CN106654433A - Method for recovering lithium by adopting waste lithium iron phosphate batteries - Google Patents
Method for recovering lithium by adopting waste lithium iron phosphate batteries Download PDFInfo
- Publication number
- CN106654433A CN106654433A CN201611018662.7A CN201611018662A CN106654433A CN 106654433 A CN106654433 A CN 106654433A CN 201611018662 A CN201611018662 A CN 201611018662A CN 106654433 A CN106654433 A CN 106654433A
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- CN
- China
- Prior art keywords
- lithium
- iron phosphate
- lithium iron
- waste lithium
- positive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 30
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 title claims abstract description 23
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 10
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940005991 chloric acid Drugs 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 230000011218 segmentation Effects 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000012298 atmosphere Substances 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000002386 leaching Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 3
- 238000005520 cutting process Methods 0.000 abstract 2
- 208000028659 discharge Diseases 0.000 abstract 1
- 238000010907 mechanical stirring Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
-
- 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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Secondary Cells (AREA)
- Primary Cells (AREA)
Abstract
The invention discloses a method for recovering lithium by using waste lithium iron phosphate batteries, which comprises the steps of firstly, carrying out safe discharge treatment on the waste lithium iron phosphate batteries, cutting the batteries along the top by using a cold cutting method, disassembling and removing shells to obtain battery roll cores, calcining the battery roll cores at 600-900 ℃ in the atmosphere of protective gas, crushing and sieving to obtain mixed materials of positive and negative electrodes; adding sodium hydroxide solution into the mixed material of the positive electrode and the negative electrode, alternately carrying out ultrasonic stirring and mechanical stirring for 4-8 minutes, and filtering to obtain filter mud; adding chloric acid into the filter mud, wherein the reaction temperature is 70-85 ℃, and the solid-liquid ratio is 1/4-1/8; leaching lithium solution, filtering to obtain leachate, adjusting the pH value of the leachate by adopting potassium hydroxide, filtering, and adding sodium carbonate into the filtrate to obtain lithium carbonate precipitate. The method has the advantages of simple process, high recovery efficiency and high recovery purity, can quickly and efficiently recover lithium in the waste lithium iron phosphate batteries, and is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to battery recycling technical field, and in particular to a kind of employing waste lithium iron phosphate battery reclaims the side of lithium
Method.
Background technology
As over the years necessarily becoming for replacement orthodox car is gradually paid attention to, promoted and become to new-energy automobile
Gesture, also has been enter into increasing the phase rapidly as the yield of the dynamic lithium battery of new-energy automobile " heart ".Expect 2012, newly
The annual production of energy automobile is up to 1,000,000, will drive the demand of 5.2 ten thousand tons of anode material of lithium battery.In view of lithium electricity
The restricted lifetime in pond, these new-energy automobile lithium batteries will progress into the superseded date of retirement after several years, the lithium in its positive electrode
If the great wasting of resources will be caused by arbitrarily discarding.
LiFePO4 (the LiFePO of olivine shape structure4) battery because with good heat endurance and cycle performance into
For the main force of dynamic lithium battery.Lithium iron phosphate positive material composition is complicated, containing substantial amounts of copper and aluminium simple substance and a small amount of iron
The impurity such as simple substance.The presence of impurity iron, copper and aluminium gives back to receipts lithium and brings difficulty.In traditional direct alkaline leaching, impurity iron, copper
Leached jointly in a large number with the leaching that aluminium is usually associated with lithium, therefore remain a need for being separated these impurity with lithium.And use
The method high cost of extract and separate these impurity, and environmental pollution is big, is unfavorable for industrial operation.
The content of the invention
It is an object of the invention to provide a kind of method that employing waste lithium iron phosphate battery reclaims lithium, process is simple, reclaim
Efficiency high, reclaims the lithium that purity is high, in recovery waste lithium iron phosphate battery that can be rapidly and efficiently, it is adaptable to which large-scale industry is given birth to
Produce.
The invention discloses a kind of method that employing waste lithium iron phosphate battery reclaims lithium, first by waste lithium iron phosphate electricity
Pond is carried out after safe-discharge process, along top open is cut battery using cold cut segmentation method, is disassembled to shell and is obtained battery roll core, will
Battery roll core 600-900 DEG C of calcining in a nitrogen atmosphere, grinding and sieving obtains both positive and negative polarity batch mixing;Add in both positive and negative polarity batch mixing
Enter for sodium hydroxide solution, after ultrasound and mechanical agitation alternately 4-8 minutes, filter to obtain filter mud;Chloric acid will be added in filter mud,
Reaction temperature is 70-85 DEG C, and solid-to-liquid ratio is 1/4-1/8;Lithium solution is leached, is filtered, obtain leachate, adjusted using potassium hydroxide
Leachate pH, filters, and to filtrate sodium carbonate is added, and obtains lithium carbonate precipitation.
Preferably, under nitrogen atmosphere calcination time is 3-5h.
Any of the above-described scheme is preferably, and the battery roll core crosses 80-120 mesh sieves after crushing, and obtains both positive and negative polarity batch mixing.
Any of the above-described scheme is preferably, and the concentration of the chloric acid is 3-5mol/L.
Any of the above-described scheme is preferably, and leachate is adjusted to pH 6.5-7.5 using potassium hydroxide, precipitates a small amount of iron, mistake
Filter to obtain filtrate.
Beneficial effects of the present invention are as follows:
Present invention process is simple, and organic efficiency is high, purity height is reclaimed, in recovery waste lithium iron phosphate battery that can be rapidly and efficiently
Lithium, it is adaptable to large-scale industrial production.
Specific embodiment
Following embodiments are further illustrating using as the explaination to the technology of the present invention content for present invention, but
The present invention flesh and blood be not limited in described in following embodiments, one of ordinary skill in the art can with and should know appoint
What simple change or replacement based on true spirit all should belong to protection domain of the presently claimed invention.
Embodiment 1:
The present invention provides a kind of method that employing waste lithium iron phosphate battery reclaims lithium, first carries out waste lithium iron phosphate battery
After safe-discharge process, battery is cut open along top using cold cut segmentation method, disassemble to shell and obtain battery roll core, by battery winding
Core 600 DEG C of calcinings under the atmosphere of protective gas nitrogen, the mesh sieve of grinding and sieving 80 obtains both positive and negative polarity batch mixing;To both positive and negative polarity
Sodium hydroxide solution is incorporated as in batch mixing, ultrasound and mechanical agitation filter to obtain filter mud after alternately 5 minutes;To add in filter mud
Enter chloric acid, reaction temperature is 70 DEG C, and solid-to-liquid ratio is 1/4;Lithium solution is leached, is filtered, obtain leachate, adjusted using potassium hydroxide and soaked
Go out liquid to pH 6.5, precipitate a small amount of iron, filter to get filtrate.
Embodiment 2:
The present invention provides a kind of method that employing waste lithium iron phosphate battery reclaims lithium, first carries out waste lithium iron phosphate battery
After safe-discharge process, battery is cut open along top using cold cut segmentation method, disassemble to shell and obtain battery roll core, by battery winding
Core 700 DEG C of calcinings under the atmosphere of protective gas nitrogen, the mesh sieve of grinding and sieving 90 obtains both positive and negative polarity batch mixing;To both positive and negative polarity
Sodium hydroxide solution is incorporated as in batch mixing, ultrasound and mechanical agitation filter to obtain filter mud after alternately 5 minutes;To add in filter mud
Enter chloric acid, reaction temperature is 75 DEG C, and solid-to-liquid ratio is 1/5;Lithium solution is leached, is filtered, obtain leachate, adjusted using potassium hydroxide and soaked
Go out liquid to pH 7, precipitate a small amount of iron, filter to get filtrate.
Embodiment 3:
The present invention provides a kind of method that employing waste lithium iron phosphate battery reclaims lithium, first carries out waste lithium iron phosphate battery
After safe-discharge process, battery is cut open along top using cold cut segmentation method, disassemble to shell and obtain battery roll core, by battery winding
Core is calcined 2 hours for 700 DEG C under the atmosphere of protective gas nitrogen, and the mesh sieve of grinding and sieving 100 obtains both positive and negative polarity batch mixing;To
Sodium hydroxide solution is incorporated as in both positive and negative polarity batch mixing, the mass fraction of NaOH is 25-35%, ultrasound replaces with mechanical agitation
After carrying out 5 minutes, filter mud is filtered to obtain;Chloric acid will be added in filter mud, reaction temperature is 80 DEG C, and solid-to-liquid ratio is 1/8;Leach lithium molten
Liquid, filters, and obtains leachate, and leachate is adjusted to pH 7.5 using potassium hydroxide, precipitates a small amount of iron, filters to get filtrate.
The preferred embodiment of the present invention described in detail above.It should be appreciated that one of ordinary skill in the art without
Need creative work just can make many modifications and variations with design of the invention.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (5)
1. a kind of method that employing waste lithium iron phosphate battery reclaims lithium, it is characterised in that first by waste lithium iron phosphate battery
After carrying out safe-discharge process, battery is cut open along top using cold cut segmentation method, disassemble to shell and obtain battery roll core, by electricity
Pond core 600-900 DEG C of calcining in a nitrogen atmosphere, grinding and sieving obtains both positive and negative polarity batch mixing;Add in both positive and negative polarity batch mixing
For sodium hydroxide solution, after ultrasound and mechanical agitation alternately 4-8 minutes, filter mud is filtered to obtain;Chloric acid will be added in filter mud, instead
Temperature is answered for 70-85 DEG C, solid-to-liquid ratio is 1/4-1/8;Lithium solution is leached, is filtered, obtain leachate, adjusted using potassium hydroxide and soaked
Go out liquid pH, filter, to filtrate sodium carbonate is added, obtain lithium carbonate precipitation.
2. the method that a kind of employing waste lithium iron phosphate battery according to claim 1 reclaims lithium, it is characterised in that in nitrogen
Atmosphere encloses lower calcination time for 3-5h.
3. the method that a kind of employing waste lithium iron phosphate battery according to claim 1 reclaims lithium, it is characterised in that described
Battery roll core crosses 80-120 mesh sieves after crushing, and obtains both positive and negative polarity batch mixing.
4. the method that a kind of employing waste lithium iron phosphate battery according to claim 1 reclaims lithium, it is characterised in that described
The concentration of chloric acid is 3-5mol/L.
5. the method that a kind of employing waste lithium iron phosphate battery according to claim 1 reclaims lithium, it is characterised in that adopt
Potassium hydroxide adjusts leachate to pH 6.5-7.5, precipitates a small amount of iron, filters to get filtrate.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201611018662.7A CN106654433A (en) | 2016-11-21 | 2016-11-21 | Method for recovering lithium by adopting waste lithium iron phosphate batteries |
Applications Claiming Priority (1)
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CN201611018662.7A CN106654433A (en) | 2016-11-21 | 2016-11-21 | Method for recovering lithium by adopting waste lithium iron phosphate batteries |
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CN201611018662.7A Pending CN106654433A (en) | 2016-11-21 | 2016-11-21 | Method for recovering lithium by adopting waste lithium iron phosphate batteries |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106981699A (en) * | 2017-05-13 | 2017-07-25 | 合肥国轩高科动力能源有限公司 | A kind of method that lithium is reclaimed from waste lithium iron phosphate battery |
CN109244586A (en) * | 2018-10-24 | 2019-01-18 | 北京工业大学 | A kind of waste and old power battery environmental protection recycling and reusing method |
Citations (4)
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CN103280610A (en) * | 2013-03-29 | 2013-09-04 | 江西省电力科学研究院 | Method for recovering waste lithium iron phosphate battery positive pieces |
CN105024106A (en) * | 2015-07-31 | 2015-11-04 | 合肥国轩高科动力能源股份公司 | Method for recovering ferric phosphate from waste lithium ion battery and scrapped anode piece |
CN105186058A (en) * | 2014-06-16 | 2015-12-23 | 上海奇谋能源技术开发有限公司 | Method for environmentally-friendly resource recycling of lithium ion battery electrodes |
WO2015192743A1 (en) * | 2014-06-16 | 2015-12-23 | 王武生 | Resource reclamation and environmental protection method for recycling lithium ion battery wastes |
-
2016
- 2016-11-21 CN CN201611018662.7A patent/CN106654433A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103280610A (en) * | 2013-03-29 | 2013-09-04 | 江西省电力科学研究院 | Method for recovering waste lithium iron phosphate battery positive pieces |
CN105186058A (en) * | 2014-06-16 | 2015-12-23 | 上海奇谋能源技术开发有限公司 | Method for environmentally-friendly resource recycling of lithium ion battery electrodes |
WO2015192743A1 (en) * | 2014-06-16 | 2015-12-23 | 王武生 | Resource reclamation and environmental protection method for recycling lithium ion battery wastes |
CN105024106A (en) * | 2015-07-31 | 2015-11-04 | 合肥国轩高科动力能源股份公司 | Method for recovering ferric phosphate from waste lithium ion battery and scrapped anode piece |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106981699A (en) * | 2017-05-13 | 2017-07-25 | 合肥国轩高科动力能源有限公司 | A kind of method that lithium is reclaimed from waste lithium iron phosphate battery |
CN109244586A (en) * | 2018-10-24 | 2019-01-18 | 北京工业大学 | A kind of waste and old power battery environmental protection recycling and reusing method |
CN109244586B (en) * | 2018-10-24 | 2021-03-30 | 北京工业大学 | Environment-friendly recycling method for waste power batteries |
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