CN109888423A - A kind of recovery method for scrapping ternary lithium battery - Google Patents
A kind of recovery method for scrapping ternary lithium battery Download PDFInfo
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- CN109888423A CN109888423A CN201910139092.4A CN201910139092A CN109888423A CN 109888423 A CN109888423 A CN 109888423A CN 201910139092 A CN201910139092 A CN 201910139092A CN 109888423 A CN109888423 A CN 109888423A
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- lithium battery
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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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
Abstract
A kind of recovery method for scrapping ternary lithium battery disclosed by the invention, comprising the following steps: 1. pairs are scrapped the dismantling of ternary lithium battery into lithium battery monomer, and carry out discharge treatment；2. pair lithium battery monomer carries out break process；3. carrying out supercritical carbon dioxide extracting processing to battery crushing slurry in extractor；4. one side carries out reduced pressure treatment to extraction mobile phase；On the other hand sorting process is carried out to residual solid mixture；5. the solution mixed by sulfuric acid and hydrogen peroxide is added to metal solid mixture；6. a pair acid solidliquid mixture is filtered processing；7. adjusting the pH value of acidic mixed solution to 7~7.5, and filters and recycled；8. adjusting the pH value of the mixed solution containing ternary metal ingredient to 11~14, and filters and recycled；9. enough sodium carbonate liquors are added to the solution containing a small amount of lithium salts, and filter and recycled.The present invention recycles electrolyte with solution morphology, and the rate of recovery is up to 90% or more.
Description
Technical field
The present invention relates to power batteries to be recycled technical field, in particular to a kind of recycling side for scrapping ternary lithium battery
Method.
Background technique
Currently, the recovery process for scrapping ternary lithium battery mainly includes discharge step, pulverising step, calcination steps, physics
The step of sorting step and hydrometallurgy recycle Ni, Co, Mn, Li et al. metallic element, the broken recovery process can not separate back
Receive electrolyte, subsequent obtained sorting product contains electrolyte decomposition products, such as fluoride, containing phosphide etc., influence wet type
The rate of recovery of metallurgy recycling.Electrolyte is recycled usually using extraction process, is also had at present using solution and/or overcritical two
Carbonoxide carries out extraction and recovery, but is individually extracted after decomposing the collector in lithium battery, and extraction efficiency is special
It is low, it is difficult to realize industrialization operation.For this purpose, the applicant has carried out beneficial exploration and research, has found and solve the above problems
Method, technical solution described below generates in this background.
Summary of the invention
Technical problem to be solved by the present invention lies in: one kind is provided in view of the deficiencies of the prior art and scraps ternary lithium electricity
The recovery method in pond, the recovery method can reduce the technique before extraction, and the lithium battery electrolytes ingredient recycling of real-time industrial mentions
The rate of recovery of high subsequent wet metallurgical technology, reduces the consumption of soda acid.
The technical problems to be solved by the invention can adopt the following technical scheme that realize:
A kind of recovery method for scrapping ternary lithium battery, comprising the following steps:
Step S1 is put to the dismantling of ternary lithium battery is scrapped at lithium battery monomer, and to the lithium battery monomer after dismantling
Electric treatment；
Step S2, in the state of being protected using inert gas as protection gas, to the lithium after discharge treatment
Battery cell carries out break process, so that lithium battery monomer forms battery crushing slurry after being broken；
The battery crushing slurry is delivered in extractor, to the battery crushing in the extractor by step S3
Slurry carries out supercritical carbon dioxide extracting processing, and obtains extraction mobile phase and residual solid mixture；
On the one hand step S4 carries out reduced pressure treatment to the extraction mobile phase, so that extraction flowing is separated into two
Carbon oxide gas and electrolyte, and the electrolyte after separation is recycled；On the other hand pneumatic separating mode pair is used
The residual solid mixture carries out sorting process so that the residual solid mixture be sorted into plastic diaphragms material and by
Metal solid mixture composed by metal material, electrode material and a small amount of lithium salts, and to the plastic diaphragms material after sorting
It is recycled；
The solution mixed by sulfuric acid and hydrogen peroxide is added in step S5, Xiang Suoshu metal solid mixture, to the gold
Belong to solid mixture to be dissolved, forms acid solidliquid mixture；
Step S6 is filtered processing to the acid solidliquid mixture, so that after the acidity solidliquid mixture filtering
It is separated into acidic mixed solution and graphite cathode powder, and recycling and reusing is carried out to the graphite cathode powder；
Step S7 slowly adjusts the pH value of the acidic mixed solution using sodium hydroxide solution to 7~7.5, so that institute
It states the copper in acidic mixed solution, iron, aluminium to precipitate in the form of hydroxide, and is obtained by filtration by Kocide SD, iron hydroxide
And the metal mixture that mixes of aluminium hydroxide and the mixed solution containing ternary metal ingredient, to described by hydroxide
The metal mixture that copper, iron hydroxide and aluminium hydroxide mix carries out recycling and reusing；
Step S8, slowly adjusted using sodium hydroxide solution the pH value of the mixed solution containing ternary metal ingredient to
11~14, until precipitating is completed, and it is obtained by filtration and is mixed by the metal that nickel hydroxide, cobalt hydroxide and manganous hydroxide mix
Object and the solution containing a small amount of lithium salts are closed, to the metal mixed by nickel hydroxide, cobalt hydroxide and manganous hydroxide
Mixture carries out recycling and reusing；
Step S9 is added enough sodium carbonate liquors to the solution containing a small amount of lithium salts, and lithium carbonate is obtained by filtration
And salt bearing liquid wastes, recycling and reusing is carried out to the lithium carbonate.
In a preferred embodiment of the invention, in the step S1, the lithium battery monomer after described pair of dismantling is adopted
Discharge treatment is carried out with salt water immersion, and the lithium battery monomer after discharge treatment is started the cleaning processing, to remove lithium battery list
The soak of body surface face attachment.
In a preferred embodiment of the invention, in the step S2, the inert gas is nitrogen.
In a preferred embodiment of the invention, in the step S4, the extraction mobile phase separates to be formed two
Carbon oxide gas is after overcompression in circulation conveying to the extractor.
In a preferred embodiment of the invention, in the step S5, the mass ratio of the sulfuric acid and hydrogen peroxide is
7:3~9:1.
In a preferred embodiment of the invention, in the step S7, the concentration of the sodium hydroxide solution is
1.5%~10%.
In a preferred embodiment of the invention, in the step S8, the concentration of the sodium hydroxide solution is 3%
~15%.
In a preferred embodiment of the invention, in the step S9, the concentration of the sodium carbonate liquor is 5%~
15%.
Due to using technical solution as above, the beneficial effects of the present invention are:
1, the present invention recycles electrolyte with solution morphology, and the rate of recovery is up to 90% or more；
2, present invention can ensure that the VOCs of exhaust gas reaches discharge standard, environment is avoided pollution；
3, it after the present invention is to residual solid mixture separating plastic diaphragm material extracted, is mentioned, be can be recycled using acidleach
Graphite cathode powdered ingredients；
4, the mixed solution that the present invention obtains after mentioning to acidleach carries out multi stage precipitation, obtains having the ternary of utility value mixed
Condensation material presoma and carbonic acid lithium material.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is process flow chart of the invention.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
Referring to Fig. 1, what is provided in figure is a kind of recovery method for scrapping ternary lithium battery, comprising the following steps:
Step S1 is put to the dismantling of ternary lithium battery is scrapped at lithium battery monomer, and to the lithium battery monomer after dismantling
Electric treatment.In the present embodiment, the lithium battery monomer after dismantling is impregnated using salt water and carries out discharge treatment, and to discharge treatment
Lithium battery monomer afterwards starts the cleaning processing, to remove the soak of lithium battery monomer surface attachment.
Step S2, in the state of being protected using inert gas as protection gas, to the lithium after discharge treatment
Battery cell carries out break process, so that lithium battery monomer forms battery crushing slurry after being broken.In the present embodiment, inertia
Gas is preferably nitrogen.
Battery crushing slurry obtained in step S2 is delivered in extractor by step S3, broken to battery in extractor
Pulping material carries out supercritical carbon dioxide extracting processing, and obtains extraction mobile phase and residual solid mixture.
On the one hand step S4 carries out reduced pressure treatment to extraction mobile phase obtained in step S3, so that extraction mobile phase point
Recycling and reusing, while two that separation is formed are carried out from carbon dioxide gas and electrolyte, and by the electrolyte after separation
Carbon oxide gas is after overcompression in circulation conveying to extractor.On the other hand using pneumatic separating mode to being obtained in step S3
Residual solid mixture carry out sorting process so that residual solid mixture is sorted into plastic diaphragms material and by metal material
Metal solid mixture composed by material, electrode material and a small amount of lithium salts, and the plastic diaphragms material after sorting is returned
Receipts processing.
Step S5, what the metal solid mixture addition sorted into step S4 was mixed by sulfuric acid and hydrogen peroxide
Solution dissolves metal solid mixture, forms acid solidliquid mixture；In the present embodiment, sulfuric acid and double in solution
The mass ratio of oxygen water is 7:3~9:1.
Step S6 is filtered processing to the step S5 acid solidliquid mixture formed, so that acid solidliquid mixture mistake
It is separated into acidic mixed solution and graphite cathode powder after filter, and recycling and reusing is carried out to graphite cathode powder.
It is obtained by filtration in step S7, the slow regulating step S6 of sodium hydroxide solution for being 1.5%~10% using concentration
The pH value of acidic mixed solution is to 7~7.5, so that the copper, iron, aluminium in acidic mixed solution are precipitated in the form of hydroxide,
And be obtained by filtration the metal mixture mixed by Kocide SD, iron hydroxide and aluminium hydroxide and containing ternary metal at
The mixed solution divided, recycles again the metal mixture mixed by Kocide SD, iron hydroxide and aluminium hydroxide
It utilizes, can specifically carry out metallurgical processing to these metal mixtures.
What is be obtained by filtration in step S8, the slow regulating step S7 of sodium hydroxide solution for being 3%~15% using concentration contains
There is the pH value of the mixed solution of ternary metal ingredient to 11~14, until precipitating is completed, and is obtained by filtration by nickel hydroxide, hydrogen-oxygen
Change the metal mixture that cobalt and manganous hydroxide mix and the solution containing a small amount of lithium salts, to by nickel hydroxide, hydroxide
The metal mixture that cobalt and manganous hydroxide mix carries out recycling and reusing, these metal mixtures can be used as regenerating ternary
Material.
Step S9, the solution containing a small amount of lithium salts being obtained by filtration into step S8 be added enough concentration be 5%~
15% sodium carbonate liquor, and lithium carbonate and salt bearing liquid wastes is obtained by filtration, recycling and reusing is carried out to lithium carbonate, it specifically can be by carbon
Sour lithium is for producing battery grade lithium material.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of recovery method for scrapping ternary lithium battery, which comprises the following steps:
Step S1 is carried out at electric discharge to the dismantling of ternary lithium battery is scrapped at lithium battery monomer, and to the lithium battery monomer after dismantling
Reason；
Step S2, in the state of being protected using inert gas as protection gas, to the lithium battery after discharge treatment
Monomer carries out break process, so that lithium battery monomer forms battery crushing slurry after being broken；
The battery crushing slurry is delivered in extractor by step S3, to the battery crushing slurry in the extractor
Supercritical carbon dioxide extracting processing is carried out, and obtains extraction mobile phase and residual solid mixture；
On the one hand step S4 carries out reduced pressure treatment to the extraction mobile phase, so that extraction flowing is separated into titanium dioxide
Carbon gas and electrolyte, and the electrolyte after separation is recycled；On the other hand using pneumatic separating mode to described
Residual solid mixture carries out sorting process, so that the residual solid mixture is sorted into plastic diaphragms material and by metal
Metal solid mixture composed by material, electrode material and a small amount of lithium salts, and the plastic diaphragms material after sorting is carried out
Recovery processing；
The solution mixed by sulfuric acid and hydrogen peroxide is added in step S5, Xiang Suoshu metal solid mixture, solid to the metal
Body mixture is dissolved, and acid solidliquid mixture is formed；
Step S6 is filtered processing to the acid solidliquid mixture, so that separating after the acidity solidliquid mixture filtering
Recycling and reusing is carried out at acidic mixed solution and graphite cathode powder, and to the graphite cathode powder；
Step S7 slowly adjusts the pH value of the acidic mixed solution using sodium hydroxide solution to 7~7.5, so that the acid
Copper, iron, aluminium in property mixed solution are precipitated in the form of hydroxide, and be obtained by filtration by Kocide SD, iron hydroxide and
The metal mixture that aluminium hydroxide mixes and the mixed solution containing ternary metal ingredient, to described by Kocide SD, hydrogen
The metal mixture that iron oxide and aluminium hydroxide mix carries out recycling and reusing；
Step S8, slowly adjusted using sodium hydroxide solution the pH value of the mixed solution containing ternary metal ingredient to 11~
14, until precipitating is completed, and the metal mixture mixed by nickel hydroxide, cobalt hydroxide and manganous hydroxide is obtained by filtration
With contain a small amount of lithium salts solution, to the metal mixed mixed by nickel hydroxide, cobalt hydroxide and manganous hydroxide
Object carries out recycling and reusing；
Step S9 is added enough sodium carbonate liquors to the solution containing a small amount of lithium salts, and lithium carbonate is obtained by filtration and contains
Bisulfate waste liquor carries out recycling and reusing to the lithium carbonate.
2. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S1, institute
It states to impregnate the lithium battery monomer after dismantling using salt water and carries out discharge treatment, and the lithium battery monomer after discharge treatment is carried out
Cleaning treatment, to remove the soak of lithium battery monomer surface attachment.
3. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S2, institute
Stating inert gas is nitrogen.
4. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S4, institute
It states extraction mobile phase and separates the carbon dioxide gas to be formed after overcompression in circulation conveying to the extractor.
5. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S5, institute
The mass ratio for stating sulfuric acid and hydrogen peroxide is 7:3~9:1.
6. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S7, institute
The concentration for stating sodium hydroxide solution is 1.5%~10%.
7. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S8, institute
The concentration for stating sodium hydroxide solution is 3%~15%.
8. scrapping the recovery method of ternary lithium battery as described in claim 1, which is characterized in that in the step S9, institute
The concentration for stating sodium carbonate liquor is 5%~15%.
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| CN110600702A (en) * | 2019-09-18 | 2019-12-20 | 上海应用技术大学 | Composite material for core-shell structure secondary battery using waste diaphragm as raw material, preparation and application thereof |
| CN111092273A (en) * | 2019-09-14 | 2020-05-01 | 湖南金源新材料股份有限公司 | Novel method for comprehensively recovering cobalt, nickel, manganese and lithium elements from ternary battery waste |
| CN111403838A (en) * | 2019-12-23 | 2020-07-10 | 余姚市鑫和电池材料有限公司 | Recycling method of retired power lithium battery diaphragm paper |
| CN111416169A (en) * | 2020-03-11 | 2020-07-14 | 长沙有色冶金设计研究院有限公司 | Device for charged crushing and electrolyte recovery of waste power lithium battery |
| CN111416168A (en) * | 2020-03-11 | 2020-07-14 | 长沙有色冶金设计研究院有限公司 | Method for recycling waste power lithium battery electrolyte |
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