CN109082522A - A kind of recovery method of waste and old ternary lithium battery anode powder - Google Patents
A kind of recovery method of waste and old ternary lithium battery anode powder Download PDFInfo
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- CN109082522A CN109082522A CN201810928779.1A CN201810928779A CN109082522A CN 109082522 A CN109082522 A CN 109082522A CN 201810928779 A CN201810928779 A CN 201810928779A CN 109082522 A CN109082522 A CN 109082522A
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- leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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 present invention relates to a kind of recovery methods of waste and old ternary lithium battery anode powder, comprising the following steps: a high-temperature roasting → lithium leaching → nickel leaching → secondary high-temperature roasting → cobalt leaches；Method of the invention is in a manner of substep high-temperature process, leaching, the preferable lithium of isolated applicability, nickel, cobalt sulfate liquor, realize classification recycling and the innoxious use of waste and old ternary lithium battery anode powder, using carbon black, oxygen, air as reducing agent and oxidant in whole flow process, production cost is low；Through detecting, leaching rate of the leaching rate during 90% or more, leaching nickel in the present invention during leaching lithium is 98% or more, leaching rate during leaching cobalt is 92% or more, the leaching rate of manganese is 0.1% hereinafter, having the advantages that good separating effect, high-efficient, suitable popularization and use in overall process.
Description
Technical field
The present invention relates to ternary technical field of lithium batteries, especially a kind of recycling side of waste and old ternary lithium battery anode powder
Method.
Background technique
Currently, domestic power battery requires to be gradually increased to energy density, with LiNixCoyMnzO2It is the three of positive electrode
First lithium battery accounting is gradually increasing.As the listing of novel electric vehicle and the old and useless battery of arrival service life are retired, recycling
Ternary lithium battery material in market is also constantly rising, and the component ratio in material is changeable, is unfavorable for comprehensive reutilization.
Major metal component in the positive electrode of waste and old ternary lithium battery is nickel, cobalt, manganese, lithium.Wherein manganese element content
Not high, metal values are low, therefore recycling has little significance.The recovery method of the ternary lithium battery anode powder of most domestic at present
In, nickel, cobalt, manganese are recycled together usually, are prepared into ternary precursor.But it is many kinds of due to ternary lithium battery,
Element ratio difference is larger, and the unified purposes for recycling ternary precursor material obtained has biggish limitation, is difficult to meet
The demand of vast battery producer.Therefore, how classification recycling is carried out to the metallic element in the positive mix of ternary lithium battery, is
The project of the previous worth research of mesh, it may have higher practical application value.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of returning for waste and old ternary lithium battery anode powder
Receiving method, isolated pure lithium sulfate, nickel sulfate, cobalt sulfate solution from the positive mix of waste and old ternary lithium battery are real
Now the classification of metallic element each in positive mix is recycled.
To achieve the above object, the invention adopts the following technical scheme:
A kind of recovery method of waste and old ternary lithium battery anode powder, comprising the following steps:
S1, a high-temperature roasting: the positive mix of ternary lithium battery is roasted into 4-6h under air atmosphere, maturing temperature control exists
750 DEG C or more；
S2, lithium leach: after the resulting powder of S1 is cooling, water logging being added to go out, dilute sulfuric acid is added in leaching process and adjusts pH to 7-
8.5, it is separated after the completion of leaching, obtains lithium sulfate solution and filter residue A；
S3, nickel leach: filter residue A being carried out acidleach with dilute sulfuric acid under conditions of being passed through oxygen, pH to 4-5.5 is adjusted, has leached
At rear separation, nickel sulfate solution and filter residue B are obtained；
S4, secondary high-temperature roasting: carbon black is added in filter residue B and is uniformly mixed, 1-2h, maturing temperature control are roasted under protective atmosphere
System is at 600 DEG C or more；
S5, cobalt leach: after S4 gained powder is cooling, carrying out acidleach with dilute sulfuric acid, then adjust pH to 5.2-5.5, and lead to simultaneously
Enter air, keep the temperature and stir sustained response, to separate after the reaction was completed, obtains cobalt sulfate solution and filter residue C.
Further, the extraction temperature of the S2 is 20-25 DEG C, extraction time 3-4h.
Further, the initial concentration of dilute sulfuric acid is 0.5-1mol/L in the S3, and acidleach temperature is 20-25 DEG C, when acidleach
Between be 2-3h, adjust pH use nickel hydroxide or sodium hydroxide.
Further, the initial concentration of dilute sulfuric acid is 1-3mol/L in the S5, and acidleach temperature is 80-95 DEG C, leaching time
For 1.5-3.5h；It adjusts pH and uses sodium hydroxide, soaking time is 1-2h after adjusting pH.
Further, the additional amount of the carbon black is the 5% of the gross mass of filter residue B.
Beneficial effects of the present invention are as follows: the present invention is using the positive mix of waste and old ternary lithium battery as raw material, first in air
A high-temperature roasting under atmosphere, by LiNixCoyMnzO2It is converted into Li2CO3、NiO、Co3O4、Mn2O3、MnO2, then carry out water-soluble
Reaction adds dilute sulfuric acid tune pH to leach, obtains lithium sulfate solution and filter residue A(isolates lithium)；Filter residue A is dissolved with dilute sulfuric acid, is led to
Enter oxygen, tune pH leaches to obtain nickel sulfate solution and filter residue B(isolates nickel)；It is restored under protective atmosphere with carbon black again
Roasting, converts acid-soluble CoO, Co and MnO for cobalt and manganese, is passed through air, dilute sulfuric acid is added and adjusts pH is selected
Property leach, obtain cobalt sulfate solution and filter residue C(isolate cobalt).
Compared with prior art, method of the invention is in a manner of substep high-temperature process, leaching, isolated applicability compared with
Good lithium, nickel, cobalt sulfate liquor, realize classification recycling and the innoxious use of waste and old ternary lithium battery anode powder,
Using carbon black, oxygen, air as reducing agent and oxidant in whole flow process, production cost is low；Through detecting, lithium is leached in the present invention
Leaching rate of leaching rate of the leaching rate in the process during 90% or more, leaching nickel during 98% or more, leaching cobalt
The leaching rate of manganese is 0.1% hereinafter, having the advantages that good separating effect, high-efficient, suitable popularization makes in 92% or more, overall process
With.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
The present invention will be further described With reference to embodiment:
Embodiment 1
To 811 obtained tertiary cathode powders are disassembled after screening is ground, roasting 6h is carried out at 750 DEG C with rotary furnace.
Distilled water is added according to liquid-solid ratio 30L/kg to powder after cooling, is dripped after mixing evenly under room temperature (20-25 DEG C)
Add dilute sulfuric acid, adjust pH=7, is kept stirring and leaches 3h, separate to obtain lithium sulfate solution and filter residue A.
0.8mol/L dilute sulfuric acid is added by liquid-solid ratio 10L/kg to filter residue A, after mixing evenly under conditions of being passed through oxygen,
PH=5.0, which are adjusted, with sodium hydroxide solution separates to obtain nickel sulfate solution and filter residue B under room temperature (20-25 DEG C) after leaching 3h.
Carbon black and ball milling are mixed into filter residue B in 5% ratio of filter residue B gross mass, under nitrogen protection, 650 DEG C of roastings
Burn 1.5h.
2mol/L dilute sulfuric acid is added according to liquid-solid ratio 3L/kg to powder after cooling, is leached at 80 DEG C after mixing evenly
After 3.5h, sodium hydroxide is added and adjusts pH to 5.5, and is passed through air simultaneously, after stirring while keeping pH and temperature 1.5h, separation
Cobalt sulfate solution and filter residue C can be obtained.
Analysis is sampled to filter residue A, B, C, lithium in filtrate, nickel, cobalt practical leaching rate respectively reach 91.0%,
98.9%, the leaching rate of 94.7%, Mn is lower than 0.07%.
Embodiment 2
It to the obtained 111 tertiary cathode powders of dismantling after screening is ground, is roasted with rotary furnace at 800 DEG C, when roasting
Between 4h.
Distilled water is added according to liquid-solid ratio 30L/kg to powder after cooling, dilute sulfuric acid is added dropwise after mixing evenly at room temperature,
PH=8.5 are adjusted, is kept stirring and leaches 4h, separate to obtain lithium sulfate solution and filter residue A.
0.5mol/L dilute sulfuric acid is added by liquid-solid ratio 10L/kg to filter residue A, oxygen and after mixing evenly is passed through, with thin hydrogen-oxygen
Change nickel powder and adjust pH=5.5, keeps after leaching 2h is stirred at room temperature, separate to obtain nickel sulfate solution and filter residue B.
Ball milling after carbon black is mixed into filter residue B in 5% ratio of filter residue B gross mass, under nitrogen protection, 700 DEG C of roastings
Burn 1h.
1mol/L dilute sulfuric acid is added according to liquid-solid ratio 4L/kg to powder after cooling, is leached at 90 DEG C after mixing evenly
After 2h, sodium hydroxide is added and adjusts pH to 5.2, and is passed through air simultaneously, after stirring while keeping pH and temperature 2h, separation can be obtained
Cobalt sulfate solution and filter residue C.
Analysis is sampled to filter residue A, B, C, lithium in filtrate, nickel, cobalt practical leaching rate respectively reach 90.7%,
99.9%, the leaching rate of 96.7%, Mn is lower than 0.11%.
Embodiment 3
It to the obtained 622 tertiary cathode powders of dismantling after screening is ground, is roasted with rotary furnace at 760 DEG C, when roasting
Between 5h.
Distilled water is added according to liquid-solid ratio 30L/kg to powder after cooling, dilute sulfuric acid is added dropwise after mixing evenly at room temperature,
PH=7.7 are adjusted, is kept stirring and leaches 3.5h, separate to obtain lithium sulfate solution and filter residue A.
1mol/L dilute sulfuric acid is added by liquid-solid ratio 10L/kg to filter residue A, oxygen and after mixing evenly is passed through, with sodium hydroxide
Solution adjusts pH=4 and separates to obtain nickel sulfate solution and filter residue B after leaching 2.5h is stirred at room temperature in holding.
Carbon black and ball milling are mixed into filter residue B in 5% ratio of filter residue B gross mass, under nitrogen protection, 600 DEG C of roastings
Burn 2h.
3mol/L dilute sulfuric acid is added according to liquid-solid ratio 4L/kg to powder after cooling, is leached at 95 DEG C after mixing evenly
After 1.5h, sodium hydroxide is added and adjusts pH to 5.3, and is passed through air simultaneously, after stirring while keeping pH and temperature 1.0h, separation
Cobalt sulfate solution and filter residue C can be obtained.
Analysis is sampled to filter residue A, B, C, lithium in filtrate, nickel, cobalt practical leaching rate respectively reach 92.5%,
97.9%, the leaching rate of 93.7%, Mn is lower than 0.09%.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (5)
1. a kind of recovery method of waste and old ternary lithium battery anode powder, which comprises the following steps:
S1, a high-temperature roasting: the positive mix of ternary lithium battery is roasted into 4-6h under air atmosphere, maturing temperature control exists
750 DEG C or more；
S2, lithium leach: after the resulting powder of S1 is cooling, water logging being added to go out, dilute sulfuric acid is added in leaching process and adjusts pH to 7-
8.5, it is separated after the completion of leaching, obtains lithium sulfate solution and filter residue A；
S3, nickel leach: filter residue A being carried out acidleach with dilute sulfuric acid under conditions of being passed through oxygen, pH to 4-5.5 is adjusted, has leached
At rear separation, nickel sulfate solution and filter residue B are obtained；
S4, secondary high-temperature roasting: carbon black is added in filter residue B and is uniformly mixed, 1-2h, maturing temperature control are roasted under protective atmosphere
System is at 600 DEG C or more；
S5, cobalt leach: after S4 gained powder is cooling, carrying out acidleach with dilute sulfuric acid, then adjust pH to 5.2-5.5, and lead to simultaneously
Enter air, keep the temperature and stir sustained response, to separate after the reaction was completed, obtains cobalt sulfate solution and filter residue C.
2. a kind of recovery method of waste and old ternary lithium battery anode powder according to claim 1, which is characterized in that described
The extraction temperature of S2 is 20-25 DEG C, extraction time 3-4h.
3. a kind of recovery method of waste and old ternary lithium battery anode powder according to claim 1, which is characterized in that described
The initial concentration of dilute sulfuric acid is 0.5-1mol/L in S3, and acidleach temperature is 20-25 DEG C, leaching time 2-3h, adjusts pH and uses
Nickel hydroxide or sodium hydroxide.
4. a kind of recovery method of waste and old ternary lithium battery anode powder according to claim 1, which is characterized in that described
The initial concentration of dilute sulfuric acid is 1-3mol/L in S5, and acidleach temperature is 80-95 DEG C, leaching time 1.5-3.5h；Adjusting pH makes
With sodium hydroxide, soaking time is 1-2h after adjusting pH.
5. a kind of recovery method of waste and old ternary lithium battery anode powder according to claim 1, which is characterized in that described
The additional amount of carbon black is the 5% of the gross mass of filter residue B.
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| CN201810928779.1A CN109082522B (en) | 2018-08-15 | 2018-08-15 | Method for recovering anode powder of waste ternary lithium battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110714124A (en) * | 2019-10-16 | 2020-01-21 | 厦门钨业股份有限公司 | Method for extracting cobalt from tungsten waste recovery slag |
| CN110714125A (en) * | 2019-10-16 | 2020-01-21 | 厦门钨业股份有限公司 | Method for extracting cobalt from tungsten waste smelting slag |
| CN111041230A (en) * | 2019-08-16 | 2020-04-21 | 中国科学院过程工程研究所 | Method for recovering metal from waste lithium ion battery |
| CN111039312A (en) * | 2019-12-26 | 2020-04-21 | 甘肃睿思科新材料有限公司 | Treatment method of nickel cobalt lithium manganate positive electrode material |
| CN111979414A (en) * | 2019-05-24 | 2020-11-24 | 杨絮 | Method for rapidly recycling nickel and cobalt elements in ternary battery material with configuration equipment |
| CN112271351A (en) * | 2020-10-26 | 2021-01-26 | 宁波互邦新材料有限公司 | Process for efficiently leaching and recovering ternary cathode material |
| CN113415813A (en) * | 2021-06-22 | 2021-09-21 | 四川长虹格润环保科技股份有限公司 | Method for recovering lithium nickel cobalt manganese from waste ternary battery material |
| CN114085995A (en) * | 2021-11-09 | 2022-02-25 | 湖北亿纬动力有限公司 | Method for preparing metal simple substance and compound thereof by recycling waste lithium ion battery and application thereof |
| CN115838181A (en) * | 2022-12-06 | 2023-03-24 | 楚能新能源股份有限公司 | Method for preparing lithium fluoride and ternary material precursor by using waste electrode powder of ternary lithium battery |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111979414A (en) * | 2019-05-24 | 2020-11-24 | 杨絮 | Method for rapidly recycling nickel and cobalt elements in ternary battery material with configuration equipment |
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| CN110714124A (en) * | 2019-10-16 | 2020-01-21 | 厦门钨业股份有限公司 | Method for extracting cobalt from tungsten waste recovery slag |
| CN110714125A (en) * | 2019-10-16 | 2020-01-21 | 厦门钨业股份有限公司 | Method for extracting cobalt from tungsten waste smelting slag |
| CN111039312A (en) * | 2019-12-26 | 2020-04-21 | 甘肃睿思科新材料有限公司 | Treatment method of nickel cobalt lithium manganate positive electrode material |
| CN112271351A (en) * | 2020-10-26 | 2021-01-26 | 宁波互邦新材料有限公司 | Process for efficiently leaching and recovering ternary cathode material |
| CN113415813A (en) * | 2021-06-22 | 2021-09-21 | 四川长虹格润环保科技股份有限公司 | Method for recovering lithium nickel cobalt manganese from waste ternary battery material |
| CN114085995A (en) * | 2021-11-09 | 2022-02-25 | 湖北亿纬动力有限公司 | Method for preparing metal simple substance and compound thereof by recycling waste lithium ion battery and application thereof |
| CN115838181A (en) * | 2022-12-06 | 2023-03-24 | 楚能新能源股份有限公司 | Method for preparing lithium fluoride and ternary material precursor by using waste electrode powder of ternary lithium battery |
| CN115838181B (en) * | 2022-12-06 | 2024-03-29 | 楚能新能源股份有限公司 | Method for preparing lithium fluoride and ternary material precursor by utilizing ternary lithium battery waste electrode powder |
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| CN109082522B (en) | 2019-12-13 |
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