CN105977569B - The method for preparing LiFePO 4 using lithium iron phosphate waste - Google Patents
The method for preparing LiFePO 4 using lithium iron phosphate waste Download PDFInfo
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- CN105977569B CN105977569B CN201610588958.6A CN201610588958A CN105977569B CN 105977569 B CN105977569 B CN 105977569B CN 201610588958 A CN201610588958 A CN 201610588958A CN 105977569 B CN105977569 B CN 105977569B
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- iron phosphate
- lithium iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The present invention discloses a kind of method preparing LiFePO 4 using lithium iron phosphate waste, includes the following steps：Lithium iron phosphate waste roasts 1~4h in 500~800 DEG C；Material after roasting phosphorates Ore Leaching, and the mixed solution of lithium phosphate and ferric phosphate is obtained by filtration；Iron powder is added, by ferric iron back in solution at ferrous iron；Filtering removes iron powder；It is 78 to adjust filtrate pH, heating reaction, and after natural cooling, filtering is dry by Washing of Filter Cake, in 500 800 DEG C of 1 4h of roasting temperature, obtains LiFePO 4.The present invention is leached using phosphoric acid, is avoided and is introduced chlorion with salt Ore Leaching, and sulfate ion is introduced with sulfuric acid leaching；The present invention is added iron powder by ferric iron back into ferrous iron, recycles hydrothermal synthesis method to prepare LiFePO 4, solve the problems, such as ferrous phosphate lithium dynamical battery resource recycling to be realized with a low cost the comprehensive reutilization of lithium iron phosphate waste.
Description
Technical field
The invention belongs to waste and old lithium ion battery utilization technology fields, specifically lithium iron phosphate waste are utilized to prepare
The method of LiFePO 4.
Background technology
Lithium ion battery is a series of green battery for having excellent performances, and since the advent of the world has been widely used.Phosphoric acid
Ferrous lithium material becomes generally acknowledged lithium ion due to having many advantages, such as high safety, high-environmental, high-energy-density, low price, long-life
The preferred material of power battery, and it has been widely used in electronic work by the lithium ion battery of positive electrode of LiFePO 4
The power batteries fields such as tool, electric bicycle, vehicle using motor, golf hurdle, ship model toy, mine lamp.With with LiFePO 4
For the application of the lithium rechargeable battery of positive electrode, the yield of battery is in rapid growth, and meeting during preparing battery
Generate a large amount of waste slurries and useless pole piece.Therefore, it for recycling material, cost-effective and environmental protection, recycles in waste material
Lithium become very necessary.The technology of common recycling lithium includes mainly roasting direct, the molten precipitation of acid etc., but during acidleach
New impurity is introduced because of the addition of acid.
At present lithium chloride is recycled by the way of roasting direct and the molten precipitation of acid.For example, Chinese patent application
201210404254.0, the method that lithium chloride is recycled from lithium iron phosphate waste is as follows：LiFePO 4 is useless
Expect to roast 1~4h in 500~800 DEG C；Material after roasting adds salt Ore Leaching, when leaching pH value control filtered 0.5~1
To the mixed solution of lithium phosphate and ferric phosphate；Gained mixed solution is heated to 80~100 DEG C, and adjusts pH value to 2~2.5, instead
1~4h is answered, is filtered, washed, is dried to obtain ferric phosphate；The filtrate of gained is filtered, pH value 6~7 is adjusted, addition calcium chloride, which is crossed, to be filtered out
Phosphorus；Filtering gained filtrate through evaporation, concentration, crystallization, wash, be dried to obtain lithium chloride.This method is simple, but with hydrochloric acid acidleach,
Generate chlorination iron tramp.
Therefore, it is still at present the heat of social common concern to the recycling research of waste lithium ion cell anode material
Point problem.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of side preparing LiFePO 4 using lithium iron phosphate waste
Method.
The purpose of the present invention can be achieved through the following technical solutions：
The method for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that this method comprises the following steps：
（1）Roasting：Lithium iron phosphate waste roasts 1~4h in 500~800 DEG C；
（2）It leaches：Material after roasting phosphorates Ore Leaching, when leaching pH value control lithium phosphate is obtained by filtration 0.5~1
With the mixed solution of ferric phosphate；
（3）Reduction：To step（2）Iron powder is added in gained mixed solution, by ferric iron back in solution at ferrous iron；
（4）Removal of impurities：Filtering removes iron powder；
（5）Hydrothermal synthesis：Regulating step（4）Gained filtrate pH is 7-8, is heated to 180 DEG C, reacts 5h, after natural cooling,
Filtering, it is dry by Washing of Filter Cake, in 500-800 DEG C of roasting temperature 1-4h, obtain LiFePO 4.
The source of lithium iron phosphate waste in the above method：
（1）The lithium iron phosphate waste generated in LiFePO 4 production process or cell production process；
（2）The useless positive plate generated in cell production process is recycled to obtain lithium iron phosphate waste, recycling side
One of method：Positive plate is heated into 300~400 DEG C of 1~4h of heat treatment, so that matrix aluminium foil is detached with positive plate, obtains ferrous phosphate
Mixture, that is, lithium iron phosphate waste of lithium, conductive agent and adhesive residue object；The two of its recovery method：Organic solvent, which impregnates, to be divided
From matrix aluminium foil and positive electrode, organic solvent, which impregnates, dissolves binder therein, and screening recycling aluminium flake collects after screening
Obtain lithium iron phosphate waste, wherein the organic solvent is N-Methyl pyrrolidone（NMP）, n,N-dimethylacetamide
（DMA）, dimethylformamide（DMF）At least one of；
（3）Old and useless battery is recycled to obtain lithium iron phosphate waste, recovery method：After old and useless battery electric discharge completely
Battery is disassembled, positive plate is taken out, according to（2）In method to positive plate carry out processing recycling obtain lithium iron phosphate waste.
Calcination temperature is crossed low reaction and cannot be carried out, and high material caking is crossed, as a preferred option, calcination temperature with 500~
800 DEG C are advisable, and object inversion of phases occurs in roasting process, and conductive agent is changed into gas effusion with binder, and LiFePO 4 occurs
Following reaction：6LiFePO4+3O2=4FePO4+2LiPO4+Fe2O3
Material acid adding after roasting leaches can phosphorate acid, hydrochloric acid, sulfuric acid etc., since hydrochloric acid is volatile, and introduces impurity
Chlorion；Sulfuric acid introduces impurity sulfate ion；Therefore the material after roasting preferably phosphorates Ore Leaching, and phosphoric acid concentration is preferably 80
~85wt%.
Washings temperature control system of the present invention is at 40~100 DEG C.
Beneficial effects of the present invention：The present invention is leached using phosphoric acid, is avoided and is introduced chlorion with salt Ore Leaching, uses sulfuric acid
It leaches and introduces sulfate ion, to keep removal of impurities simple and the purity height of final product, the present invention is to be realized with a low cost phosphoric acid
The comprehensive reutilization of ferrous lithium waste material is added iron powder by ferric iron back into ferrous iron, hydrothermal synthesis method is recycled to prepare phosphorus
Ferrous silicate lithium solves the problems, such as ferrous phosphate lithium dynamical battery resource recycling.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
Clear, complete description is carried out to design, the technology path etc. of the present invention with attached drawing with reference to embodiments, to fill
The sub-argument solution purpose of the present invention, feature and effect.Based on the embodiment of the present invention, others skilled in the art are not paying creative labor
The other embodiment obtained under the premise of dynamic, belongs to the scope of protection of the invention.Each technology in the invention is special
Sign, can be with combination of interactions under the premise of not conflicting conflict.
The object of the present invention is the LiFePO 4 waste slurry and LiFePO 4 generated in lithium ion battery manufacturing process
Useless positive plate and waste and old ferrous phosphate lithium battery.
The method for preparing LiFePO 4 using lithium iron phosphate waste, includes the following steps：
（1）Roasting：Lithium iron phosphate waste roasts 1~4h in 500~800 DEG C；It can be carried out in conventional calcining kiln,
Such as：Rotary kiln；
（2）It leaches：Material after roasting adds 80%~85% phosphoric acid to leach, and pH value control is 0.5~1 when leaching, filtering
Obtain the mixed solution of lithium phosphate and ferric phosphate；
（3）Reduction：To iron powder is added in the mixed solution of lithium phosphate and ferric phosphate, by ferric iron back in solution at divalent
Iron；
（4）Removal of impurities：Filtering removes iron powder；
（5）Hydrothermal synthesis：It is 7-8 to adjust gained filtrate pH, is heated to 180 DEG C, reacts 5h, after natural cooling, is filtered, will
Washing of Filter Cake, washings temperature control system is dry at 40~100 DEG C, in 500-800 DEG C of roasting temperature 1-4h, obtains ferrous phosphate
Lithium.
The source of lithium iron phosphate waste：
（1）The lithium iron phosphate waste generated in LiFePO 4 production process or cell production process；
（2）The useless positive plate generated in cell production process is recycled to obtain lithium iron phosphate waste, recycling side
One of method：Positive plate is heated into 300~400 DEG C of 1~4h of heat treatment, so that matrix aluminium foil is detached with positive plate, obtains ferrous phosphate
Mixture, that is, lithium iron phosphate waste of lithium, conductive agent and adhesive residue object；The two of its recovery method：Organic solvent, which impregnates, to be divided
From matrix aluminium foil and positive electrode, organic solvent, which impregnates, dissolves binder therein, and screening recycling aluminium flake collects after screening
Obtain lithium iron phosphate waste, wherein the organic solvent is N-Methyl pyrrolidone（NMP）, n,N-dimethylacetamide
（DMA）, dimethylformamide（DMF）At least one of；
（3）Old and useless battery is recycled to obtain lithium iron phosphate waste, recovery method：After old and useless battery electric discharge completely
Battery is disassembled, positive plate is taken out, according to（2）In method to positive plate carry out processing recycling obtain lithium iron phosphate waste.
Embodiment 1
As shown in Figure 1, waste and old ferrous phosphate lithium battery remaining capacity is discharged, battery is then disassembled, takes out anode
Piece crushes after ferrous lithium phosphate cathode piece is roasted 2h in 400 DEG C, or ferrous lithium phosphate cathode piece is soaked in NMP, sieves
The positive aluminium flake of recycling, obtains lithium iron phosphate waste.
1h is roasted under the conditions of 800 DEG C of lithium iron phosphate waste, product adds 85% phosphoric acid to leach after roasting, and pH is controlled when leaching
It makes to 0.5, the mixed solution of lithium phosphate and ferric phosphate is obtained after filtering, iron powder is added, by ferric iron back in solution at divalent
Iron is filtered to remove excessive iron powder, filtrate is placed in reaction kettle, and it is 7 to adjust pH value of solution, is heated to 180 DEG C, reacts 5h, from
So after cooling, filtering, by Washing of Filter Cake, washings temperature control system is dry at 40 DEG C, in 800 DEG C of roasting temperature 1h, obtains phosphoric acid
Ferrous lithium.
Embodiment 2
The lithium iron phosphate waste generated in cell production process is taken, roasts 4h under the conditions of 500 DEG C, product adds after roasting
80% phosphoric acid leaches, when leaching pH controls obtain the mixed solution of lithium phosphate and ferric phosphate after filtering to 1, iron powder be added, will
Ferric iron back is filtered to remove excessive iron powder, filtrate is placed in reaction kettle at ferrous iron in solution, and it is 8 to adjust pH value of solution,
It is heated to 180 DEG C, reacts 5h, after natural cooling, filtering, by Washing of Filter Cake, washings temperature control system is dry at 80 DEG C, at 500 DEG C
Roasting temperature 4h, obtains LiFePO 4.
Embodiment 3
The lithium iron phosphate waste generated in LiFePO 4 production process is taken, 2h is roasted under the conditions of 600 DEG C, is produced after roasting
Object adds 82% phosphoric acid to leach, and pH controls 0.8, obtain the mixed solution of lithium phosphate and ferric phosphate after filtering when leaching, and iron is added
Powder is filtered to remove excessive iron powder, filtrate is placed in reaction kettle by ferric iron back in solution at ferrous iron, adjusts solution
PH is 7, is heated to 180 DEG C, reacts 5h, and after natural cooling, filtering, by Washing of Filter Cake, washings temperature control system is dry at 100 DEG C,
In 600 DEG C of roasting temperature 3h, LiFePO 4 is obtained.
The above is only the specific implementation mode of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection domain of the application.
Claims (7)
1. the method for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that this method comprises the following steps：
（1）Roasting：Lithium iron phosphate waste roasts 1~4h in 500~800 DEG C；
（2）It leaches：Material after roasting phosphorates Ore Leaching, when leaching pH value control lithium phosphate and phosphorus is obtained by filtration 0.5~1
The mixed solution of sour iron；
（3）Reduction：To step（2）Iron powder is added in gained mixed solution, by ferric iron back in solution at ferrous iron；
（4）Removal of impurities：Filtering removes iron powder；
（5）Hydrothermal synthesis：By step（4）Gained filtrate is placed in reaction kettle, and it is 7-8 to adjust filtrate pH, is heated to 180 DEG C, instead
Answer 5h, after natural cooling, filtering is dry by Washing of Filter Cake, in 500-800 DEG C of roasting temperature 1-4h, obtains ferrous phosphate
Lithium.
2. the method according to claim 1 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that institute
State step（1）The source of middle lithium iron phosphate waste is：The phosphorus generated in LiFePO 4 production process or cell production process
Ferrous silicate lithium waste material；Or the useless positive plate generated in cell production process is recycled to obtain lithium iron phosphate waste；Or it is right
Old and useless battery is recycled to obtain lithium iron phosphate waste.
3. the method according to claim 2 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that right
The recovery method that the useless positive plate generated in cell production process is recycled to obtain lithium iron phosphate waste is：By positive plate plus
300~400 DEG C of 1~4h of heat treatment of heat, make matrix aluminium foil be detached with positive plate, obtain LiFePO 4, conductive agent and binder
The mixture of residue, i.e. lithium iron phosphate waste.
4. the method according to claim 2 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that right
The recovery method that the useless positive plate generated in cell production process is recycled to obtain lithium iron phosphate waste is：Organic solvent soaks
Matrix separation aluminium foil and positive electrode are steeped, organic solvent, which impregnates, dissolves binder therein, screening recycling aluminium flake, after screening
Collection obtains lithium iron phosphate waste, wherein the organic solvent be N-Methyl pyrrolidone, n,N-dimethylacetamide,
At least one of dimethylformamide.
5. the method according to claim 2 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that right
The recovery method that old and useless battery is recycled to obtain lithium iron phosphate waste is：Battery is disassembled after old and useless battery electric discharge completely, is taken
Go out positive plate, is recycled to obtain the method pair of lithium iron phosphate waste according to the useless positive plate generated in cell production process
Positive plate carries out processing recycling.
6. the method according to claim 1 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that institute
The phosphoric acid concentration stated is 80~85wt%.
7. the method according to claim 1 for preparing LiFePO 4 using lithium iron phosphate waste, which is characterized in that institute
Washings temperature control system is stated at 40~100 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10741890B2 (en) | 2012-04-04 | 2020-08-11 | Worcester Polytechnic Institute | Method and apparatus for recycling lithium iron phosphate batteries |
| CN106549195A (en) * | 2016-10-26 | 2017-03-29 | 荆门市格林美新材料有限公司 | A kind of method that waste lithium iron phosphate positive plate reclaims iron phosphate presoma |
| CN106910889B (en) * | 2017-02-27 | 2019-07-23 | 中南大学 | A method of regenerating positive active material from waste lithium iron phosphate battery |
| WO2018209164A1 (en) * | 2017-05-11 | 2018-11-15 | Worcester Polytechnic Institute | Method and apparatus for recycling lithium iron phosphate batteries |
| CN108110357B (en) * | 2017-12-14 | 2020-07-17 | 眉山顺应动力电池材料有限公司 | Method for recovering valuable metals from waste lithium iron phosphate battery positive electrode materials |
| CN114506871A (en) * | 2020-11-16 | 2022-05-17 | 周思齐 | Method for hydraulically producing double salt from single salt powder |
| CN113097591B (en) * | 2021-02-26 | 2022-01-11 | 云南航开科技有限公司 | Method for recovering anode material of lithium iron phosphate battery |
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| CN101359756A (en) * | 2007-07-31 | 2009-02-04 | 比亚迪股份有限公司 | Method for recycling lithium iron phosphate anode material from lithium ionic cell waste |
| CN101916889A (en) * | 2010-08-16 | 2010-12-15 | 长春劲能锂电池科技有限公司 | Method for preparing iron lithium phosphate by recovering water-system waste lithium-ion power battery |
| CN102956936A (en) * | 2011-08-25 | 2013-03-06 | 深圳市格林美高新技术股份有限公司 | Method for treating lithium iron phosphate cathode material of waste and old power lithium battery of automobile |
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| KR101439427B1 (en) * | 2013-03-14 | 2014-09-11 | 한국과학기술연구원 | Recycling method of olivine-based cathode material for lithium secondary battery, cathode material fabricated therefrom, and cathode and lithium secondary battery having the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101359756A (en) * | 2007-07-31 | 2009-02-04 | 比亚迪股份有限公司 | Method for recycling lithium iron phosphate anode material from lithium ionic cell waste |
| CN101916889A (en) * | 2010-08-16 | 2010-12-15 | 长春劲能锂电池科技有限公司 | Method for preparing iron lithium phosphate by recovering water-system waste lithium-ion power battery |
| CN102956936A (en) * | 2011-08-25 | 2013-03-06 | 深圳市格林美高新技术股份有限公司 | Method for treating lithium iron phosphate cathode material of waste and old power lithium battery of automobile |
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