CN103682510A - Electrolyte used for waste lithium battery discharge, and waste lithium battery discharge method - Google Patents

Electrolyte used for waste lithium battery discharge, and waste lithium battery discharge method Download PDF

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Publication number
CN103682510A
CN103682510A CN201310642412.0A CN201310642412A CN103682510A CN 103682510 A CN103682510 A CN 103682510A CN 201310642412 A CN201310642412 A CN 201310642412A CN 103682510 A CN103682510 A CN 103682510A
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electrolyte
waste lithium
waste
discharge
lithium battery
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CN201310642412.0A
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CN103682510B (en
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魏增福
谈天
任平
刘世念
钟国彬
苏伟
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Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Electric Power Research Institute of Guangdong Power Grid Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • 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 an electrolyte used for waste lithium battery discharge, and a waste lithium battery discharge method. The electrolyte contains copper sulfate and the concentration of copper sulfate is 0.1-1mol/L; the electrolyte also contains ascorbic acid; and the discharge method comprises a step that a waste lithium battery is immersed in the electrolyte until the voltage tends toward stability. The electrolyte used for waste lithium battery discharge is obtained through a large amount of experiments and researches by the inventors of the invention, and has the advantages of safety, environmental protection, high discharge efficiency, no precipitation of the above solution in the discharge process, and no dissolving loss of the shell of the battery. The waste lithium ion battery discharge method has the advantages of simple technology, easy operation, and suitableness for the industrial application.

Description

Electrolyte and charging method for waste lithium cell electric discharge
Technical field
The present invention relates to electrolyte field, particularly relate to a kind of electrolyte and charging method of waste lithium cell electric discharge.
Background technology
Along with lithium ion battery is applied widely, produced a large amount of waste and old lithium ion batteries, at present owing to containing a large amount of virose rare metal cobalts in waste and old lithium ion battery, but because cobalt is a kind of important strategy metal, for example, so contrasting at present the research of waste and old lithium ion battery focuses mostly on aspect the recycling of precious metal: current ternary lithium battery, also contains the noble metals such as manganese, nickel, meanwhile, in lithium ion battery, also contain the valuable metals such as picture aluminium, copper.Yet, waste and old lithium ion battery is in the electric treatment process that disappears (being about to the inner remaining electric weight of waste and old lithium ion battery emits) in batches, because can making the electric weight that battery is remaining, the process such as short circuit, fragmentation in decomposable process sharply discharges, cause local overheating even to explode, therefore waste and old lithium ion battery fully electric discharge before recycling, must be to the waste and old lithium ion battery electric treatment that disappears.
At present, for the safe-discharge of waste and old lithium ion battery, mainly contain two kinds of methods, a kind of is physical method electric discharge, be mainly by the external load electricity that disappears, by battery, be connected with resistance, the electric weight in battery consumes by heat release, but the method is laboratory test, discharge on a large scale infeasible; Another kind is chemical method electric discharge, the both positive and negative polarity metal that utilizes battery is negative electrode and anode, in solution, by electrolytic process, carry out electric weight remaining in consuming cells, mainly take sodium chloride solution at present as electrolyte, waste and old lithium ion battery is that power supply discharges, the method simple possible, but because anode when sodium chloride solution discharges can be separated out chlorine, can corroding electrode pollute electrolyte system on the one hand, operating personnel's operational environment is also had to impact simultaneously, simultaneously also can cause battery case solution loss and the recovery problem of the lysate that brings thus.
Summary of the invention
Based on this, one of object of the present invention is for providing a kind of electrolyte for waste and old lithium ion battery electric discharge.
The concrete technical scheme solving the problems of the technologies described above is as follows:
An electrolyte for waste and old lithium ion battery electric discharge, contains copper sulphate in described electrolyte; The concentration of described copper sulphate is 0.1-1mol/L.
In some embodiment, the concentration of described copper sulphate is 0.5mol/L therein.
In some embodiment, in described electrolyte, also comprise ascorbic acid (Vc) therein.
In some embodiment, the concentration of described ascorbic acid is 0.05-0.3mol/L therein.
In some embodiment, the concentration of described ascorbic acid is 0.1mol/L therein.
The present invention also provides a kind of method of waste and old lithium ion battery safe-discharge, comprises the steps: pending waste and old lithium ion battery in batches to put into above-mentioned electrolyte, until electric current and voltage tends towards stability.
Of the present inventionly a kind ofly for waste and old lithium ion battery, lay electric electrolyte and charging method has the following advantages and beneficial effect:
(1) electrolyte of waste and old lithium ion battery safe-discharge of the present invention is to draw through a large amount of experiment of inventor and research, its safety, environmental protection, ion in electrolyte is larger in the reaction speed of anode and negative electrode, discharging efficiency is high, and in discharge process, solution forms without precipitation, do not produce poisonous and harmful substances, and battery case can solution loss yet, specifically, lithium ion battery is when electric discharge, battery just, the more incident anode reaction in negative pole metal surface and cathode reaction, and the product generating can not polluted the electric electrolyte that disappears, as produce precipitation, just, negative pole dissolving etc.
(2) in the electrolyte of waste and old lithium ion battery safe-discharge of the present invention except copper sulphate, also further comprise ascorbic acid, itself and copper sulphate combine, make the electrochemical reaction of anode by separating out of oxygen, be changed into the oxidation of ascorbic acid, negative electrode is the reduction of copper ion, can further promote anode reaction, make these two electrode reactions can effectively solve polarization in battery discharge procedure and the problems such as pollution of product.
(3) waste and old lithium ion battery safe-discharge method of the present invention, technique is simple to operation, is applicable to industrial applications.
Accompanying drawing explanation
Fig. 1 is the voltage-time curve comparison diagram in dissimilar electrolyte electric discharge;
Fig. 2 is the CuSO of variable concentrations 4voltage-time curve figure in electrolyte electric discharge;
Fig. 3 is 0.5mol/LCuSO 4with the voltage-time curve figure in the ascorbic acid electrolyte electric discharge of variable concentrations;
Fig. 4 is the voltage-to-current curve comparison figure in electrolyte electric discharge.
Embodiment
The present invention has eliminated the remaining capacity in waste and old lithium ion battery by chemical method, has solved potential safety hazard and the environmental pollution causing and other security hidden troubles such as burning that waste and old lithium ion battery in enormous quantities produces due to battery short circuit in elementary removal process or blast.
Below with reference to specific embodiment, the present invention will be further described.
Embodiment 1
For an electrolyte for waste and old lithium ion battery electric discharge, CuSO in described electrolyte 4concentration be 0.1mol/L.
When investigating the discharge scenario of electrolyte, adopted laboratory test methods, comprise the steps:
Waste and old lithium ion battery both positive and negative polarity is drawn with wire, and be connected with nickel sheet respectively, again nickel sheet is put into respectively to above-mentioned electrolyte, measure immediately electric current in battery discharge procedure and (or) voltage over time, observe the variation on both positive and negative polarity nickel sheet surface in electrolyte simultaneously, until electric current and voltage tend towards stability, electric discharge finishes.
Embodiment 2
For an electrolyte for waste and old lithium ion battery electric discharge, CuSO in described electrolyte 4concentration be 0.3mol/L;
A method for waste and old lithium ion battery safe-discharge, refers to embodiment 1.
Embodiment 3
For an electrolyte for waste and old lithium ion battery electric discharge, CuSO in described electrolyte 4concentration is 0.5mol/L;
A method for waste and old lithium ion battery safe-discharge, refers to embodiment 1.
Embodiment 4
For an electrolyte for waste and old lithium ion battery electric discharge, CuSO in described electrolyte 4concentration is 1mol/L;
A method for waste and old lithium ion battery electric discharge, refers to embodiment 1.
Embodiment 5
An electrolyte for waste and old lithium ion battery electric discharge, contains electrolyte copper sulphate and ascorbic acid, described CuSO in described electrolyte 4concentration 0.5mol/L, the concentration of described ascorbic acid is 0.1mol/L.
A method for waste and old lithium ion battery electric discharge, refers to embodiment 1.
Embodiment 6
For an electrolyte for waste and old lithium ion battery electric discharge, described electrolyte is substantially the same manner as Example 5, and difference is: the concentration of ascorbic acid is 0.05mol/L.
Embodiment 7
For an electrolyte for waste and old lithium ion battery electric discharge, described electrolyte is substantially the same manner as Example 5, and difference is: the concentration of ascorbic acid is 0.3mol/L.
The evaluation method of embodiment 8 waste and old lithium ion battery electric discharges
One, experiment purpose
By the variation of solution in discharging efficiency, the feature of environmental protection, fail safe and the discharge process of electrolyte described in comparative analysis Evaluation operation example 1-7.
Two, experimental technique
Comparative example 1: electrolyte is the NaCl solution of concentration 0.1mol/L;
Comparative example 2: electrolyte is the Na of concentration 0.1mol/L 2sO 3solution;
Comparative example 3:Na 2sO 3and CuSO 4mixed electrolytic solution, Na wherein 2sO 3concentration be 0.1mol/L and CuSO 4concentration be 0.1mol/L;
By recording electric current in waste and old lithium ion battery discharge process and voltage over time, observe the variation on both positive and negative polarity nickel sheet surface and electrolyte in electrolyte simultaneously.
Three, experimental result
Result is referring to Fig. 1, Fig. 2, Fig. 3 and Fig. 4.
As can be seen from Figure 1, waste and old lithium ion battery is at electrolyte Na 2sO 3while disappearing electric treatment in solution, the final piezoelectric voltage that disappears is higher, more than 2.5V. and the electric process that disappears is slow, and speed is minimum, and anode Ni dissolving, cathode hydrogen evolution, visible CuSO in solution 3flocculent deposit.Therefrom known: Na 2sO 3can not be oxidized at anode, anode mainly be take and is analysed oxygen as main, and the dissolving of nickel has been accelerated in the existence of dissolved oxygen, and Na 2sO 3solution is alkaline system, has suppressed separating out of cathode hydrogen, and the piezoelectric voltage that therefore disappears is higher.
Using copper-bath and sodium chloride solution respectively as the electrolyte electricity that disappears, and the final piezoelectric voltage that disappears all can drop to below 1.5V, and the electric speed that disappears is higher.Wherein, what in sodium chloride solution Anodic reaction, be chlorine separates out, and it has promoted the dissolving of nickel, has formed the hydrolytic precipitation of nickel ion and cathode hydrogen evolution in electrolyte; When copper-bath disappears electricity, anode is for analysing oxygen process, the copper of negative electrode visible deposition, because system is acid system, in electrolyte solution without precipitation; In this two individual system, there is respectively Cl -ion and Cu 2+ion, as the depolarizing agent of anode and negative electrode, has obviously reduced the electric voltage that disappears, but contrasts knownly, and sodium chloride solution Anodic has chlorine to separate out, and has precipitation to form, and this brings extra recovery process for the recovery of follow-up waste electrolyte.
And using copper sulphate and sodium sulfite mixed solution as the electrolyte electricity that disappears, and the piezoelectric voltage that finally disappears can drop to 1.0V left and right, and voltage drop speed is very fast, and efficiency is higher, but this solution forms CuSO 3precipitation; Show relatively independent NaCl solution and CuSO simultaneously 4solution, using copper sulphate and sodium sulfite mixed solution as electrolytical voltage lower be because solution in total ion concentration higher, the voltage drop of battery in solution is less, also illustrates in the electric solution that disappears, and when solution concentration is large, can reduce the piezoelectric voltage that disappears.
In order further to promote the carrying out of anodic process, in the optimization of electrolyte, introduced reducing agent ascorbic acid, by copper sulphate and ascorbic acid combination, in such situation, the electrochemical reaction of anode is changed into the oxidation of ascorbic acid by separating out of oxygen, negative electrode is the reduction of copper ion, and these two electrode reactions can solve polarization in battery discharge procedure and the problems such as pollution of product effectively.Ascorbic acid has stronger reproducibility, copper ion can be reduced to the copper of simple substance, but show by test under certain condition, and ascorbic acid is in certain concentration range, and coexisting of the two is stable.
As can be seen from Figure 2, the CuSO of variable concentrations 4solution, the piezoelectric voltage that finally disappears all can drop to below 1.5V, and CuSO 4cuSO in solution 4concentration larger, pressure drop rate is larger, efficiency is higher.
Fig. 3 is containing CuSO 4concentration is the voltage-time curve figure during the electrolyte of the ascorbic acid (Vc) of 0.5mol/L and variable concentrations discharges, as seen from Figure 3, along with ascorbic acid concentrations increases, battery discharge lower voltage, discharge effect is better.In electrolyte, add after reducing agent ascorbic acid, the electrochemical reaction of anode is changed into the oxidation of ascorbic acid by separating out of oxygen, and nickel sheet surface does not have separating out of oxygen, and nickel sheet also keeps bright state.Negative electrode is the reduction of copper ion, visible by copper sulphate and ascorbic acid combination, can further promote the carrying out of anodic process and cathodic process, so these two electrode reactions can solve polarization in battery discharge procedure and the problems such as pollution of product effectively, realize the discharge process of greater efficiency.
Therefore, from discharging efficiency and environmental protection equal angles, using the electrolyte that contains electrolyte copper sulphate and ascorbic acid, as the electric solution that disappears, be, more satisfactory.Although CuSO in electrolyte 4higher with the concentration of ascorbic acid, discharge effect is better, but considers the cost of the electric electrolyte that disappears and the difference of variable concentrations electrolyte discharge effect, here CuSO in preferred electrolyte 4concentration be that the concentration of 0.5mol/L, ascorbic acid (Vc) is 0.1mol/L.
As can be seen from Figure 4, in discharge process, all there is the phenomenon increasing with lower voltage electric current in various electrolyte solutions at first, along with the reducing of voltage, electric current also reduced afterwards, and voltage curve presents straight line substantially, be in discharge process, to meet Ohm's law, it is constant that resistance keeps substantially.In discharge process, the resistance of copper-bath is more bigger, and the resistance of mixed solution is minimum, and this is mainly when the electrolyte solution of same concentrations, due to not of uniform size the causing of conductivity of solution.When lithium ion battery reclaims, a large amount of waste and old lithium ion batteries can be put into copper sulphate and ascorbic acid solution discharges, can eliminate rapidly the participation electric weight of inside battery, for follow-up recovery process provides safety guarantee.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.

Claims (6)

1. for an electrolyte for waste lithium cell electric discharge, it is characterized in that, in described electrolyte, contain copper sulphate; The concentration of described copper sulphate is 0.1-1mol/L.
2. the electrolyte for waste lithium cell electric discharge according to claim 1, is characterized in that, the concentration of described copper sulphate is 0.5mol/L.
3. according to the electrolyte for waste lithium cell electric discharge described in claim 1-2 any one, it is characterized in that, described electrolyte also comprises ascorbic acid.
4. the electrolyte for waste lithium cell electric discharge according to claim 3, is characterized in that, the concentration of described ascorbic acid is 0.05～0.3mol/L.
5. the electrolyte for waste lithium cell electric discharge according to claim 4, is characterized in that, the concentration of described ascorbic acid is 0.1mol/L.
6. a method for waste lithium cell safe-discharge, is characterized in that, comprise the steps: pending waste lithium cell in batches to put into the electrolyte described in claim 1-5 any one, until electric current and voltage tends towards stability.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104037468A (en) * 2014-06-05 2014-09-10 浙江工业大学 Method for recycling manganese and copper resources from waste lithium ion batteries
CN104882645A (en) * 2015-04-01 2015-09-02 长安大学 Method for recycling metal ions in waste and old LiCoO2 cells
CN109004308A (en) * 2018-08-27 2018-12-14 惠州亿纬锂能股份有限公司 Waste and old lithium ion battery charging method
CN110391474A (en) * 2018-04-23 2019-10-29 中南大学 A kind of charging method of waste and old lithium ion battery
CN110635185A (en) * 2018-06-22 2019-12-31 中天储能科技有限公司 Discharge method of waste lithium battery
CN114361623A (en) * 2021-12-09 2022-04-15 万向一二三股份公司 Waste lithium ion battery discharging method suitable for large-scale application
CN114552044A (en) * 2022-02-22 2022-05-27 中国科学院生态环境研究中心 Method for quickly releasing residual electric quantity of waste lithium ion battery by coupling electrolyte with ultrasonic waves
CN117438682A (en) * 2023-12-21 2024-01-23 深圳市杰成镍钴新能源科技有限公司 Method for completely discharging waste lithium ion battery

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CN106058358A (en) * 2016-08-17 2016-10-26 合肥国轩高科动力能源有限公司 Discharge method of improving discharge degree of waste lithium ion battery

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CN101054631A (en) * 2007-05-18 2007-10-17 北京矿冶研究总院 Method for recovering valuable metal in invalid lithium ion battery
CN101519726A (en) * 2009-04-16 2009-09-02 北京矿冶研究总院 Method for directly roasting and treating waste lithium ion battery and recycling valuable metal
CN102709624A (en) * 2012-05-24 2012-10-03 北京理工大学 Immiscible water/polymer two-phase electrolyte and battery

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Publication number Priority date Publication date Assignee Title
CN101054631A (en) * 2007-05-18 2007-10-17 北京矿冶研究总院 Method for recovering valuable metal in invalid lithium ion battery
CN101519726A (en) * 2009-04-16 2009-09-02 北京矿冶研究总院 Method for directly roasting and treating waste lithium ion battery and recycling valuable metal
CN102709624A (en) * 2012-05-24 2012-10-03 北京理工大学 Immiscible water/polymer two-phase electrolyte and battery

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104037468A (en) * 2014-06-05 2014-09-10 浙江工业大学 Method for recycling manganese and copper resources from waste lithium ion batteries
CN104037468B (en) * 2014-06-05 2016-06-22 浙江工业大学 A kind of method reclaiming manganese and copper resource from waste and old lithium ion battery
CN104882645A (en) * 2015-04-01 2015-09-02 长安大学 Method for recycling metal ions in waste and old LiCoO2 cells
CN104882645B (en) * 2015-04-01 2017-03-29 长安大学 It is a kind of to reclaim waste and old LiCoO2The method of metal ion in battery
CN110391474A (en) * 2018-04-23 2019-10-29 中南大学 A kind of charging method of waste and old lithium ion battery
CN110391474B (en) * 2018-04-23 2020-09-29 中南大学 Discharging method of waste lithium ion battery
CN110635185A (en) * 2018-06-22 2019-12-31 中天储能科技有限公司 Discharge method of waste lithium battery
CN109004308A (en) * 2018-08-27 2018-12-14 惠州亿纬锂能股份有限公司 Waste and old lithium ion battery charging method
CN114361623A (en) * 2021-12-09 2022-04-15 万向一二三股份公司 Waste lithium ion battery discharging method suitable for large-scale application
CN114552044A (en) * 2022-02-22 2022-05-27 中国科学院生态环境研究中心 Method for quickly releasing residual electric quantity of waste lithium ion battery by coupling electrolyte with ultrasonic waves
CN117438682A (en) * 2023-12-21 2024-01-23 深圳市杰成镍钴新能源科技有限公司 Method for completely discharging waste lithium ion battery
CN117438682B (en) * 2023-12-21 2024-02-27 深圳市杰成镍钴新能源科技有限公司 Method for completely discharging waste lithium ion battery

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