CN109468463A - The recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery - Google Patents
The recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery Download PDFInfo
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- CN109468463A CN109468463A CN201811400329.1A CN201811400329A CN109468463A CN 109468463 A CN109468463 A CN 109468463A CN 201811400329 A CN201811400329 A CN 201811400329A CN 109468463 A CN109468463 A CN 109468463A
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- lithium battery
- dynamic lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The present invention relates to a kind of recovery methods of cobalt nickel metal in useless dynamic lithium battery comprising following steps: useless dynamic lithium battery a, being carried out discharge treatment；B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；C, cell positive material is put into the first container and is ground, and be put into microwave oven；D, after by microwave heating stove heating, held for some time, there are solid residues in second container；E, certain aqueous is added into the second container there are solid residue, obtains the first solution；F, after the first solution being carried out suction filtration processing by suction filtration machine, the second solution is obtained；G, cleaner is added into the second solution and carries out removal of impurities processing, obtain third solution；H, extractant is added into third solution and carries out extraction processing.The present invention can obtain the cobalt of high-purity, nickel product, to realize the recycling to cobalt nickel metal in useless dynamic lithium battery, improve resource utilization.
Description
Technical field
The present invention relates to battery recycling processing technology field, the recycling of cobalt nickel metal in especially a kind of useless dynamic lithium battery
Method.
Background technique
The power resources of electric car are mainly dynamic lithium battery, and the service life of dynamic lithium battery is generally 5 years, the service life
Once to will do it replacement.Include cell positive material in dynamic lithium battery after scrapping, includes cobalt in cell positive material
Nickel metal, cobalt nickel metal belong to useful metal.Currently, dynamic lithium battery is usually handled by the way that solidification is buried after scrapping,
Processing has certain influence to environment and human body in this way, and causes the serious wasting of resources, and resource utilization is low.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to return to cobalt nickel metal in useless dynamic lithium battery
Receiving method improves resource utilization.
The present invention solves the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery used by its technical problem, including
Following steps:
A, useless dynamic lithium battery is subjected to discharge treatment；
B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；
C, cell positive material obtained in step b is put into the first container and is ground, obtain positive electrode powder,
Positive electrode powder and sodium bisulfate powder are put into togerther in second container, and second container is put into microwave oven；
D, after by microwave heating stove heating, held for some time, then room temperature is cooled the temperature to, and second container is taken
Out, there are solid residues in second container；
E, certain aqueous is added into the second container there are solid residue and is stirred, obtains the first solution；
F, after the first solution being carried out suction filtration processing by suction filtration machine, the second solution is obtained；
G, cleaner is added into the second solution and carries out removal of impurities processing, obtain third solution；
H, extractant is added into third solution and carries out extraction processing.
Further, useless dynamic lithium battery impregnates electric discharge in sodium chloride solution, sodium chloride solution in step a
Concentration is between 0.1-1mol/L.
Further, the material of second container is glass.
Further, the mass ratio of positive electrode powder and sodium bisulfate powder is 1 in second container in step c:
Between 2-1:3.
Further, the heating frequency of microwave oven is 2405-2505MHz, and microwave oven adds in step d
The hot time is less than 15min, and microwave oven temperature after heating is between 600-650 DEG C, and microwave oven soaking time is in 45-
Between 60min, internal pressure is not more than 0.2Mpa when microwave oven is kept the temperature.
Further, the gas excluded to microwave oven is collected, and the gas of collection is led in step d
Enter in the sodium hydroxide solution of 1mol/L.
Further, between 70-90 DEG C, the liquid-solid ratio for obtaining the first solution is the temperature of aqueous in step e
20mL/g。
Further, suction filtration machine is vacuum filtration machine in step f.
Further, in step g, cleaner is P204 extractant, and the volume ratio of cleaner and the second solution is 1:
3。
Further, P507 extractant is added first into third solution in step h, third solution and P507 extract
The volume ratio for taking agent is 1:4, after a certain period of time, the extractant taking-up on third solution top is put into third container, and past
2mol/L sulfuric acid solution is added in third container；Remaining third solution is the 4th solution, is then added into the 4th solution
The volume ratio of P204 extractant, the 4th solution and P204 extractant is 1:4, after a certain period of time, by the extraction on the 4th solution top
Agent taking-up is put into the 4th container, and 2mol/L sulfuric acid solution is added into the 4th container.
The beneficial effects of the present invention are: the present invention obtains anode material first by after useless power lithium battery tank discharge, dismantling
Material, then cell positive material is ground to obtain positive electrode powder, positive electrode powder in microwave oven with sulfuric acid
Hydrogen sodium powder body is reacted, and solid residue is obtained, and solid residue is mainly the soluble sulphate mixture of the nickel containing cobalt, most
After being dissolved by the soluble sulphate mixture of the obtained nickel containing cobalt afterwards, clean, extract, the cobalt of high-purity is obtained, nickel produces
Product improve resource utilization to realize the recycling to cobalt nickel metal in useless dynamic lithium battery.Moreover, recycling of the invention
That there are process flows is short for method, rapidly and efficiently, acid consumption it is low will not generate spent acid, the advantages that disposal of pollutants is few, be conducive to promote.
Specific embodiment
The recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery of the present invention, which comprises the steps of:
A, useless dynamic lithium battery is subjected to discharge treatment；
B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；
C, cell positive material obtained in step b is put into the first container and is ground, obtain positive electrode powder,
Positive electrode powder and sodium bisulfate powder are put into togerther in second container, and second container is put into microwave oven；
D, after by microwave heating stove heating, held for some time, then room temperature is cooled the temperature to, and second container is taken
Out, there are solid residues in second container；
E, certain aqueous is added into the second container there are solid residue and is stirred, obtains the first solution；
F, after the first solution being carried out suction filtration processing by suction filtration machine, the second solution is obtained；
G, cleaner is added into the second solution and carries out removal of impurities processing, obtain third solution；
H, extractant is added into third solution and carries out extraction processing.
Specifically, useless dynamic lithium battery impregnates electric discharge preferably in sodium chloride solution, sodium chloride solution in step a
Concentration is between 0.1-1mol/L, discharge time 2-4h.
In stepb, by detection, obtained cell positive material includes waste cell melt, PVDF binder etc., and PVDF is viscous
Knot agent is called Kynoar binder.
In step c, in order to enable positive electrode powder to react completely with sodium bisulfate powder, cobalt nickel metal is improved
The rate of recovery, the mass ratio of positive electrode powder and sodium bisulfate powder is between 1:2-1:3 in second container.For the ease of passing
Heat, the material of second container are preferably glass.
In step d, by obtaining in largely practicing and testing, the heating frequency of microwave oven is 2405-
2505MHz, microwave oven heating time are less than 15min, and microwave oven temperature after heating is between 600-650 DEG C, microwave
Heating furnace soaking time is between 45-60min, and internal pressure is not more than 0.2Mpa when microwave oven is kept the temperature.Microwave oven
When heat preservation, PVDF binder (Kynoar binder) is decomposed into CO2, HF and carbon dust, cell positive material and sodium bisulfate
Powder is reacted between 600-650 DEG C, obtains the soluble sulphate mixture of the nickel containing cobalt, that is to say will be in waste cell melt
Cobalt nickel metal is converted into the sulfate mixture of the nickel containing cobalt.The gaseous contamination environment of micro-wave oven discharge in order to prevent, to microwave plus
The gas that hot stove excludes is collected, and the gas of collection is passed through in the sodium hydroxide solution of 1mol/L and is handled.
In step e, certain aqueous is added in the soluble sulphate mixture of carbon dust and the nickel containing cobalt and is diluted, is obtained
To the first solution, the temperature of aqueous is between 70-90 DEG C, mixing speed 150r/min, mixing time 0.5h, the first solution
Liquid-solid ratio be 20mL/g.
In step f, suction filtration machine is vacuum filtration machine, and the second solution is the clear aqueous solution containing cobalt, nickel.
In step g, cleaner is P204 extract liquor, and P204 extract liquor is called bis- (2- ethylhexyl) phosphates, is cleaned
The volume ratio or mass ratio of agent and the second solution are 1:3.Utilize the original of high-dissolvability of the Fe plasma in P204 extract liquor
Reason is removed the impurity such as Fe ion by way of abstraction impurity removal.
In step h, P507 extractant is added first into third solution, P507 extractant is called 2- ethylhexyl phosphine
The volume ratio of sour single 2-ethyl hexyl ester, third solution and P507 extractant is 1:4, after a certain period of time, by third solution top
Extractant taking-up be put into third container, and into third container addition 2mol/L sulfuric acid solution, to obtain high concentration
Cobalt sulfate solution, that is to say the principle of the high-dissolvability using Co2+ in P507 extract liquor, by P507 extractant and
Sulfuric acid solution is extracted the cobalt of third solution by way of extracting and being stripped；Remaining third solution is the 4th molten
Liquid, is then added P204 extractant into the 4th solution, and the volume ratio of the 4th solution and P204 extractant is 1:4, certain time
Afterwards, the extractant taking-up on the 4th solution top is put into the 4th container, and addition 2mol/L sulfuric acid is molten into the 4th container
Liquid that is to say the principle of the high-dissolvability using Ni2+ in P204 extract liquor to obtain the nickel sulfate solution of high concentration, lead to
P204 extractant and sulfuric acid solution is crossed to extract the nickel of third solution by way of extracting and being stripped.
In conclusion the present invention obtains cell positive material, then will be electric first by after useless power lithium battery tank discharge, dismantling
Pond positive electrode is ground to obtain positive electrode powder, positive electrode powder in microwave oven with sodium bisulfate powder into
Row reaction, obtains solid residue, solid residue is mainly the soluble sulphate mixture of the nickel containing cobalt, will finally obtain
After the soluble sulphate mixture of the nickel containing cobalt is dissolved, cleaned, extracted, cobalt, the nickel product of high-purity are obtained, to realize
Recycling to cobalt nickel metal in useless dynamic lithium battery, improves resource utilization.Moreover, there are techniques for recovery method of the invention
Process is short, rapidly and efficiently, acid consumption it is low will not generate spent acid, the advantages that disposal of pollutants is few, be conducive to promote.
Embodiment 1
To the recovery method of cobalt nickel metal in 50 useless dynamic lithium batteries of certain brand, include the following steps:
A, useless dynamic lithium battery is impregnated to electric discharge preferably in sodium chloride solution, the concentration of sodium chloride solution is 0.1mol/
L, discharge time 4h；
B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；
C, cell positive material obtained in step b is put into the first container and is ground, obtain positive electrode powder,
Positive electrode powder is carried out to be weighed as 563.1g, positive electrode powder and sodium bisulfate powder are put into togerther second container
In, the mass ratio of positive electrode powder and sodium bisulfate powder is 1:2, and second container is glass container, and second container is put
Enter in microwave oven；
D, after by microwave heating stove heating, held for some time, the heating frequency of microwave oven is 2405MHz, micro-
The Wave heating stove heating time is less than 15min, and microwave oven temperature after heating is between 600 DEG C, microwave oven soaking time
Between 45min, internal pressure is not more than 0.2Mpa when microwave oven is kept the temperature, then cools the temperature to room temperature, and second is held
Device takes out, and there are solid residues in second container；
E, certain aqueous is added into the second container there are solid residue and is stirred, the temperature of aqueous is 70
Between DEG C, mixing speed 150r/min, mixing time 0.5h, the liquid-solid ratio of the first solution are 20mL/g.
F, after the first solution being carried out suction filtration processing by vacuum filtration machine, the second solution is obtained；
G, cleaner is added into the second solution and carries out removal of impurities processing, cleaner is that P204 extract liquor obtains third solution；
H, P507 extractant, the volume ratio or quality of third solution and P507 extractant are added first into third solution
Than the extractant taking-up on third solution top being put into third container, and into third container after a certain period of time for 1:4
2mol/L sulfuric acid solution is added, to obtain the cobalt sulfate solution of high concentration；Remaining third solution is the 4th solution, then
P204 extractant is added into the 4th solution, the volume ratio or mass ratio of the 4th solution and P204 extractant are 1:4, a timing
Between after, the taking-up of the extractant on the 4th solution top is put into the 4th container, and the addition 2mol/L sulfuric acid into 4th container
Solution, to obtain the nickel sulfate solution of high concentration.
It after being evaporated to cobalt sulfate solution and nickel sulfate solution and weighs, obtains cobaltous sulfate 482.4g, nickel sulfate 121.7g.
Embodiment 2
To the recovery method of cobalt nickel metal in 50 useless dynamic lithium batteries of another brand, include the following steps:
A, useless dynamic lithium battery is impregnated to electric discharge preferably in sodium chloride solution, the concentration of sodium chloride solution is 1mol/L,
Discharge time is 2h；
B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；
C, cell positive material obtained in step b is put into the first container and is ground, obtain positive electrode powder,
Positive electrode powder is carried out to be weighed as 786.6g, positive electrode powder and sodium bisulfate powder are put into togerther second container
In, the mass ratio of positive electrode powder and sodium bisulfate powder is 1:3, and second container is glass container, and second container is put
Enter in microwave oven；
D, after by microwave heating stove heating, held for some time, the heating frequency of microwave oven is 2505MHz, micro-
The Wave heating stove heating time is less than 15min, and microwave oven temperature after heating is between 650 DEG C, microwave oven soaking time
Between 60min, internal pressure is not more than 0.2Mpa when microwave oven is kept the temperature, then cools the temperature to room temperature, and second is held
Device takes out, and there are solid residues in second container；
E, certain aqueous is added into the second container there are solid residue and is stirred, the temperature of aqueous is 90
Between DEG C, mixing speed 150r/min, mixing time 0.5h, the liquid-solid ratio of the first solution are 20mL/g.
F, after the first solution being carried out suction filtration processing by vacuum filtration machine, the second solution is obtained；
G, cleaner is added into the second solution and carries out removal of impurities processing, cleaner is that P204 extract liquor obtains third solution；
H, P507 extractant, the volume ratio or quality of third solution and P507 extractant are added first into third solution
Than the extractant taking-up on third solution top being put into third container, and into third container after a certain period of time for 1:4
2mol/L sulfuric acid solution is added, to obtain the cobalt sulfate solution of high concentration；Remaining third solution is the 4th solution, then
P204 extractant is added into the 4th solution, the volume ratio or mass ratio of the 4th solution and P204 extractant are 1:4, a timing
Between after, the taking-up of the extractant on the 4th solution top is put into the 4th container, and the addition 2mol/L sulfuric acid into 4th container
Solution, to obtain the nickel sulfate solution of high concentration.
It after being evaporated to cobalt sulfate solution and nickel sulfate solution and weighs, obtains cobaltous sulfate 621.3g, nickel sulfate 1163.4g.
Claims (10)
1. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery, which comprises the steps of:
A, useless dynamic lithium battery is subjected to discharge treatment；
B, the useless dynamic lithium battery Jing Guo discharge treatment is disassembled, obtains cell positive material；
C, cell positive material obtained in step b is put into the first container and is ground, obtain positive electrode powder, it will just
Pole material powder and sodium bisulfate powder are put into togerther in second container, and second container is put into microwave oven；
D, after by microwave heating stove heating, held for some time, then room temperature is cooled the temperature to, and second container is taken out, the
There are solid residues in two containers；
E, certain aqueous is added into the second container there are solid residue and is stirred, obtains the first solution；
F, after the first solution being carried out suction filtration processing by suction filtration machine, the second solution is obtained；
G, cleaner is added into the second solution and carries out removal of impurities processing, obtain third solution；
H, extractant is added into third solution and carries out extraction processing.
2. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In a, useless dynamic lithium battery impregnates electric discharge in sodium chloride solution, and the concentration of sodium chloride solution is between 0.1-1mol/L.
3. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: second holds
The material of device is glass.
4. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In c, the mass ratio of positive electrode powder and sodium bisulfate powder is between 1:2-1:3 in second container.
5. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In d, the heating frequency of microwave oven is 2405-2505MHz, and microwave oven heating time is less than 15min, microwave oven
Temperature after heating is between 600-650 DEG C, and for microwave oven soaking time between 45-60min, microwave oven is interior when keeping the temperature
Portion's pressure is not more than 0.2Mpa.
6. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In d, the gas excluded to microwave oven is collected, and the gas of collection is passed through in the sodium hydroxide solution of 1mol/L.
7. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In e, for the temperature of aqueous between 70-90 DEG C, the liquid-solid ratio for obtaining the first solution is 20mL/g.
8. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In f, suction filtration machine is vacuum filtration machine.
9. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as described in claim 1, it is characterised in that: in step
In g, cleaner is P204 extractant, and the volume ratio of cleaner and the second solution is 1:3.
10. the recovery method of cobalt nickel metal in a kind of useless dynamic lithium battery as claimed in any one of claims 1 to 9, special
Sign is: in step h, P507 extractant, the volume ratio of third solution and P507 extractant being added first into third solution
The extractant taking-up on third solution top is put into third container, and is added into third container after a certain period of time for 1:4
Enter 2mol/L sulfuric acid solution；Remaining third solution is the 4th solution, then the addition P204 extractant into the 4th solution, the 4th
The volume ratio of solution and P204 extractant is 1:4, after a certain period of time, the extractant taking-up on the 4th solution top is put into the 4th appearance
In device, and 2mol/L sulfuric acid solution is added into the 4th container.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855759A (en) * | 2023-08-31 | 2023-10-10 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538696A (en) * | 2015-01-08 | 2015-04-22 | 兰州理工大学 | Method for recycling metal from waste lithium ion battery with Ni-Co lithium manganite positive electrode materials |
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2018
- 2018-11-22 CN CN201811400329.1A patent/CN109468463A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538696A (en) * | 2015-01-08 | 2015-04-22 | 兰州理工大学 | Method for recycling metal from waste lithium ion battery with Ni-Co lithium manganite positive electrode materials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116855759A (en) * | 2023-08-31 | 2023-10-10 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
| CN116855759B (en) * | 2023-08-31 | 2023-11-17 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
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Application publication date: 20190315 |