CN102916236A - Comprehensive recycling method for lithium iron phosphate positive plates - Google Patents
Comprehensive recycling method for lithium iron phosphate positive plates Download PDFInfo
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- CN102916236A CN102916236A CN2012104048439A CN201210404843A CN102916236A CN 102916236 A CN102916236 A CN 102916236A CN 2012104048439 A CN2012104048439 A CN 2012104048439A CN 201210404843 A CN201210404843 A CN 201210404843A CN 102916236 A CN102916236 A CN 102916236A
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Abstract
The invention relates to a comprehensive recycling method for lithium iron phosphate positive plates, belonging to the technical field of waste lithium resource recycling. The invention is designed for solving the technical problem of providing a comprehensive recycling method for lithium iron phosphate positive plates. The comprehensive recycling method for lithium iron phosphate positive plates, disclosed by the invention, comprises the following steps of: taking a lithium iron phosphate positive plate, heating the lithium iron phosphate positive plate to 300-400 DEG C and carrying out heat treatment for 1-4 h, separating a matrix aluminum foil from a positive material so as to obtain a mixture of a lithium iron phosphate positive material, a conductive agent and adhesive residues, and roasting the mixture for 1-4 h at the temperature of 500-800DEG C; carrying out sulfuric acid leaching on an obtained material subjected to roasting, controlling the pH value of the material when leached to be 0.5-1, and filtering the obtained material so as to obtain a mixed solution of lithium phosphate, iron phosphate and ferric sulfate; heating the obtained mixed solution to 80-100 DEG C, adjusting the pH value of the mixed solution to be 2-2.5, carrying out reaction for 1-4 h on the obtained product, and then filtering, washing and drying the obtained product so as to obtain iron phosphates; and adjusting the pH value of filter liquor obtained through filtering to be 10-12, carrying out reaction on the filter liquor for 0.5-2 h, and filtering, washing and drying the obtained product so as to obtain lithium phosphates.
Description
Technical field
The present invention relates to ferrous lithium phosphate cathode sheet comprehensive reutilization method, belong to waste and old lithium resource recovery and utilization technology field.
Background technology
Lithium ion battery is the green battery with a series of premium properties, 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-life, become the preferred material of generally acknowledged lithium-ion-power cell, and the lithium ion battery take LiFePO 4 as positive electrode the electrokinetic cell fields such as electric 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 extensive use and the large-scale production of lithium ion battery, inevitably can produce waste product or the defect ware of ferrous lithium phosphate cathode sheet in the lithium ion battery production process, also become the technical barrier that enterprise faces for the processing of these waste products or defect ware.The positive plate of lithium ion battery mainly is made of aluminium foil, organic binder bond and lithium salts (LiFePO 4).At present, mainly be divided into following three classes about its recycling technology:
(1) adopt the mode of roasting direct to reclaim LiFePO 4.Such as, Chinese patent application 200710129898.2, the recovery method of lithium iron phosphate cathode 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 inert gas, then mix in the ethanolic solution with described powdered product adding soluble ferric iron salt, drying at 300-500 ℃ of lower roasting 2-5 hour, reclaims and obtains lithium iron phosphate cathode material under the atmosphere of inert gas.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 furnace under vacuum atmosphere, inert gas and/or reducibility gas and/or the nitrogen protection, under 150-750 ℃ temperature, heat-treat; Adopt machinery to separate or the ultrasonic oscillation method fragment after the heat treatment, the aluminium foil matrix is separated from fragment, obtain the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing; With the mixture of lithium iron phosphate cathode 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 case; Cover plate and battery case are shifted out glove box, recycle after treatment polypropylene PP plastics, steel or the aluminium of described cover plate and battery case; 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 heat treatment.After LiFePO 4 usefulness acid dissolving, utilize vulcanized sodium to remove copper ion wherein, and utilize NaOH solution or ammoniacal liquor to make iron in the solution, lithium, phosphonium ion generate sediment, and in sediment, 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 lithium iron phosphate cathode 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 material and the conductive agent mixture of reclaiming sieves; 2) dried electrode material and conductive agent mixture adding inorganic acid are processed, filtered and obtain Li
+, Fe
2+, PO
4 3-Acid solution; 3) to containing Li
+, Fe
2+, PO
4 3-Acid solution in add lithium salts or molysite, add ascorbic acid 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 said 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, how better the ferrous lithium phosphate cathode sheet to be recycled and become this area technical barrier in the urgent need to address.Summary of the invention
Technical problem to be solved by this invention provides a kind of comprehensive reutilization method of ferrous lithium phosphate cathode sheet.
Ferrous lithium phosphate cathode sheet comprehensive reutilization method of the present invention comprises the steps:
A, roasting: get the ferrous lithium phosphate cathode sheet, be heated to 300-400 ℃ of heat treatment 1～4h, the matrix aluminium foil is separated with positive electrode, obtain the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing, mixture is in 500-800 ℃ of roasting 1～4h; Wherein, can the baking furnace 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 mixed solution that obtains lithium phosphate, ferric phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain ferric 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 lithium phosphate.
Wherein, the described ferrous lithium phosphate cathode sheet of above-mentioned a step is preferably useless positive plate or the inferior positive plate that produces in the Production Process of Lithium Battery.
Further, in the said method, preferred machinery separation, the separation of ultrasonic oscillation method or the organic solvent of adopting soaks matrix separation aluminium foil and positive electrode; Wherein, described organic solvent is at least a in 1-METHYLPYRROLIDONE (NMP), DMA (DMA), the dimethyl formamide (DMF).Organic solvent soaks dissolving binding agent wherein, and sheet metal 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.
Sintering 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, sintering 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, described sulfuric acid concentration is preferably 93～98wt%.
Further, in order to obtain high-purity phosphoric acid iron and lithium 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, and gained filtrate is regulated pH value to 10～12 again.
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 lithium phosphate cathode sheet of recycling becomes ferric phosphate with it and lithium phosphate reclaims respectively.Solved the recycling problem of inferior ferrous lithium phosphate cathode sheet, for trouble and worry is removed in the development of electric automobile.
Description of drawings
Fig. 1 is the flow chart of one of embodiment of LiFePO 4 recovery technique of the present invention.
Embodiment
Ferrous lithium phosphate cathode sheet comprehensive reutilization method of the present invention comprises the steps:
A, roasting: get the ferrous lithium phosphate cathode sheet, be heated to 300-400 ℃ of heat treatment 1～4h, the matrix aluminium foil is separated with positive electrode, obtain the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing, mixture is in 500-800 ℃ of roasting 1～4h; Wherein, can the baking furnace of routine as: carry out roasting in the rotary kiln;
B, leaching: the material after the roasting adds Ore Leaching, and the pH value is controlled at 0.5～1 during leaching, filters the mixed solution that obtains lithium phosphate, ferric phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain ferric 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 lithium phosphate.
Wherein, the described ferrous lithium phosphate cathode sheet of above-mentioned a step is preferably useless positive plate or the inferior positive plate that produces in the Production Process of Lithium Battery.
Further, in the said method, preferred machinery separation, the separation of ultrasonic oscillation method or the organic solvent of adopting soaks matrix separation aluminium foil and positive electrode; Wherein, described organic solvent is at least a in 1-METHYLPYRROLIDONE (NMP), DMA (DMA), the dimethyl formamide (DMF).Organic solvent soaks dissolving binding agent wherein, and sheet metal 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.
Sintering 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, sintering 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, described sulfuric acid concentration is preferably 93～98wt%.
Further, in order to obtain high-purity phosphoric acid iron and lithium 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, and gained filtrate is regulated pH value to 10～12 again.
Following examples are implemented by following execution mode:
A. will pulverize behind 300-400 ℃ of roasting 1～4h of waste phosphoric acid ferrous lithium positive plate.
B. anodal aluminium flake is reclaimed in screening.
C. the 500-800 ℃ of roasting 1～4h of LiFePO 4 waste material after sieving.
D. material adds 93%～98% sulfuric acid leaching after the roasting, filters to obtain ferric phosphate, lithium phosphate, ferric sulfate mixed solution.
E. lithium phosphate, ferric phosphate, ferric sulfate mixed solution are heated to 80-100 ℃, and regulate the pH value to 2-2.5, react 1-4 hour, and filtration, washing, drying obtain ferric phosphate.
F.e step filtrate is regulated pH value 4-7,, remove by filter a small amount of ferric iron impurity.
The filtrate that the g.f step obtains is regulated the pH value to 10-12, reacts 0.5-2 hour, and filtration, washing, drying obtain lithium phosphate.The lithium rate of recovery reaches more than 90% in the LiFePO 4 waste material.
Embodiment 1 adopts the inventive method comprehensive reutilization ferrous lithium phosphate cathode sheet
With 400 ℃ of roasting 1.5h of waste phosphoric acid ferrous lithium positive plate, anodal aluminium flake is reclaimed in screening after pulverizing; LiFePO 4 waste material 100kg, lithium content 3.51%.
Then 800 ℃ of roastings of LiFePO 4 waste material 1.5 hours add water and size mixing, and add 98% concentrated sulfuric acid adjusting pH value to 0.5, filter and obtain ferric phosphate, lithium phosphate, ferric sulfate mixed solution; Mixed solution is heated to 80 ℃, adds alkali and regulate pH value to 2.0, reaction 4h filters and obtains raw phosphoric acid iron, obtains ferric phosphate through 40 ℃ of water washings, dryings again; Filtrate is regulated pH value to 4, 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 lithium phosphate 14.58kg through 40 ℃ of water washings, dryings.The purity of gained ferric phosphate and lithium phosphate is respectively shown in table 1,2.
Table 1
Table 2
After testing, the lithium rate of recovery is 92.53% in the LiFePO 4 waste material.Embodiment 2 adopts the inventive method comprehensive reutilization ferrous lithium phosphate cathode sheet
With 350 ℃ of roasting 2h of waste phosphoric acid ferrous lithium positive plate, anodal aluminium flake is reclaimed in screening after pulverizing; LiFePO 4 waste material 100kg, lithium content 3.50%.
Then 600 ℃ of roastings of LiFePO 4 waste material 2 hours add water and size mixing, and add 98% concentrated sulfuric acid adjusting pH value to 0.8, filter and obtain ferric phosphate, lithium phosphate, ferric sulfate mixed solution; Mixed solution is heated to 90 ℃, adds alkali and regulate pH value to 2.3, reaction 2h filters and obtains raw phosphoric acid iron, obtains ferric 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 lithium phosphate 14.5kg through 60 ℃ of water washings, dryings.The purity of gained ferric phosphate and lithium phosphate is respectively shown in table 3,4.
Table 3
Table 4
After testing, the lithium rate of recovery is 91.58% in the LiFePO 4 waste material.
Embodiment 3 adopts the inventive method comprehensive reutilization ferrous lithium phosphate cathode sheet
With 300 ℃ of roasting 4h of waste phosphoric acid ferrous lithium positive plate, anodal aluminium flake is reclaimed in screening after pulverizing; LiFePO 4 waste material 100kg, lithium content 3.49%.
Then 500 ℃ of roastings of LiFePO 4 waste material 4 hours add water and size mixing, and add 98% concentrated sulfuric acid adjusting pH value to 1, filter and obtain ferric phosphate, lithium phosphate, ferric sulfate mixed solution; Mixed solution is heated to 100 ℃, adds alkali and regulate pH value to 2.5, reaction 1h filters and obtains raw phosphoric acid iron, obtains ferric 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 lithium phosphate 14.58kg through 100 ℃ of water washings, dryings.The purity of gained ferric phosphate and lithium phosphate is respectively shown in table 5,6.
Table 5
Table 6
After testing, the lithium rate of recovery is 91.84% in the LiFePO 4 waste material.
Claims (6)
1. ferrous lithium phosphate cathode sheet comprehensive reutilization method is characterized in that comprising the steps:
A, roasting: get the ferrous lithium phosphate cathode sheet, be heated to 300-400 ℃ of heat treatment 1～4h, the matrix aluminium foil is separated with positive electrode, obtain the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing, mixture 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 mixed solution that obtains lithium phosphate, ferric phosphate and ferric sulfate;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 ℃, and regulates pH value to 2～2.5, reaction 1～4h, and filtration, washing, drying obtain ferric 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 lithium phosphate.
2. ferrous lithium phosphate cathode sheet comprehensive reutilization method according to claim 1, it is characterized in that: the described ferrous lithium phosphate cathode sheet of a step is useless positive plate or the inferior positive plate that produces in the Production Process of Lithium Battery.
3. ferrous lithium phosphate cathode sheet comprehensive reutilization method according to claim 1 and 2 is characterized in that: adopt machinery separation, ultrasonic oscillation method to separate or organic solvent immersion matrix separation aluminium foil and positive electrode; Wherein, described organic solvent is at least a in 1-METHYLPYRROLIDONE, DMA, the dimethyl formamide.
4. each described ferrous lithium phosphate cathode sheet 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 lithium phosphate cathode sheet 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 lithium phosphate cathode sheet 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, and gained filtrate is regulated pH value to 10～12 again.
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Cited By (8)
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|---|---|---|---|---|
| CN103241720A (en) * | 2013-05-20 | 2013-08-14 | 昆明理工大学 | Method for preparing amorphous iron phosphate by using phosphate sludge |
| CN104953200A (en) * | 2015-06-30 | 2015-09-30 | 哈尔滨工业大学 | Method for recycling battery-grade iron phosphate in lithium iron phosphate battery and preparing lithium iron phosphate positive material by utilizing waste lithium ion phosphate battery |
| CN106629646A (en) * | 2016-11-28 | 2017-05-10 | 荆门市格林美新材料有限公司 | Resource recovery method of lithium iron phosphate waste materials |
| 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 |
| CN106997973A (en) * | 2017-05-12 | 2017-08-01 | 湖南省正源储能材料与器件研究所 | The phosphatic method of ferric phosphate and lithium is prepared in a kind of anode material from 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 |
| CN109935922A (en) * | 2019-03-14 | 2019-06-25 | 北京矿冶科技集团有限公司 | A method of recycling valuable metal from waste and old lithium ion battery material |
| SE543505C2 (en) * | 2019-04-15 | 2021-03-09 | Northvolt Ab | Process for the recovery of cathode materials in the recycling of lithium ion batteries |
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| CN106997973A (en) * | 2017-05-12 | 2017-08-01 | 湖南省正源储能材料与器件研究所 | The phosphatic method of ferric phosphate and lithium is prepared in a kind of anode material from waste lithium iron phosphate |
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| CN109935922A (en) * | 2019-03-14 | 2019-06-25 | 北京矿冶科技集团有限公司 | A method of recycling valuable metal from waste and old lithium ion battery material |
| SE543505C2 (en) * | 2019-04-15 | 2021-03-09 | Northvolt Ab | Process for the recovery of cathode materials in the recycling of lithium ion batteries |
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