CN102891345B - Method for recycling lithium chloride from waste lithium iron phosphate - Google Patents
Method for recycling lithium chloride from waste lithium iron phosphate Download PDFInfo
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Abstract
The invention relates to a method for recycling lithium chloride from waste lithium iron phosphate, belongs to the technical field of waste and old lithium ion battery recycle, and solves the technical problem that the method for recycling lithium chloride from the waste lithium iron phosphate is provided. The method comprises the following steps of: roasting the waste lithium iron phosphate for 1-4hours under the temperature of 500-800 DEG C; leaching the materials after roasting by using hydrochloric acid, wherein the pH value is controlled to be within 0.5-1 during leaching; filtering so as to obtain a mixing liquid of lithium phosphate, iron phosphate and ferric chloride; heating the obtained mixing liquid to be at 80-100 DEG C; adjusting the pH value to be 2-2.5; reacting for 1-4hours; filtering; washing; drying so as to obtain the iron phosphate; adjusting the pH value of obtained filtrate to be 6-7; adding calcium chloride to perform phosphorous removal; and filtering; evaporating, concentrating, crystallizing, washing and drying the obtained filtrate to obtain lithium chloride.
Description
Technical field
The present invention relates to reclaim the method for lithium chloride from LiFePO 4 waste material, 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 properties, comes out 10 for many years, is widely used.LiFePO 4 (LiFePO
4) material is owing to having the features such as high safety, high-environmental, low price, long-life, become the preferred material of generally acknowledged lithium-ion-power cell, and lithium ion battery taking 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 are now 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 the field such as mobile communication base station, energy storage device.
Along with the extensive use of lithium ion battery, will enter in a large number inefficacy, recovery stage.How to reclaim waste and old lithium ion battery and resource recycling utilization has become social question of common concern.For the object of resource circulation utilization and industry sustainable development, tackle wherein elemental lithium and reclaim.
Lithium ion battery is made up of shell and inner battery core.The shell of battery is stainless steel or nickel plating box hat, has the different models such as square and cylindrical.Inner battery core is rolled structure, is made up of major parts such as positive pole, electrolyte and negative poles, and positive plate is mainly made up of aluminium foil, organic binder bond and lithium salts (LiFePO 4); And negative plate is mainly Copper Foil and graphite, the composition of negative material is relatively single, easily separation.The recycling of waste lithium ion cell anode material becomes the emphasis of people's research.Its recycling technology is mainly divided into following three classes:
(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 2-5 hour by described waste material under the atmosphere of inert gas at 450-600 DEG C, then described powdered product is added in the ethanolic solution of soluble ferric iron salt and mixes, dry, under the atmosphere of inert gas at 300-500 DEG C roasting 2-5 hour, reclaim and obtain lithium iron phosphate cathode material.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 in by the sintering furnace under vacuum atmosphere, inert gas and/or reducibility gas and/or nitrogen protection, at the temperature of 150-750 DEG C, heat-treats; Adopt machinery to separate or ultrasonic oscillation method the fragment after heat treatment, aluminium foil matrix is separated from fragment, obtain the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing; By the mixture of lithium iron phosphate cathode material, conductive agent and adhesive residue thing, at 80-150 DEG C of temperature, toast 8-24 hour; By classification after the mixture abrasive dust after baking, the particle diameter of controlling powder is not more than 20 μ m, and D50 is controlled at 3-10 μ m, obtains ferrous lithium phosphate cathode reclaimed materials.
Although the method is simple, energy consumption is slightly high, and product alloy purity is lower, reclaims the LiFePO 4 obtaining, of low quality, can not use as cell positive material.
(2) ferrous lithium phosphate cathode sheet is just directly recycled after simple cleaning-drying.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 completely, battery is moved in the vacuum glove box that is filled with nitrogen protection, open the cover plate of described battery by mechanical force, take out the battery core being contained in this battery case; Cover plate and battery case are shifted out to 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 is after cleaning, dry, screening, coordinate new negative plate making to become new ferrous phosphate lithium dynamical battery.
The possibility that this mode can realize is smoothly not high.
(3) adopt the mode of acid-soluble 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 organic solvent dissolution battery core fragment, by screening, realize ferrousphosphate lithium material and separate with clean aluminium, Copper Foil, wherein aluminium, Copper Foil reclaim by melting; Utilize NaOH solution to remove aluminium foil bits remaining in ferrousphosphate lithium material, remove graphite and remaining binding agent by heat treatment.By LiFePO 4 with after acid-soluble solution, utilize vulcanized sodium to remove copper ion wherein, and utilize NaOH solution or ammoniacal liquor to make iron in 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, finally add carbon source, in ball milling, inert atmosphere, calcining obtains new lithium iron phosphate cathode material.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) by after water-system waste lithium ion battery shearing-crushing, by deionized water processing, dry rear electrode material and the conductive agent mixture of reclaiming sieves; 2) add inorganic acid to process dried electrode material and conductive agent mixture, filter 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 to stir, control pH value=3-7; Filter, be precipitated; 4) LiFePO step 3) being obtained
4thick product joins in aqueous sucrose solution and carries out ball milling, and drying and calcining obtains the LiFePO of regeneration
4material.
If said method impurity removal obtains 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, can not meet the needs of industrialized production recovery LiFePO 4.
Therefore, the research of the recycling to waste lithium ion cell anode material at present remains the hot issue of social common concern.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that reclaims lithium chloride from LiFePO 4 waste material.
The method that the present invention reclaims lithium chloride from LiFePO 4 waste material comprises the steps:
A, roasting: LiFePO 4 waste material is in 500～800 DEG C of roasting 1～4h; Wherein, can conventional baking furnace as: in rotary kiln, carry out roasting;
B, leaching: the material after roasting adds Leaching in Hydrochloric Acid, when leaching, pH value is controlled at 0.5～1, filters the mixed solution that obtains lithium phosphate, ferric phosphate and iron chloride;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 DEG C, and regulates pH value to 2～2.5, reaction 1～4h, filtration, washing, the dry ferric phosphate that obtains;
D, removal of impurities: the filtrate that c step is filtered gained regulates pH value 6～7, adds calcium chloride dephosphorization, filters;
E, concentrated lithium chloride: the filtrate that d step is filtered gained is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains.
Wherein, LiFePO 4 waste material in said method can be the LiFePO 4 waste material producing in the LiFePO 4 waste material that produces in LiFePO 4 production process or battery production process, also can adopt following methods to reclaim obtains: old and useless battery is disassembled battery after discharging completely, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 DEG C of heat treatment 1～4h, matrix aluminium foil is separated with positive electrode, and the mixture that obtains lithium iron phosphate cathode material, conductive agent and adhesive residue thing is LiFePO 4 waste material; Or reclaim and obtain LiFePO 4 waste material in the useless positive plate that employing said method produces from Production Process of Lithium Battery or inferior positive plate; Or the LiFePO 4 waste material producing in the positive plate production process for lithium battery.
Further, in said method, preferably adopt machinery separation, the separation of ultrasonic oscillation method or organic solvent to soak matrix separation aluminium foil and positive electrode; Wherein, described organic solvent is at least one in 1-METHYLPYRROLIDONE (NMP), DMA (DMA), dimethyl formamide (DMF).Organic solvent soaks the binding agent dissolving wherein, and sheet metal is reclaimed in screening, can collect and obtain LiFePO 4 waste material after screening.
In roasting process, thing phase conversion reaction can occur, the iron in 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 material caking.As preferred scheme, sintering temperature is advisable with 500～800 DEG C.Calcination formula is:
6LiFePO
4+3O
2＝4FePO
4+2Li
3PO
4+Fe
2O
3
Wherein, in b step, selected concentration of hydrochloric acid is preferably 20～35wt%.
Further, in order to obtain high-purity phosphoric acid iron and lithium chloride, in above-mentioned c, e step, temperature of washing water is preferably controlled at 40～100 DEG C.
Beneficial effect of the present invention: the present inventor, from another one angle, provides a kind of brand-new method, low cost recycling lithium iron phosphate cathode material, is become ferric phosphate and lithium chloride reclaims respectively.Solve ferrous phosphate lithium dynamical battery resource recycling problem, for trouble and worry is removed in the development of electric automobile.
Brief description of the drawings
Fig. 1 is the flow chart of one of embodiment of LiFePO 4 recovery process of the present invention.
Fig. 2 is two flow chart of the embodiment of LiFePO 4 recovery process of the present invention.
Embodiment
The method that the present invention reclaims lithium chloride from LiFePO 4 waste material comprises the steps:
A, roasting: LiFePO 4 waste material is in 500～800 DEG C of roasting 1～4h; Wherein, can conventional baking furnace as: in rotary kiln, carry out roasting;
B, leaching: the material after roasting adds Leaching in Hydrochloric Acid, when leaching, pH value is controlled at 0.5～1, filters the mixed solution that obtains lithium phosphate, ferric phosphate and iron chloride;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 DEG C, and regulates pH value to 2～2.5, reaction 1～4h, filtration, washing, the dry ferric phosphate that obtains;
D, removal of impurities: the filtrate that c step is filtered gained regulates pH value 6～7, adds calcium chloride dephosphorization, filters;
E, concentrated lithium chloride: the filtrate that d step is filtered gained is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains.
Wherein, LiFePO 4 waste material in said method can be the LiFePO 4 waste material producing in the LiFePO 4 waste material that produces in LiFePO 4 production process or battery production process, also can adopt following methods to reclaim obtains: old and useless battery is disassembled battery after discharging completely, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 DEG C of heat treatment 1～4h, matrix aluminium foil is separated with positive electrode, and the mixture that obtains lithium iron phosphate cathode material, conductive agent and adhesive residue thing is LiFePO 4 waste material; Or reclaim and obtain LiFePO 4 waste material in the useless positive plate that employing said method produces from Production Process of Lithium Battery or inferior positive plate; Or the LiFePO 4 waste material producing in the positive plate production process for lithium battery.
Further, in said method, preferably adopt machinery separation, the separation of ultrasonic oscillation method or organic solvent to soak matrix separation aluminium foil and positive electrode; Wherein, described organic solvent is at least one in 1-METHYLPYRROLIDONE (NMP), DMA (DMA), dimethyl formamide (DMF).Organic solvent soaks the binding agent dissolving wherein, and sheet metal is reclaimed in screening, can collect and obtain LiFePO 4 waste material after screening.
In roasting process, thing phase conversion reaction can occur, the iron in 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 material caking.As preferred scheme, sintering temperature is advisable with 500～800 DEG C.Calcination formula is:
6LiFePO
4+3O
2＝4FePO
4+2Li
3PO
4+Fe
2O
3
Wherein, in b step, selected concentration of hydrochloric acid is preferably 20～35wt%.
Further, in order to obtain high-purity phosphoric acid iron and lithium chloride, in above-mentioned c, e step, temperature of washing water is preferably controlled at 40～100 DEG C.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Following examples are implemented by following execution mode:
A. waste and old ferrous phosphate lithium battery remaining capacity is discharged, then disassemble battery, take out positive plate.
B. will after 300-400 DEG C of roasting 1～4h of ferrous lithium phosphate cathode sheet, pulverize.
C. anodal aluminium flake is reclaimed in screening, obtains LiFePO 4 waste material.
D. LiFePO 4 waste material 500-800 DEG C of roasting 1～4h.
E. after roasting, material adds 20%～35% Leaching in Hydrochloric Acid, filters and obtains ferric phosphate, lithium phosphate, iron chloride mixed solution.
F. lithium phosphate, ferric phosphate, iron chloride mixed solution are heated to 80-100 DEG C, and regulate pH value to 2-2.5, reaction 1-4 hour, filtration, washing, the dry ferric phosphate that obtains.
G.f step filtrate regulates pH value 6-7,, add calcium chloride to remove a small amount of foreign matter of phosphor.
The filtrate that h.g step obtains is through evaporation, concentrated, crystallization, filtration, washing, the dry lithium chloride that obtains.In LiFePO 4 waste material, the lithium rate of recovery reaches more than 80%.
Wherein, step a-h is applicable to old and useless battery and reclaims, for the LiFePO 4 waste material producing in the LiFePO 4 waste material producing in LiFePO 4 production process or battery production process, directly from steps d.
Embodiment 1 adopts the inventive method comprehensive reutilization LiFePO 4 waste 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; By 400 DEG C of roasting 1h of ferrous lithium phosphate cathode sheet, after pulverizing, anodal aluminium flake is reclaimed in screening; LiFePO 4 waste material 100kg, lithium content 3.50%.
800 DEG C of roastings of LiFePO 4 waste material 1 hour, then add water and size mixing, and add 20% salt acid for adjusting pH value to 0.5, filter and obtain ferric phosphate, lithium phosphate, iron chloride mixed solution; Mixed solution is heated to 80 DEG C, adds alkali and regulate pH value to 2.0, reaction 4h, filters and obtains raw phosphoric acid iron, then through 40 DEG C of water washings, the dry ferric phosphate that obtains; Filtrate regulates pH value to 6, adds 100g calcium chloride, then filtering and impurity removing; After removal of impurities, filtrate is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains, through 40 DEG C of water washings, the dry lithium chloride 17.65kg that obtains.The purity of gained ferric phosphate and lithium chloride is respectively as shown in table 1,2, and lithium chloride quality meets LiCl-T trade mark requirement in GB/T 10575-2007 standard.
Table 1
Table 2
After testing, in LiFePO 4 waste material, the lithium rate of recovery is 82.51%.
Embodiment 2 adopts the inventive method comprehensive reutilization LiFePO 4 waste material
The LiFePO 4 waste material 100kg producing in the production process of power taking pond, lithium content 3.53%.600 DEG C of roastings of LiFePO 4 waste material 2 hours, then add water and size mixing, and add 30% salt acid for adjusting pH value to 0.8, filter and obtain ferric phosphate, lithium phosphate, iron chloride mixed solution; Mixed solution is heated to 90 DEG C, adds alkali and regulate pH value to 2.3, reaction 2h, filters and obtains raw phosphoric acid iron, then through 60 DEG C of water washings, the dry ferric phosphate that obtains; Filtrate regulates pH value to 7, adds calcium chloride 100g, then filtering and impurity removing; After removal of impurities, filtrate is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains, through 40 DEG C of water washings, the dry lithium chloride 17.98kg that obtains.Respectively as shown in Table 3, 4, lithium chloride quality meets LiCl-T trade mark requirement in GB/T10575-2007 standard to the purity of gained ferric phosphate and lithium chloride.
Table 3
Table 4
After testing, in LiFePO 4 waste material, the lithium rate of recovery is 84.32%.
Embodiment 3 adopts the inventive method comprehensive reutilization LiFePO 4 waste material
Get the LiFePO 4 waste material 100kg producing in LiFePO 4 production process, lithium content 4.38%.500 DEG C of roastings of LiFePO 4 waste material 4 hours, then add water and size mixing, and add 35% salt acid for adjusting pH value to 1, filter and obtain ferric phosphate, lithium phosphate, iron chloride mixed solution; Mixed solution is heated to 100 DEG C, adds alkali and regulate pH value to 2.5, reaction 1h, filters and obtains raw phosphoric acid iron, then through 80 DEG C of water washings, the dry ferric phosphate that obtains; Filtrate regulates pH value to 6, adds 100g calcium chloride, then filtering and impurity removing; After removal of impurities, filtrate is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains, through 40 DEG C of water washings, the dry lithium chloride 17.33kg that obtains.Respectively as shown in Table 5,6, lithium chloride quality meets LiCl-T trade mark requirement in GB/T10575-2007 standard to the purity of gained ferric phosphate and lithium chloride.
Table 5
Table 6
After testing, in LiFePO 4 waste material, the lithium rate of recovery is 81.35%.
Claims (8)
1. the method that reclaims lithium chloride from LiFePO 4 waste material, is characterized in that comprising the steps:
A, roasting: LiFePO 4 waste material is in 500～800 DEG C of roasting 1～4h;
B, leaching: the material after roasting adds Leaching in Hydrochloric Acid, when leaching, pH value is controlled at 0.5～1, filters the mixed solution that obtains lithium phosphate, ferric phosphate and iron chloride;
C, precipitate phosphoric acid iron: b step gained mixed solution is heated to 80～100 DEG C, and regulates pH value to 2～2.5, reaction 1～4h, filtration, washing, the dry ferric phosphate that obtains;
D, removal of impurities: the filtrate that c step is filtered gained regulates pH value 6～7, adds calcium chloride dephosphorization, filters;
E, concentrated lithium chloride: the filtrate that d step is filtered gained is through evaporation, concentrated, crystallization, washing, the dry lithium chloride that obtains.
2. the method that reclaims lithium chloride from LiFePO 4 waste material according to claim 1, it is characterized in that: described LiFePO 4 waste material is the LiFePO 4 waste material producing in the LiFePO 4 waste material that produces in LiFePO 4 production process or battery production process, or adopt following methods recovery to obtain: old and useless battery is disassembled battery after discharging completely, separate negative plate and barrier film, and positive plate, positive plate is heated to 300-400 DEG C of heat treatment 1～4h, matrix aluminium foil is separated with positive electrode, obtain lithium iron phosphate cathode material, the mixture of conductive agent and adhesive residue thing is LiFePO 4 waste material.
3. the method that reclaims lithium chloride from LiFePO 4 waste material according to claim 1, it is characterized in that: described LiFePO 4 waste material adopts following methods to reclaim and obtains: the useless positive plate producing in Production Process of Lithium Battery or inferior positive plate are heated to 300-400 DEG C of heat treatment 1～4h, matrix aluminium foil is separated with positive electrode, and the mixture that obtains lithium iron phosphate cathode material, conductive agent and adhesive residue thing is LiFePO 4 waste material.
4. the method that reclaims lithium chloride from LiFePO 4 waste material according to claim 2, is characterized in that: the LiFePO 4 waste material producing in the positive plate production process that described LiFePO 4 waste material is lithium battery.
5. the method that reclaims lithium chloride from LiFePO 4 waste material according to claim 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 one in 1-METHYLPYRROLIDONE (NMP), DMA (DMA), dimethyl formamide (DMF).
6. according to the method that reclaims lithium chloride from LiFePO 4 waste material described in claim 1～5 any one, it is characterized in that: in b step, described concentration of hydrochloric acid is 20～35wt%.
7. according to the method that reclaims lithium chloride from LiFePO 4 waste material described in claim 1～5 any one, it is characterized in that: in c, e step, temperature of washing water is controlled at 40～100 DEG C.
8. the method that reclaims lithium chloride from LiFePO 4 waste material according to claim 6, is characterized in that: in c, e step, temperature of washing water is controlled at 40～100 DEG C.
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| CN108147384A (en) * | 2017-12-28 | 2018-06-12 | 江西赣锋循环科技有限公司 | A kind of method that battery-grade lithium dihydrogen phosphate is prepared using lithium iron phosphate waste |
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| KR101918234B1 (en) * | 2016-09-05 | 2018-11-13 | 주식회사 포스코 | Method for manufacturing lithium chloride and method for manufacturing lithium carbonate |
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| CN109264748B (en) * | 2018-09-29 | 2021-04-20 | 广东邦普循环科技有限公司 | Method for preparing lithium carbonate from crude lithium phosphate |
| CN109921087B (en) * | 2019-01-29 | 2023-01-17 | 深圳市泰力废旧电池回收技术有限公司 | Comprehensive treatment method of waste lithium iron phosphate battery |
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