CN103641175A - Method for dissolving positive material of waste/used lithium-ion batteries - Google Patents
Method for dissolving positive material of waste/used lithium-ion batteries Download PDFInfo
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- CN103641175A CN103641175A CN201310630768.2A CN201310630768A CN103641175A CN 103641175 A CN103641175 A CN 103641175A CN 201310630768 A CN201310630768 A CN 201310630768A CN 103641175 A CN103641175 A CN 103641175A
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- lithium
- waste
- lithium ion
- malic acid
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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
Abstract
The invention discloses a method for dissolving a positive material of waste/used lithium-ion batteries. The key point of the technical scheme of the invention is as follows: the method mainly comprises the step of dissolving the lithium manganate positive material of the waste/used lithium-ion batteries by using organic acid and malic acid which serve as solvents, and specific dissolving steps and the setting of all parameters of a dissolving process are disclosed specifically. According to the invention, organic acid and malic acid are used as the solvents, so that the damage to equipment is less, and the method has the advantages of environmental friendliness, simple process, high recovery ratio, capability of industrial popularization, and the like; in addition, malic acid which has relatively strong acidity and relatively high conductivity is suitable for serving as an organic acid solvent.
Description
Technical field
The present invention relates to waste and old lithium ion battery reutilization field, be specifically related to a kind of method of dissolving waste lithium ion cell anode material.
Background technology
Lithium ion battery has a series of premium propertiess, there is high-energy-density, high power density, operating voltage is high, and the advantage such as have extended cycle life, since the more than ten years of coming out, the fields such as mobile telephone, notebook computer, pick up camera have been widely used in, again progressively to new-energy automobile, power tool class is seted out now, and the market share significantly improves.Anode material for lithium-ion batteries mainly contains LiMO at present
2(LiCoO
2, LiNiO
2, LiNi
1/3co
1/3mn
1/3o
2) system, lithium manganese oxide (LiMn
2o
4) system and iron lithium system (LiFePO
4) system, wherein lithium manganese oxide system have preparation easily, pollute low, low price,, the advantage such as security height, thereby obtained studying widely and utilizing.
Yet the lithium ion battery normal service life that the lithium manganate of take is positive electrode material approximately only had about 3 years, along with the widespread use of lithium ion battery, old and useless battery amount is soaring year by year.In lithium ion battery, contain the chemical substances such as lithium hexafluoro phosphate, organic solvent carbonic ether, aluminium, copper, manganese, wherein lithium hexafluoro phosphate has severe corrosive, and the boiling point of carbonic ether is 90 ℃ of left and right, volatile, inflammable and explosive, these hazardous and noxious substances can cause serious pollution to atmosphere, water, soil, and can be detrimental to health.Plastics in waste and old lithium ion battery or metal shell, electrolytic solution, electrolytic salt and electrode waste material all have recovery value, so recycle waste and old lithium ion battery, have the value of environmental protection and economic benefit.
After obtaining the positive electrode material of battery after processing waste and old lithium ion battery, it again be dissolved and could further make high value added product.At present, a lot of correlative studys are all to take mineral acid to dissolve anode material for lithium-ion batteries as solvent as nitric acid, sulfuric acid, hydrochloric acid, but the corrodibility of mineral acid is strong, and easily contaminate environment, larger to experimental installation infringement.This patent is to waste lithium ion cell anode material LiMn
2o
4solubility property in organic acid is studied.
Summary of the invention
The present invention provides a kind of method of dissolving waste lithium ion cell anode material for overcoming the deficiencies in the prior art, and the method is higher to the dissolution rate of waste lithium ion cell anode material, and less to the damage of equipment.
Technical scheme of the present invention is: a kind of method of dissolving waste lithium ion cell anode material, it is characterized in that mainly take that organic acid oxysuccinic acid dissolves waste and old lithium ion battery manganate cathode material for lithium as solvent, concrete steps are: (1) obtains the manganate cathode material for lithium in waste and old lithium ion battery by waste and old lithium ion battery through peeling off shell, fragmentation, Screening Treatment; (2) manganate cathode material for lithium step (1) being obtained is dissolved in the malic acid solution that volumetric molar concentration is 0.1-2.0mol/L, wherein the quality of manganate cathode material for lithium and the volume ratio of malic acid solution are 45-90g/L, are then placed in constant temperature blender with magnetic force and carry out heating in water bath dissolving in 40-50 ℃; (3) in the solution making to step (2), adding mass concentration is 30% superoxol, wherein the volume add-on of superoxol is the 3%-7% that step (2) makes liquor capacity, produce after bubble, filter, wash, complete the dissolution process of waste and old lithium ion battery manganate cathode material for lithium.
The volumetric molar concentration of the malic acid solution in step of the present invention (2) is 0.75-1.25mol/L, is wherein preferably 1.0mol/L; In described step (2), the quality of manganate cathode material for lithium and the volume ratio of malic acid solution are 45-75g/L, are wherein preferably 60g/L; The temperature that in described step (2), heating in water bath dissolves is 45 ℃; In described step (3), the volume add-on of superoxol is that step (2) makes 5% of liquor capacity.
It is less to equipment damage that the present invention uses organic acid oxysuccinic acid to make solvent, and there is environmental protection, technique is simple, the rate of recovery is high, can advantage such as industry popularization etc., in addition, the acidity of oxysuccinic acid is stronger, specific conductivity is higher, the suitable organic acid solvent of doing, adopts dissolving method of the present invention to can reach 99.05% to the dissolution rate of waste and old lithium ion battery manganate cathode material for lithium.
Accompanying drawing explanation
Fig. 1 is the impact analysis figure of the embodiment of the present invention 1 dissolution time to manganate cathode material for lithium dissolution rate, Fig. 2 is the impact analysis figure of the concentration of the embodiment of the present invention 2 malic acid solutions to dissolution rate, Fig. 3 is the impact analysis figures of the embodiment of the present invention 3 solid-liquid ratios to dissolution rate, Fig. 4 is the impact analysis figures of the embodiment of the present invention 4 solvent temperatures to dissolution rate, and Fig. 5 is the impact analysis figures of the embodiment of the present invention 5 superoxols to dissolution rate.
Embodiment
By the following examples foregoing of the present invention is described in further details, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on foregoing of the present invention all belong to scope of the present invention.
Waste and old lithium ion battery (take lithium manganate as positive electrode material) is peeled off to the processing such as shell, simple crushing, screening according to correct method steps, to obtain the manganate cathode material for lithium in waste and old lithium ion battery.
First with electronic balance, taking quality is m
1manganate cathode material for lithium sample, be dissolved in malic acid solution, then be placed on and in constant temperature blender with magnetic force, carry out heating in water bath dissolving, approximately after 2min, survey the pH value of mixed solution, to adding mass concentration in solution, be 30% superoxol again, there are immediately a large amount of Bubble formations, after bubble collapse, record pH value now, in solution, add ammoniacal liquor again, make the pH=7 of solution, prevent from occurring precipitating in dissolution process, after arriving certain reaction times, solution is carried out to suction filtration, filter residue is dried 24h in electric heating air blast thermostatic drying chamber 100 ℃ of left and right, weigh its quality and be designated as m
2, the dissolution rate of lithium ion battery manganate cathode material for lithium is: ω (%)=[(m
1-m
2)/m
1] * 100.
This test high spot reviews solvent temperature, dissolution time, solid-liquid ratio (quality of manganate cathode material for lithium and the volume ratio of malic acid solution), superoxol add-on (volume of superoxol and the volume percent that adds the mixing solutions after malic acid solution, wherein the mass concentration of superoxol is 30%) and the impact of five factors such as volumetric molar concentration dissolution rate in malic acid solution on manganate cathode material for lithium of malic acid solution, in order to seek suitable dissolution conditions, according to the result of single factor experiment, respectively get three levels and carry out orthogonal test.
embodiment 1
The impact of dissolution time on manganate cathode material for lithium dissolution rate
Setting respectively dissolution time is 5min, 10min, 15min, 20min, 30min, and 50 ℃ of solvent temperatures, solid-liquid ratio 60g/L, superoxol add-on 7.0%, malic acid concentration 1.0mol/L, then measure corresponding dissolution rate.
As shown in Figure 1 along with the increase of dissolution time, dissolution rate increases gradually, after 10min, dissolution rate is substantially constant, the former of this phenomenon do not react completely with malic acid solution because of manganate cathode material for lithium when 5min, and the state that tends to balance of the chemical reaction in solubility test after 10min, therefore determine that dissolution time is 10min.
embodiment 2
The impact of the volumetric molar concentration of malic acid solution on manganate cathode material for lithium dissolution rate
The volumetric molar concentration of setting respectively malic acid solution is 0.1mol/L, 0.5mol/L, 1.0mol/L, 1.5mol/L, 2.0mol/L, 50 ℃ of solvent temperatures, solid-liquid ratio 60g/L, superoxol add-on 7.0%, dissolution time 10min, then measure corresponding dissolution rate.
As shown in Figure 2, along with the increase of malic acid solution volumetric molar concentration, dissolution rate increases gradually, when the volumetric molar concentration of malic acid solution is 1.0mol/L, dissolution rate is maximum, the volumetric molar concentration of malic acid solution continues to increase afterwards, and dissolution rate declines, because oxysuccinic acid is weak electrolyte, its ionization equilibrium in water is subject to the impact of concentration, during excessive concentration, its degree of ionization declines, so select 0.75-1.25mol/L for malic acid concentration preferably.
embodiment 3
The impact of solid-liquid ratio on manganate cathode material for lithium dissolution rate
Setting respectively solid-liquid ratio is 45g/L, 60g/L, 75g/L, 80g/L, 90g/L, and the volumetric molar concentration 1.0mol/L of dissolution time 10min, 50 ℃ of solvent temperatures, superoxol add-on 7.0%, malic acid solution measures respectively the dissolution rate after dissolving.
As shown in Figure 3, when solid-liquid ratio is 80g/L, 90g/L, dissolution rate is lower, when solid-liquid ratio is 75g/L, dissolution rate almost reaches maximum value, although dissolution rate is also very large when solid-liquid ratio is 45g/L, but now malic acid solution is excessive, malic acid solution is excessive can follow-up gel reaction and the calcination process of impact, and can produce certain impact to the form of the positive electrode material of finally making and chemical property, therefore selects 60-75g/L for solid-liquid ratio preferably.
embodiment 4
The impact of solvent temperature on manganate cathode material for lithium dissolution rate
Temperature is one of key factor affecting dissolution rate, setting successively heating in water bath solvent temperature is 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, the volumetric molar concentration 1.0mol/L of dissolution time 10min, solid-liquid ratio 60g/L, superoxol add-on 7.0%, malic acid solution, measures respectively the dissolution rate after dissolving.
As shown in Figure 4, when temperature is increased to 40 ℃ from 20 ℃, dissolution rate is lower, when temperature reaches 40-50 ℃, speed of reaction is obviously accelerated, because the activation energy of reactant is lower when temperature is lower, make speed of reaction lower, and the degree of ionization of temperature rising oxysuccinic acid increases, and when temperature continues to be increased to 60 ℃, dissolution rate presents downward trend, because when excess Temperature, oxysuccinic acid volatilization causes the concentration of malic acid solution to reduce, thereby reduces dissolution rate, therefore select 40-50 ℃ for solvent temperature preferably.
embodiment 5
The impact of superoxol add-on on manganate cathode material for lithium dissolution rate
Setting respectively superoxol add-on (volume percent) is 0.0%, 2.0%, 3.0%, 5.0%, 7.0%, the volumetric molar concentration 1.0mol/L of 50 ℃ of solvent temperatures, solid-liquid ratio 60g/L, dissolution time 10min, oxysuccinic acid, measures respectively the dissolution rate after dissolving.
Superoxol is at positive electrode material LiMn
2o
4dissolution process in play a reductive agent, as long as so make its excessive a little needs that just can meet reaction, add as shown in Figure 5 appropriate superoxol can improve significantly dissolution rate, dissolution rate increases along with the increase of superoxol add-on, after superoxol add-on reaches 5.0%, dissolution rate is substantially constant, so select 3.0%-5.0%, is the add-on of superoxol preferably.
orthogonal test is preferred
On the basis of single factor experiment, take dissolution rate as investigating index, adopt L9 (34) orthogonal table to arrange orthogonal test, investigate malic acid concentration, solvent temperature, the add-on of superoxol, 4 factors of solid-liquid ratio, dissolution time is defined as 10min.Orthogonal test level of factor is in Table 1, orthogonal test scheme with the results are shown in Table 2.
Table 1 orthogonal test level of factor coding schedule
Table 2 orthogonal test scheme and result
From quadrature result and range analysis, the positive electrode material LiMn of used Li ion cell
2o
4suitable dissolution conditions is A
2b
2c
3d
1, i.e. the volumetric molar concentration 1.0mol/L of malic acid solution, 45 ℃ of solvent temperatures, superoxol add-on 5.0%, solid-liquid ratio 60g/L.In addition, according to range analysis, obtained the primary and secondary of each factor to Index Influence, each factor affects size order to dissolution rate and is: the volumetric molar concentration > solid-liquid ratio > solvent temperature > superoxol add-on of oxysuccinic acid.
malic acid solution dissolves the mechanism of manganate cathode material for lithium
Under the suitable dissolution conditions drawing in above-mentioned orthogonal test, the dissolution mechanism of manganate cathode material for lithium in malic acid solution is as follows: spinel type LiMn
2o
4the mn ion that contains three kinds of different valence state, i.e. Mn
2+, Mn
3+, Mn
4+, Mn wherein
3+, Mn
4+content reach more than 95%, and can not exist in solution with simple ionic species, and Mn
2+can stable existence in the acidic solution without strong oxidizer, so will make pressed powder LiMn
2o
4be dissolved in better in malic acid solution, the mn ion of high valence state will be reduced to divalent manganesetion.Dissolution process can be divided into following two stages:
1, from single factor experiment, when superoxol add-on is 0%, oxysuccinic acid also can dissolve a certain amount of manganate cathode material for lithium, is due to spinel type LiMn
2o
4in Mn
3+there is disproportionation reaction, thus under suitable dissolution conditions, before adding superoxol, Mn
3+also can there is disproportionation reaction, because disproportionation reaction is special redox reaction, so also can explain this reaction from the angle of electrode potential.
Manganese element potential energy diagram E Φ/V is as follows:
MnO
2 
mn
3+ 
mn
2+(acidic solution)
From potential energy diagram, E
Φ right=1.51, E
Φ left=0.95, E
Φ right-E
Φ left=1.51-0.95>0, thus this disproportionation reaction can occur, lgK again
θ=n (E
Φ right-E
Φ left)/0.0592, it is generally acknowledged, works as K
θ>10
4reaction is carried out thoroughly, calculates K
θ=10
9.56>10
4therefore it is thorough that this reaction not only can occur but also can react, ion-reaction equation: 2Mn
3++ 2H
2o=MnO
2+ Mn
2++ 4H
+;
2, Mn
3+after there is disproportionation reaction, in mixed solution, also has the mn ion of high price, so will add strong reductant H
2o
2with its generation redox reaction, and be reduced to Mn
2+, from the relation of electrode potential and redox reaction, explain reaction mechanism.A redox reaction is to be all Ox by two half-reactions
1+ 2e → R
1, R
2-2e → Ox
2(in formula, Ox, R represent respectively oxidized form, reduced form material) forms, and its reaction tendency and completeness can be by two the poor Δ E=of half-reaction electrode potential E
Φ oxygenant-E
Φ reductive agentjudge.
H
2o
2 
o
2, MnO
2 
mn
2+(acidic solution)
From above potential energy diagram, H
2o
2make reductive agent, MnO
2make oxygenant, E
Φ oxygenant=0.95, E
Φ reductive agent=0.699, Δ E=E
Φ oxygenant-E
Φ reductive agent=0.95-0.699>0, thus this redox reaction can occur, same calculating K
θ=10
4.24>10
4so this redox reaction can occur and can react thoroughly ion-reaction equation: MnO
2+ 2H
++ H
2o
2=Mn
2++ 2H
2o+O
2↑.
In sum, used Li ion cell positive electrode material LiMn
2o
4solubilizing reaction equation in malic acid solution is as follows:
C
4H
6O
5?+LiMn
2O
4+?H
2O
2 (C
4H
4O
5)Li
2+(C
4H
4O
5)Mn+H
2O+O
2↑。
Above embodiment has described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; do not departing under the scope of the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (5)
1. a method of dissolving waste lithium ion cell anode material, it is characterized in that mainly take that organic acid oxysuccinic acid dissolves waste and old lithium ion battery manganate cathode material for lithium as solvent, concrete steps are: (1) obtains the manganate cathode material for lithium in waste and old lithium ion battery by waste and old lithium ion battery through peeling off shell, fragmentation, Screening Treatment; (2) manganate cathode material for lithium step (1) being obtained is dissolved in the malic acid solution that volumetric molar concentration is 0.1-2.0mol/L, wherein the ratio of the quality of manganate cathode material for lithium and the volume of malic acid solution is 45-90g/L, is then placed in constant temperature blender with magnetic force and carries out heating in water bath dissolving in 40-50 ℃; (3) in the solution making to step (2), adding mass concentration is 30% superoxol, wherein the volume add-on of superoxol is the 3%-7% that step (2) makes liquor capacity, produce after bubble, filter, wash, complete the dissolution process of waste and old lithium ion battery manganate cathode material for lithium.
2. the method for dissolving waste lithium ion cell anode material according to claim 1, is characterized in that: the volumetric molar concentration of the malic acid solution in described step (2) is 0.75-1.25mol/L.
3. the method for dissolving waste lithium ion cell anode material according to claim 1 and 2, is characterized in that: the volumetric molar concentration of the malic acid solution in described step (2) is 1.0mol/L.
4. the method for dissolving waste lithium ion cell anode material according to claim 1, is characterized in that: in described step (2), the quality of manganate cathode material for lithium and the volume ratio of malic acid solution are 60-75g/L.
5. the method for dissolving waste lithium ion cell anode material according to claim 1, is characterized in that: in described step (3), the volume add-on of superoxol is that step (2) makes 5% of liquor capacity.
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| CN109687051A (en) * | 2018-12-25 | 2019-04-26 | 云南能投汇龙科技股份有限公司 | A kind of method for recycling anode material of waste and old lithium ion battery |
| CN110563046A (en) * | 2019-09-10 | 2019-12-13 | 广州大学 | method for recycling waste lithium ion battery anode material |
| CN112345324A (en) * | 2020-11-02 | 2021-02-09 | 东北石油大学 | Preparation method of natural crack in rock core |
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Application publication date: 20140319 |