CN106981699A - Method for recovering lithium from waste lithium iron phosphate batteries - Google Patents
Method for recovering lithium from waste lithium iron phosphate batteries Download PDFInfo
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- CN106981699A CN106981699A CN201710336688.4A CN201710336688A CN106981699A CN 106981699 A CN106981699 A CN 106981699A CN 201710336688 A CN201710336688 A CN 201710336688A CN 106981699 A CN106981699 A CN 106981699A
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- Prior art keywords
- lithium
- powder
- solution
- phosphate
- value
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- 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.)
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002699 waste material Substances 0.000 title claims abstract description 21
- 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 20
- 239000000843 powder Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001386 lithium phosphate Inorganic materials 0.000 claims abstract description 9
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 8
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 8
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 37
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 22
- 239000008346 aqueous phase Substances 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 4
- 229910021529 ammonia Inorganic materials 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 9
- 239000004411 aluminium Substances 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 235000011118 potassium hydroxide Nutrition 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 206010016766 flatulence Diseases 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012071 phase Substances 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)
- Secondary Cells (AREA)
- Primary Cells (AREA)
Abstract
The invention discloses a method for recovering lithium from waste lithium iron phosphate batteries, which comprises the following steps: disassembling and shelling the waste lithium iron phosphate battery, crushing the obtained battery roll core, and mechanically separating to obtain powder; calcining in air to remove carbon in the powder; adding the mixture into alkali liquor to carry out chemical reaction, and filtering the product to obtain an aluminum hydroxide precipitate and filter mud; adding water into the filter mud, uniformly stirring, adding strong acid for reaction, and filtering to obtain a lithium solution; adjusting the pH value of the lithium solution, extracting a small amount of iron in the lithium solution by using an extracting agent, and reserving an extracted water phase; adjusting the pH value of the water phase, and adding sodium phosphate solid to obtain lithium phosphate precipitate. The lithium is recovered in the form of lithium phosphate, the recovery process is simple, the battery roll core is directly treated, the treatment process efficiency is high, and the method is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to lithium recovery technology field, and in particular to a kind of side that lithium is reclaimed from waste lithium iron phosphate battery
Method.
Background technology
Lithium ion battery has the advantages that energy density is high, had extended cycle life, self discharge is small, memory-less effect, from commodity
It is of great interest with applying since change.But because of breakage, flatulence, the reason such as scrap caused by waste and old lithium ion battery
Increasingly increase, how to handle these old and useless batterys extremely urgent.
It is at present to first pass through to disassemble to isolate positive plate on most of recovery of lithium in ferric phosphate lithium cell, then just
Pole material is separated with positive plate, and this process efficiency is low, is not suitable for large-scale industrial production.And at present from lithium-ion electric
In the technique that lithium is reclaimed in pond reclaimed in the form of lithium carbonate mostly, and reclaim the complex procedures of lithium carbonate, efficiency is low.
The content of the invention
It is an object of the invention to provide a kind of method that lithium is reclaimed from waste lithium iron phosphate battery, lithium is with the shape of lithium phosphate
Formula recovery, recovery process is simple, efficiency high, and product purity is high, and time that lithium ion can be rapidly and efficiently is leached by selectivity
Receive the lithium in waste lithium iron phosphate battery, it is adaptable to large-scale industrial production.
Technical scheme is as follows：
A kind of method that lithium is reclaimed from waste lithium iron phosphate battery, comprises the following steps：
（1）Waste lithium iron phosphate battery is disassembled and shelled, then the battery roll core of gained is crushed, it is mechanically decoupled, obtain powder；
（2）Isolated powder is calcined in atmosphere, the carbon in powder is removed；
（3）Will be through step（2）Powder after calcination is added to be chemically reacted in alkali lye, and product is carried out to filter to obtain aluminium hydroxide
Sediment and filter mud；
（4）After water is added into filter mud and is stirred, add strong acid and reacted, filter to obtain lithium solution；
（5）Lithium pH value of solution is adjusted, iron a small amount of in lithium solution is extracted with extractant, retains the aqueous phase after extraction；
（6）Aqueous phase pH is adjusted, sodium phosphate solid is added and obtains lithium phosphate precipitation.
Further scheme, the step（2）The temperature that middle powder is calcined in atmosphere is 600 DEG C -700 DEG C, calcination time
For 4-6h.
Further scheme, the step（3）Middle alkali lye is at least one of sodium hydroxide or potassium hydroxide.
Further scheme, the step（4）In strong acid be sulfuric acid, control solution ph for 0.3-0.5, the temperature of reaction
For 60 DEG C -80 DEG C.
Further scheme, the step（4）In filter mud and water quality and volume ratio g：ML is 1：2.
Further scheme, the step（5）It is middle to adjust lithium with least one of sodium hydroxide, potassium hydroxide, ammoniacal liquor
The pH value of solution is 1-1.5；The extractant is p204.
Further scheme, the step（6）It is middle to adjust water with least one of sodium hydroxide, potassium hydroxide, ammoniacal liquor
Phase pH is value 8-10, and the addition of sodium phosphate is 1.2-1.5 times of aqueous phase quality, and reaction temperature is 80-90 DEG C.
P204 in the present invention is the extractant that American Cyanamid Company is used as Separation of nickel and cobalt, is extraction commonly used in the art
Agent.
Beneficial effects of the present invention are as follows：
1st, a kind of method that lithium is reclaimed from waste lithium iron phosphate battery that the present invention is provided, lithium is returned in the form of lithium phosphate
Receive, recovery process is simple；
2nd, the present invention by the direct progress of battery roll core is handled burnt after powder, reduce the step that battery roll core disassembles separation
Suddenly, it is adaptable to mass produce；
3rd, present invention selectivity leaching lithium, efficiently separates lithium and iron, it is simple efficiently, it is cost-effective, can be rapidly and efficiently return
Receive the lithium in waste lithium iron phosphate battery, it is adaptable to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the method flow diagram that lithium is reclaimed from waste lithium iron phosphate battery of the present invention.
Embodiment
It is following that present invention is further illustrated in conjunction with the embodiments：
Embodiment 1
The present invention provides a kind of method that lithium is reclaimed from waste lithium iron phosphate battery, and it is as shown in figure 1, comprise the following steps：
（1）Waste lithium iron phosphate battery after overdischarge disassemble shell after obtain battery roll core；
（2）By mechanically decoupled after battery roll core is crushed, powder is isolated；
（3）Powder is calcined into 5h for 650 DEG C under nitrogen atmosphere, carbon dust, powder after being burnt are removed by high temperature；
（4）Sodium hydroxide solution is added into the powder after burning, the oxide of the aluminium remained in powder and aluminium is removed, protected after filtering
Stay filter mud；
（5）Add water into filter mud, the ratio of filter mud and water is 1/2 (kg/L), add sulfuric acid and control pH value of solution to be 0.4, react
Temperature is 60 DEG C, and filter residue is removed after reaction result and obtains lithium solution；
（6）It is 1.5 by sodium hydrate regulator solution pH, adds iron a small amount of in p204 extraction solution, standing separation goes out aqueous phase；
（7）With sodium hydroxide regulation aqueous phase pH=8, the sodium phosphate solid of 1.3 times of addition filters to obtain lithium phosphate precipitation.
Embodiment 2
A kind of method that lithium is reclaimed from waste lithium iron phosphate battery, comprises the following steps：
（1）Waste lithium iron phosphate battery after overdischarge disassemble shell after obtain battery roll core；
（2）By mechanically decoupled after battery roll core crushing, powder is isolated；
（3）Powder is calcined into 6h for 600 DEG C under nitrogen atmosphere, carbon dust, powder after being burnt are removed by high temperature；
（4）Potassium hydroxide solution is added into the powder after burning, the oxide of the aluminium remained in powder and aluminium is removed, protected after filtering
Stay filter mud；
（5）Add water into filter mud, the ratio of filter mud and water is 1/2 (kg/L), add sulfuric acid and control pH value of solution to be 0.5, react
Temperature is 80 DEG C, and filter residue is removed after reaction result and obtains lithium solution；
（6）It is 1 to adjust pH value of solution by potassium hydroxide, adds iron a small amount of in p204 extraction solution, and standing separation goes out aqueous phase；
（7）With potassium hydroxide regulation aqueous phase pH=9, the sodium phosphate solid of 1.2 times of addition filters to obtain lithium phosphate precipitation.
Embodiment 3
A kind of method that lithium is reclaimed from waste lithium iron phosphate battery, comprises the following steps：
（1）Waste lithium iron phosphate battery after overdischarge disassemble shell after obtain battery roll core；
（2）By mechanically decoupled after battery roll core crushing, powder is isolated；
（3）Powder is calcined into 4h for 700 DEG C under nitrogen atmosphere, carbon dust, powder after being burnt are removed by high temperature；
（4）Sodium hydroxide solution is added into the powder after burning, the oxide of the aluminium remained in powder and aluminium is removed, protected after filtering
Stay filter mud；
（5）Add water into filter mud, the ratio of filter mud and water is 1/2 (kg/L), add sulfuric acid and control pH value of solution to be 0.3, react
Temperature is 80 DEG C, and filter residue is removed after reaction result and obtains lithium solution；
（6）It is 1.5 to adjust pH value of solution by ammoniacal liquor, adds iron a small amount of in p204 extraction solution, and standing separation goes out aqueous phase；
（7）Aqueous phase pH=8.5 are adjusted by ammoniacal liquor, 1.5 times of sodium phosphate solid is added, lithium phosphate precipitation is filtered to obtain.
Preferred embodiment of the 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 according to the design of the present 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 (7)
1. a kind of method that lithium is reclaimed from waste lithium iron phosphate battery, it is characterised in that：Comprise the following steps：
（1）Waste lithium iron phosphate battery is disassembled and shelled, then the battery roll core of gained is crushed, it is mechanically decoupled, obtain powder；
（2）Isolated powder is calcined in atmosphere, the carbon in powder is removed；
（3）Will be through step（2）Powder after calcination is added to be chemically reacted in alkali lye, and product is carried out to filter to obtain aluminium hydroxide
Sediment and filter mud；
（4）After water is added into filter mud and is stirred, add strong acid and reacted, filter to obtain lithium solution；
（5）Lithium pH value of solution is adjusted, iron a small amount of in lithium solution is extracted with extractant, retains the aqueous phase after extraction；
（6）Aqueous phase pH is adjusted, sodium phosphate solid is added and obtains lithium phosphate precipitation.
2. according to the method described in claim 1, it is characterised in that：The step（2）The temperature that middle powder is calcined in atmosphere
It is 4-6h for 600 DEG C -700 DEG C, calcination time.
3. according to the method described in claim 1, it is characterised in that：The step（3）Middle alkali lye is sodium hydroxide or hydroxide
At least one of potassium.
4. according to the method described in claim 1, it is characterised in that：The step（4）In strong acid be sulfuric acid, control pH value of solution
It is worth for 0.3-0.5, the temperature of reaction is 60 DEG C -80 DEG C.
5. according to the method described in claim 1, it is characterised in that：The step（4）In filter mud and water quality and volume
Compare g：ML is 1：2.
6. according to the method described in claim 1, it is characterised in that：The step（5）Middle use sodium hydroxide, potassium hydroxide, ammonia
At least one of water is 1-1.5 come the pH value for adjusting lithium solution；The extractant is p204.
7. according to the method described in claim 1, it is characterised in that：The step（6）Middle use sodium hydroxide, potassium hydroxide, ammonia
At least one of water adjusts aqueous phase pH for value 8-10, and the addition of sodium phosphate is 1.2-1.5 times of aqueous phase quality, react
Temperature is 80-90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710336688.4A CN106981699A (en) | 2017-05-13 | 2017-05-13 | Method for recovering lithium from waste lithium iron phosphate batteries |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710336688.4A CN106981699A (en) | 2017-05-13 | 2017-05-13 | Method for recovering lithium from waste lithium iron phosphate batteries |
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| Publication Number | Publication Date |
|---|---|
| CN106981699A true CN106981699A (en) | 2017-07-25 |
Family
ID=59342044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710336688.4A Pending CN106981699A (en) | 2017-05-13 | 2017-05-13 | Method for recovering lithium from waste lithium iron phosphate batteries |
Country Status (1)
| Country | Link |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540004A (en) * | 2017-09-21 | 2018-01-05 | 合肥国轩高科动力能源有限公司 | Method for recovering battery-grade lithium carbonate from waste lithium iron phosphate battery positive electrode powder |
| CN109524735A (en) * | 2018-10-19 | 2019-03-26 | 合肥国轩高科动力能源有限公司 | Recovery method of waste lithium iron phosphate-lithium titanate battery |
| CN111009660A (en) * | 2019-11-26 | 2020-04-14 | 宁夏百川新材料有限公司 | Method for preparing lithium iron phosphate positive electrode material from waste lithium iron phosphate battery |
| CN112180261A (en) * | 2020-09-16 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Lithium analysis detection method for lithium iron phosphate power battery |
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| CN107540004A (en) * | 2017-09-21 | 2018-01-05 | 合肥国轩高科动力能源有限公司 | Method for recovering battery-grade lithium carbonate from waste lithium iron phosphate battery positive electrode powder |
| CN109524735A (en) * | 2018-10-19 | 2019-03-26 | 合肥国轩高科动力能源有限公司 | Recovery method of waste lithium iron phosphate-lithium titanate battery |
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| CN112180261A (en) * | 2020-09-16 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Lithium analysis detection method for lithium iron phosphate power battery |
| CN112180261B (en) * | 2020-09-16 | 2022-04-12 | 合肥国轩高科动力能源有限公司 | Lithium analysis detection method for lithium iron phosphate power battery |
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Application publication date: 20170725 |