CN102910607A - Comprehensive recycling method for lithium iron phosphate cathode material - Google Patents
Comprehensive recycling method for lithium iron phosphate cathode material Download PDFInfo
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Abstract
The invention relates to a comprehensive recycling method for a lithium iron phosphate cathode material, belonging to the technical field of recycle of waste lithium ion batteries. The invention aims to provide the comprehensive recycling method for the lithium iron phosphate cathode material, comprising the following steps of: a, roasting the lithium iron phosphate cathode material at the temperature of 500-800 DEG C for 1-4h; b, adding sulfuric acid into a roasted material to leach, controlling the pH value between 0.5 and 1 during leaching, and filtering to obtain a mixed solution of lithium phosphate, ferric phosphate and ferric sulfate; c, heating the mixed solution obtained in the step b to 80-100 DEG C, adjusting the pH value of the mixed solution to 2-2.5, reacting for 1-4h, filtering, cleaning and drying to obtain the ferric phosphate; and d, adjusting the pH value of a filtrate obtained through filtering in the step c to 10-12, reacting for 0.5-2h, filtering, cleaning and drying to obtain the lithium phosphate.
Description
Technical field
The present invention relates to the ferrous phosphate doping lithium anode material comprehensive reutilization method, belong to waste and old lithium ion battery recovery and utilization technology field.
Background technology
Lithium ion battery is the green battery with a series of premium propertiess, comes out 10 for many years, is widely used.LiFePO 4 (LiFePO
4) material is owing to having characteristics such as high safety, high-environmental, low price, long lifetime, become the preferred material of generally acknowledged lithium-ion-power cell, and the lithium ion battery take LiFePO 4 as positive electrode material the power cell fields such as power tool, electric bicycle, vehicle using motor, golf cart, ship model toy, mine lamp now have been widely used in.Car manufactures is also being tested use ferrousphosphate lithium material in startup power supply lithium ion battery (12V/24V 50Ah) repeatedly.Following this material also has development space in fields such as mobile communication base station, energy storage devices.
Along with the widespread use of lithium ion battery, will enter in a large number inefficacy, recovery stage.How to reclaim waste and old lithium ion battery and the resource recycling utilization has become social question of common concern.For the purpose of resource circulation utilization and industry Sustainable development, tackling wherein, elemental lithium reclaims.
Lithium ion battery is comprised of shell and inner battery core.The shell of battery is stainless steel or nickel plating box hat, and the different models such as square and cylindrical are arranged.Inner battery core is rolled structure, is comprised of major portions such as positive pole, electrolytic solution and negative poles, and positive plate mainly is made of aluminium foil, organic binder bond and lithium salts (LiFePO 4); And negative plate is mainly Copper Foil and graphite, relatively single, the easy separation of the composition of negative material.The recycling of waste lithium ion cell anode material becomes the emphasis of people's research.Its recycling technology mainly is divided into following three classes:
(1) adopt the mode of direct roasting to reclaim LiFePO 4.Such as, Chinese patent application 200710129898.2, the recovery method of ferrous phosphate doping lithium anode material in a kind of lithium ion battery waste material, it toasts described waste material 2-5 hour under 450-600 ℃ under the atmosphere of rare gas element, then mix in the ethanolic soln with described powdered product adding soluble ferric iron salt, drying at 300-500 ℃ of lower roasting 2-5 hour, reclaims and obtains ferrous phosphate doping lithium anode material under the atmosphere of rare gas element.Chinese patent application 200710076890.4, the comprehensive recovering process of the useless sheet of a kind of ferrous phosphate lithium battery anode comprises following steps: the anode material waste sheet Mechanical Crushing of collecting is fragmentated; Fragment is placed by the sintering oven under vacuum atmosphere, rare gas element and/or reducing gas and/or the nitrogen protection, under 150-750 ℃ temperature, heat-treat; Fragment after the thermal treatment is adopted mechanical separation or ultrasonic oscillation method, the aluminium foil matrix is separated from fragment, obtain the mixture of ferrous phosphate doping lithium anode material, conductive agent and adhesive residue thing; With the mixture of ferrous phosphate doping lithium anode material, conductive agent and adhesive residue thing, baking is 8-24 hour under 80-150 ℃ of temperature; With classification behind the mixture abrasive dust after the baking, the particle diameter of control powder is not more than 20 μ m, and D50 is controlled at 3-10 μ m, namely gets the ferrous lithium phosphate cathode reclaimed materials.
Although the method is simple, energy consumption is slightly high, and product purity is lower, reclaims the LiFePO 4 that obtains, and is of low quality, can not use as cell positive material.
(2) will just directly recycle behind the simple cleaning-drying of ferrous lithium phosphate cathode sheet process.Such as, Chinese patent application 200980100912.3, a kind of recoverying and utilizing method of waste and old ferrous phosphate lithium dynamical battery, after first described waste and old ferrous phosphate lithium battery being discharged fully, battery is moved in the vacuum glove box that is filled with nitrogen protection, open the cover plate of described battery with mechanical force, take out the battery core that is contained in this battery jar; Cover plate and battery jar are shifted out glove box, recycle after treatment polypropylene PP plastics, steel or the aluminium of described cover plate and battery jar; In described vacuum glove box, separate again negative plate and barrier film, and positive plate; Wherein negative plate and barrier film are recycled after treatment; And positive plate cooperates new negative plate making to become new ferrous phosphate lithium dynamical battery after cleaning, dry, screening.
The possibility that this mode can realize smoothly is not high.
(3) adopt the mode of sour molten precipitation to reclaim LiFePO 4.Such as Chinese patent application, 201010148325.6, a kind of waste and old ferrous phosphate lithium battery comprehensive recovering process, the method is utilized the binding agent on the organic solvent dissolution battery core fragment, by screening, realize that ferrousphosphate lithium material separates with clean aluminium, Copper Foil, wherein aluminium, Copper Foil reclaim by melting; Utilize NaOH solution to remove aluminium foil bits remaining in the ferrousphosphate lithium material, remove graphite and remaining binding agent by thermal treatment.After LiFePO 4 usefulness acid dissolving, utilize sodium sulphite to remove cupric ion wherein, and utilize NaOH solution or ammoniacal liquor to make iron in the solution, lithium, phosphonium ion generate throw out, and in throw out, add source of iron, lithium source or P source compound to adjust the mol ratio of iron, lithium, phosphorus, add at last carbon source, calcining obtains new ferrous phosphate doping lithium anode material in ball milling, inert atmosphere.Chinese patent application 201010253859.5, a kind of water-system waste lithium-ion-power cell reclaims the method for preparing LiFePO 4, concrete steps are as follows: 1) with behind the water-system waste lithium ion battery shearing-crushing, processed by deionized water, dry rear electrode materials and the conductive agent mixture of reclaiming sieves; 2) dried electrode materials and conductive agent mixture adding mineral acid are processed, filtered and obtain Li
+, Fe
2+, PO
4 3-Acidic solution; 3) to containing Li
+, Fe
2+, PO
4 3-Acidic solution in add lithium salts or molysite, add xitix and stir, control pH value=3-7; Filter, be precipitated; 4) LiFePO that step 3) is obtained
4Thick product joins and carries out ball milling, the LiFePO that drying and calcining obtains regenerating in the aqueous sucrose solution
4Material.
If the aforesaid method impurity removal gets totally, in theory should be feasible.But because the quality of raw material alters a great deal, homogeneity of product is difficult to be guaranteed, and can not satisfy the needs that LiFePO 4 is reclaimed in industrialized production.
Therefore, at present the research of the recycling of waste lithium ion cell anode material is remained the hot issue of social common concern.
Summary of the invention
Technical problem to be solved by this invention provides a kind of ferrous phosphate doping lithium anode material comprehensive reutilization method.
Ferrous phosphate doping lithium anode material comprehensive reutilization method of the present invention comprises the steps:
A, roasting: ferrous phosphate doping lithium anode material is in 500-800 ℃ of roasting 1～4h; Wherein, can the stoving oven of routine as: carry out roasting in the rotary kiln;
B, leaching: the material after the roasting adds sulfuric acid leaching, and the pH value is controlled at 0.5～1 during leaching, filters the mixing solutions that obtains Trilithium phosphate, tertiary iron phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixing solutions is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain tertiary iron phosphate;
D, precipitate phosphoric acid lithium: the c step is filtered the filtrate of gained and is regulated pH value to 10～12, reaction 0.5～2h, and filtration, washing, drying obtain Trilithium phosphate.
Wherein, the described ferrous phosphate doping lithium anode material of a step is the LiFePO 4 waste material that produces in the LiFePO 4 waste material that produces in the LiFePO 4 production process or the battery production process, or adopt the following methods recovery to obtain: old and useless battery is disassembled battery after discharging fully, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 ℃ of thermal treatment 1～4h, the matrix aluminium foil is separated with positive electrode material, obtain the mixture of ferrous phosphate doping lithium anode material, conductive agent and adhesive residue thing, mixture is processed getting final product by the method for a step.
Further, in the aforesaid method, preferably adopt mechanical separation, ultrasonic oscillation method to separate or organic solvent immersion matrix separation aluminium foil and positive electrode material; Wherein, described organic solvent is at least a in N-Methyl pyrrolidone (NMP), N,N-dimethylacetamide (DMA), the dimethyl formamide (DMF).Organic solvent soaks dissolving binding agent wherein, and tinsel is reclaimed in screening, can collect after the screening and obtain the LiFePO 4 waste material.
In the roasting process phase conversion reaction can occur, the iron in the LiFePO 4 changes trivalent into by divalence.
Maturing temperature is crossed low reaction and can not be carried out, but temperature is also unsuitable too high, prevents the material caking.As preferred scheme, maturing temperature is advisable with 500～800 ℃.The calcination formula is:
6LiFePO
4+3O
2＝4FePO
4+2Li
3PO
4+Fe
2O
3
Wherein, in the b step, the material after the roasting adds Ore Leaching can add sulfuric acid, hydrochloric acid etc., because hydrochloric acid is volatile, considers Working environment, and the material after the roasting preferably adds sulfuric acid leaching.Further, described sulfuric acid concentration is preferably 93～98wt%.
Further, in order to obtain high-purity phosphoric acid iron and Trilithium phosphate, temperature of washing water need be controlled at 40～100 ℃ in above-mentioned c, the d step.
Wherein, in the d step, the c step is filtered the filtrate of gained and is preferably regulated first pH value 4～7, then removes by filter a small amount of ferric iron, gained filtrate re-adjustment pH value to 10～12.
Beneficial effect of the present invention: the present inventor provides a kind of brand-new method from the another one angle, and the low-cost ferrous phosphate doping lithium anode material of recycling becomes tertiary iron phosphate with it and Trilithium phosphate reclaims respectively.Solved ferrous phosphate lithium dynamical battery resource recycling problem, for trouble and worry is removed in the development of electromobile.
Description of drawings
Fig. 1 is the schema of one of embodiment of LiFePO 4 recovery technique of the present invention.
Fig. 2 is two schema of the LiFePO 4 of the present invention embodiment that reclaims technique.
Embodiment
Ferrous phosphate doping lithium anode material comprehensive reutilization method of the present invention comprises the steps:
A, roasting: ferrous phosphate doping lithium anode material is in 500-800 ℃ of roasting 1～4h; Wherein, can the stoving oven of routine as: carry out roasting in the rotary kiln;
B, leaching: the material after the roasting adds sulfuric acid leaching, and the pH value is controlled at 0.5～1 during leaching, filters the mixing solutions that obtains Trilithium phosphate, tertiary iron phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixing solutions is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain tertiary iron phosphate;
D, precipitate phosphoric acid lithium: the c step is filtered the filtrate of gained and is regulated pH value to 10～12, reaction 0.5～2h, and filtration, washing, drying obtain Trilithium phosphate.
Wherein, the described ferrous phosphate doping lithium anode material of a step is the LiFePO 4 waste material that produces in the LiFePO 4 waste material that produces in the LiFePO 4 production process or the battery production process, or adopt the following methods recovery to obtain: old and useless battery is disassembled battery after discharging fully, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 ℃ of thermal treatment 1～4h, the matrix aluminium foil is separated with positive electrode material, obtain the mixture of ferrous phosphate doping lithium anode material, conductive agent and adhesive residue thing, mixture is processed getting final product by the method for a step.
Further, in the aforesaid method, preferably adopt mechanical separation, ultrasonic oscillation method to separate or organic solvent immersion matrix separation aluminium foil and positive electrode material; Wherein, described organic solvent is at least a in N-Methyl pyrrolidone (NMP), N,N-dimethylacetamide (DMA), the dimethyl formamide (DMF).Organic solvent soaks dissolving binding agent wherein, and tinsel is reclaimed in screening, can collect after the screening and obtain the LiFePO 4 waste material.
In the roasting process phase conversion reaction can occur, the iron in the LiFePO 4 changes trivalent into by divalence.
Maturing temperature is crossed low reaction and can not be carried out, but temperature is also unsuitable too high, prevents the material caking.As preferred scheme, maturing temperature is advisable with 500～800 ℃.The calcination formula is:
6LiFePO
4+3O
2＝4FePO
4+2Li
3PO
4+Fe
2O
3
Wherein, in the b step, the material after the roasting adds Ore Leaching can add sulfuric acid, hydrochloric acid etc., because hydrochloric acid is volatile, considers Working environment, and the material after the roasting preferably adds sulfuric acid leaching.Further, described sulfuric acid concentration is preferably 93～98wt%.
Further, in order to obtain high-purity phosphoric acid iron and Trilithium phosphate, temperature of washing water need be controlled at 40～100 ℃ in above-mentioned c, the d step.
Wherein, in the d step, the c step is filtered the filtrate of gained and is preferably regulated first pH value 4～7, then removes by filter a small amount of ferric iron, gained filtrate re-adjustment pH value to 10～12.
Following examples are implemented by following embodiment:
A. waste and old ferrous phosphate lithium battery remaining capacity is discharged, then disassemble battery, take out positive plate.
B. will pulverize behind 300-400 ℃ of roasting 1～4h of ferrous lithium phosphate cathode sheet.
C. anodal aluminium flake is reclaimed in screening, gets the LiFePO 4 waste material.
D. LiFePO 4 waste material 500-800 ℃ of roasting 1～4h.
E. material adds 93%～98% sulfuric acid leaching after the roasting, filters to obtain tertiary iron phosphate, Trilithium phosphate, ferric sulfate mixing solutions.
F. Trilithium phosphate, tertiary iron phosphate, ferric sulfate mixing solutions are heated to 80-100 ℃, and regulate the pH value to 2-2.5, react 1-4 hour, and filtration, washing, drying obtain tertiary iron phosphate.
G.f step filtrate is regulated pH value 4-7,, remove by filter a small amount of ferric iron impurity.
The filtrate that the h.g step obtains is regulated the pH value to 10-12, reacts 0.5-2 hour, and filtration, washing, drying obtain Trilithium phosphate.The lithium rate of recovery reaches more than 90% in the LiFePO 4 waste material.
Wherein, step a-h is applicable to old and useless battery and reclaims, for the LiFePO 4 waste material that produces in the LiFePO 4 waste material that produces in the LiFePO 4 production process or the battery production process, directly from steps d.
Embodiment 1 adopts the inventive method comprehensive reutilization ferrous phosphate doping lithium anode material
Waste and old ferrous phosphate lithium dynamical battery remaining capacity is discharged, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; With 400 ℃ of roasting 1h of ferrous lithium phosphate cathode sheet, anodal aluminium flake is reclaimed in screening after pulverizing; Obtain LiFePO 4 waste material 100kg, lithium content 3.53%.
Then 800 ℃ of roastings of LiFePO 4 waste material 1 hour add water and size mixing, and add 98% vitriol oil adjusting pH value to 0.5, filter and obtain tertiary iron phosphate, Trilithium phosphate, ferric sulfate mixing solutions; Mixing solutions is heated to 80 ℃, adds alkali and regulate pH value to 2.0, reaction 4h filters and obtains raw phosphoric acid iron, obtains tertiary iron phosphate through 40 ℃ of water washings, dryings again; Filtrate is regulated pH value to 4.0, then filtering and impurity removing; The removal of impurities rear filtrate is regulated pH value to 12, reacts 0.5 hour, filters and obtains the raw phosphoric acid lithium, obtains Trilithium phosphate 14.26kg through 40 ℃ of water washings, dryings.The purity of gained tertiary iron phosphate and Trilithium phosphate is respectively shown in table 1,2.
Table 1
Table 2
After testing, the lithium rate of recovery is 90.13% in the LiFePO 4 waste material.
Embodiment 2 adopts the inventive method comprehensive reutilization ferrous phosphate doping lithium anode material
The LiFePO 4 waste material 100kg that produces in the production process of power taking pond, lithium content 3.51%.Then 600 ℃ of roastings of LiFePO 4 waste material 2 hours add water and size mixing, and add 98% vitriol oil adjusting pH value to 0.8, filter and obtain tertiary iron phosphate, Trilithium phosphate, ferric sulfate mixing solutions; Mixing solutions is heated to 90 ℃, adds alkali and regulate pH value to 2.3, reaction 2h filters and obtains raw phosphoric acid iron, obtains tertiary iron phosphate through 60 ℃ of water washings, dryings again; Filtrate is regulated pH value to 5, then filtering and impurity removing; The removal of impurities rear filtrate is regulated pH value to 11, reacts 1 hour, filters and obtains the raw phosphoric acid lithium, obtains Trilithium phosphate 14.42kg through 60 ℃ of water washings, dryings.The purity of gained tertiary iron phosphate and Trilithium phosphate is respectively shown in table 3,4.
Table 3
Table 4
After testing, the lithium rate of recovery is 91.35% in the LiFePO 4 waste material.
Embodiment 3 adopts the inventive method comprehensive reutilization ferrous phosphate doping lithium anode material
Get the LiFePO 4 waste material 100kg that produces in the LiFePO 4 production process, lithium content 4.39%.Then 500 ℃ of roastings of LiFePO 4 waste material 4 hours add water and size mixing, and add 98% vitriol oil adjusting pH value to 1, filter and obtain tertiary iron phosphate, Trilithium phosphate, ferric sulfate mixing solutions; Mixing solutions is heated to 100 ℃, adds alkali and regulate pH value to 2.5, reaction 1h filters and obtains raw phosphoric acid iron, obtains tertiary iron phosphate through 80 ℃ of water washings, dryings again; Filtrate is regulated pH value to 7, then filtering and impurity removing; The removal of impurities rear filtrate is regulated pH value to 10, reacts 2 hours, filters and obtains the raw phosphoric acid lithium, obtains Trilithium phosphate 14.36kg through 100 ℃ of water washings, dryings.The purity of gained tertiary iron phosphate and Trilithium phosphate is respectively shown in table 5,6.
Table 5
Table 6
After testing, the lithium rate of recovery is 90.65% in the LiFePO 4 waste material.
Claims (6)
1. the ferrous phosphate doping lithium anode material comprehensive reutilization method is characterized in that comprising the steps:
A, roasting: ferrous phosphate doping lithium anode material is in 500-800 ℃ of roasting 1～4h;
B, leaching: the material after the roasting adds sulfuric acid leaching, and the pH value is controlled at 0.5～1 during leaching, filters the mixing solutions that obtains Trilithium phosphate, tertiary iron phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixing solutions is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain tertiary iron phosphate;
D, precipitate phosphoric acid lithium: the c step is filtered the filtrate of gained and is regulated pH value to 10～12, reaction 0.5～2h, and filtration, washing, drying obtain Trilithium phosphate.
2. ferrous phosphate doping lithium anode material comprehensive reutilization method according to claim 1, it is characterized in that: the described ferrous phosphate doping lithium anode material of a step is the LiFePO 4 waste material that produces in the LiFePO 4 waste material that produces in the LiFePO 4 production process or the battery production process, or adopt the following methods recovery to obtain: old and useless battery is disassembled battery after discharging fully, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 ℃ of thermal treatment 1～4h, the matrix aluminium foil is separated with positive electrode material, obtain ferrous phosphate doping lithium anode material, the mixture of conductive agent and adhesive residue thing.
3. ferrous phosphate doping lithium anode material comprehensive reutilization method according to claim 2 is characterized in that: adopt mechanical separation, ultrasonic oscillation method to separate or organic solvent immersion matrix separation aluminium foil and positive electrode material; Wherein, described organic solvent is at least a in N-Methyl pyrrolidone, N,N-dimethylacetamide, the dimethyl formamide.
4. each described ferrous phosphate doping lithium anode material comprehensive reutilization method according to claim 1～3, it is characterized in that: in the b step, described sulfuric acid concentration is 93～98wt%.
5. each described ferrous phosphate doping lithium anode material comprehensive reutilization method according to claim 1～4 is characterized in that: the water temperature in c, the d step during washing is 40～100 ℃.
6. each described ferrous phosphate doping lithium anode material comprehensive reutilization method according to claim 1～5 is characterized in that: in the d step, the c step is filtered the filtrate of gained and is regulated first pH value 4～7, then filtration, gained filtrate re-adjustment pH value to 10～12.
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| CN106756049A (en) * | 2016-12-23 | 2017-05-31 | 江西合纵锂业科技有限公司 | A kind of method that iron and lithium are reclaimed in the lithium iron phosphate battery positive material from failure |
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| CN108110357A (en) * | 2017-12-14 | 2018-06-01 | 眉山顺应动力电池材料有限公司 | A kind of method that valuable metal is recycled from positive material of waste lithium iron phosphate |
| CN108336442A (en) * | 2018-03-01 | 2018-07-27 | 中国科学院过程工程研究所 | A method of detaching aluminium foil and anode waste from lithium ion battery positive plate |
| CN111675203A (en) * | 2020-06-17 | 2020-09-18 | 中国科学院宁波材料技术与工程研究所 | Method for recovering lithium from waste lithium iron phosphate batteries and method for recovering lithium and iron phosphate |
| CN111675203B (en) * | 2020-06-17 | 2021-12-14 | 中国科学院宁波材料技术与工程研究所 | Method for recovering lithium from waste lithium iron phosphate batteries and method for recovering lithium and iron phosphate |
| CN112410556A (en) * | 2020-09-25 | 2021-02-26 | 湖北金泉新材料有限公司 | Method for recovering waste lithium iron phosphate powder |
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