese is 1: 0.5: 0.2: 0.3, is used
Ammonium hydroxide adjust pH be 6,70 DEG C at water-bath until formed gel；Gel is put in vacuum drying chamber at 80 DEG C dry 12h to obtain
Xerogel obtains nickel-cobalt-manganternary ternary anode material using ball milling after tube furnace high-temperature calcination xerogel, wherein calcined temperature is
300 DEG C, calcination temperature is 800 DEG C, calcination time 8h.Fig. 2 is the XRD spectra of the nickel-cobalt-manganternary ternary anode material prepared, right
Than nickle cobalt lithium manganate standard spectrogram, characteristic peak is almost the same, thus illustrates that prepared product is nickel-cobalt-manganternary ternary anode material.
Embodiment 2：Positive electrode will be obtained after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；By positive electrode
At 200Hz, positive electrode material mixture and aluminium foil are obtained after being ultrasonically treated 0.5h；Positive-active is leached using citric acid and fructose
Mixture, concentration of saccharide 0.5wt.%, citric acid concentration 1mol/L, extraction temperature are 70 DEG C, mixing speed 300rpm,
Solid-to-liquid ratio is 30g/L, extraction time 60min, and the mixed solution and insoluble matter of lithium, nickel, cobalt, manganese are obtained after filtering；Use lemon
Lemon acid cobalt, manganese citrate, citric acid nickel, lithium citrate adjust lithium, nickel, cobalt, manganese molar ratio be 1: 0.5: 0.2: 0.3, make
With ammonium hydroxide adjust pH be 8,80 DEG C at water-bath until formed gel；Gel is put in vacuum drying chamber at 100 DEG C dry 18h to obtain
To xerogel, nickel-cobalt-manganternary ternary anode material is obtained using ball milling after tube furnace high-temperature calcination xerogel, wherein calcined temperature is
350 DEG C, calcination temperature is 850 DEG C, calcination time 10h.
Embodiment 3：Positive electrode will be obtained after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；By positive electrode
At 200Hz, positive electrode material mixture and aluminium foil are obtained after being ultrasonically treated 0.5h；Positive-active is leached using citric acid and fructose
Mixture, concentration of saccharide 1wt.%, citric acid concentration 2.5mol/L, extraction temperature are 90 DEG C, mixing speed 600rpm,
Solid-to-liquid ratio is 50g/L, extraction time 180min, and the mixed solution and insoluble matter of lithium, nickel, cobalt, manganese are obtained after filtering；Use lemon
Lemon acid cobalt, manganese acetate, citric acid nickel, lithium acetate adjust lithium, nickel, cobalt, manganese molar ratio be 1: 0.5: 0.2: 0.3, use ammonia
Water adjust pH be 10,90 DEG C at water-bath until formed gel；Gel is put in vacuum drying chamber drying at 120 DEG C to obtain for 24 hours
Xerogel obtains nickel-cobalt-manganternary ternary anode material using ball milling after tube furnace high-temperature calcination xerogel, wherein calcined temperature is
400 DEG C, calcination temperature is 950 DEG C, calcination time 16h.
Claims (7)
1. a kind of regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery, positive electrode is nickle cobalt lithium manganate, feature
It is to include the following steps：
Step 1：Positive plate will be obtained after the electric discharge of waste and old nickel-cobalt-manganese ternary lithium battery, dismantling, sorting；
Step 2：Positive electrode material mixture and aluminium foil are obtained after positive plate is ultrasonically treated；
Step 3：Positive-active mixture is leached using organic acid and carbohydrate, the mixed solution of lithium, nickel, cobalt, manganese is obtained after filtering
And insoluble matter；
Step 4：The metal ion ratio in mixed solution is adjusted, the ratio and mixed liquor of each ion in mixed solution are adjusted
Middle organic acid content, adjusts pH value of solution, and heating water bath is to forming gel；
Step 5：High-temperature calcination obtains nickel-cobalt-manganese ternary anode material of lithium battery presoma after gel is dried in vacuo.
2. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 1, it is characterised in that：Step
Carbohydrate is lactose, sucrose, maltose, fructose, glucose, at least one of galactolipin in rapid three, concentration of saccharide is 0.1~
1wt.%, organic acid concentration are 0.1~2.5mol/L, and extraction temperature is 50~90 DEG C, and mixing speed is 0~600rpm, solid-liquid
Than for 10~50g/L, extraction time is 30~180min, organic acid is lactic acid, citric acid, one kind in malic acid or tartaric acid
Or it is two or more.
3. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 2, it is characterised in that：Sugar
A concentration of 0.6~0.8wt.% of class, citric acid concentration are 1~2mol/L, and extraction temperature is 80~90 DEG C.
4. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 1, it is characterised in that：Step
The lithium salts that metal ion ratio is adjusted in rapid four is at least one of lithium acetate and lithium citrate, and nickel salt is nickel acetate and citric acid
At least one of nickel, cobalt salt are at least one of cobalt acetate and citric acid cobalt, and manganese salt is at least one in manganese acetate and manganese citrate
Kind, lithium in mixed solution, nickel, cobalt, manganese molar ratio be 1: 0.5: 0.2: 0.3, pH be 6~10, bath temperature is 70~90
℃。
5. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 4, it is characterised in that：pH
It is 6.5~8.5, bath temperature is 75~85 DEG C.
6. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 1, it is characterised in that：Step
In rapid five vacuum drying temperature be 80~120 DEG C, drying time be 12~for 24 hours, calcined temperature be 300~400 DEG C, calcining temperature
Degree is 800~950 DEG C, and calcination time is 8~16h.
7. the regeneration method of waste and old nickel-cobalt-manganese ternary anode material of lithium battery according to claim 6, it is characterised in that：It is dry
Dry temperature is 85~95 DEG C, and calcination temperature is 850~900 DEG C, and calcination time is 12~14h.
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Cited By (8)
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|---|---|---|---|---|
| CN110061319A (en) * | 2018-12-31 | 2019-07-26 | 圣戈莱（北京）科技有限公司 | A kind of reclaiming method of waste and old power lithium-ion battery tertiary cathode material |
| CN110240207A (en) * | 2019-06-17 | 2019-09-17 | 昆明理工大学 | A kind of method that waste lithium cell recycling prepares tertiary cathode material |
| CN111180822A (en) * | 2020-02-05 | 2020-05-19 | 中国科学院化学研究所 | Recycling method of nickel-cobalt-manganese waste ternary lithium battery positive electrode material |
| CN113921928A (en) * | 2021-10-09 | 2022-01-11 | 张火锐 | Method for recycling heavy metal in waste lithium battery anode material |
| CN114497788A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Method for recovering metal from waste battery and preparing metal into positive electrode material |
| CN115716660A (en) * | 2022-10-14 | 2023-02-28 | 东南大学 | Composite ternary metal oxide oxygen carrier material and preparation method and application thereof |
| CN116425213A (en) * | 2020-05-08 | 2023-07-14 | 江苏载驰科技股份有限公司 | Method for recycling valuable metals of waste lithium ion batteries and regenerating ternary positive electrode materials |
| CN116864850A (en) * | 2023-08-21 | 2023-10-10 | 中国矿业大学 | Method for regenerating ternary positive electrode material from waste ternary lithium ion battery leaching liquid |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110061319A (en) * | 2018-12-31 | 2019-07-26 | 圣戈莱（北京）科技有限公司 | A kind of reclaiming method of waste and old power lithium-ion battery tertiary cathode material |
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| CN110240207A (en) * | 2019-06-17 | 2019-09-17 | 昆明理工大学 | A kind of method that waste lithium cell recycling prepares tertiary cathode material |
| CN111180822A (en) * | 2020-02-05 | 2020-05-19 | 中国科学院化学研究所 | Recycling method of nickel-cobalt-manganese waste ternary lithium battery positive electrode material |
| CN111180822B (en) * | 2020-02-05 | 2021-06-22 | 中国科学院化学研究所 | Recycling method of nickel-cobalt-manganese waste ternary lithium battery positive electrode material |
| CN116425213A (en) * | 2020-05-08 | 2023-07-14 | 江苏载驰科技股份有限公司 | Method for recycling valuable metals of waste lithium ion batteries and regenerating ternary positive electrode materials |
| CN114497788A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Method for recovering metal from waste battery and preparing metal into positive electrode material |
| CN113921928A (en) * | 2021-10-09 | 2022-01-11 | 张火锐 | Method for recycling heavy metal in waste lithium battery anode material |
| CN113921928B (en) * | 2021-10-09 | 2023-06-20 | 张火锐 | Method for recycling heavy metal in waste lithium battery anode material |
| CN115716660A (en) * | 2022-10-14 | 2023-02-28 | 东南大学 | Composite ternary metal oxide oxygen carrier material and preparation method and application thereof |
| CN116864850A (en) * | 2023-08-21 | 2023-10-10 | 中国矿业大学 | Method for regenerating ternary positive electrode material from waste ternary lithium ion battery leaching liquid |
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Application publication date: 20181106 |