CN109461948A - Utilize the method for the electrolyte liquid regeneration V electrolyte of failure vanadium cell - Google Patents
Utilize the method for the electrolyte liquid regeneration V electrolyte of failure vanadium cell Download PDFInfo
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- CN109461948A CN109461948A CN201811279104.5A CN201811279104A CN109461948A CN 109461948 A CN109461948 A CN 109461948A CN 201811279104 A CN201811279104 A CN 201811279104A CN 109461948 A CN109461948 A CN 109461948A
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/008—Disposal or recycling of fuel cells
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
- H01M2300/00—Electrolytes
- H01M2300/0002—Aqueous electrolytes
- H01M2300/0005—Acid electrolytes
- H01M2300/0011—Sulfuric acid-based
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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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
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- Manufacturing & Machinery (AREA)
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The method that the present invention relates to the use of the electrolyte liquid regeneration V electrolyte of failure vanadium cell, belongs to vanadium battery field.To be solved by this invention is that existing failure V electrolyte recycles the problem that technique is cumbersome, utilization rate is low, its technical solution there is provided the method for the electrolyte liquid regeneration V electrolyte using failure vanadium cell includes the following steps: that vanadic anhydride and H are added into electrolyte liquid2SO4, sufficiently react, be separated by solid-liquid separation, collect liquid phase, be diluted with water to get regenerating electrolytes, the failure vanadium cell is using sulfuric acid as supporting electrolyte.Using regeneration method of the present invention, it can be with the electrolyte liquid of 100% rate of recovery recycling failure vanadium cell, both the waste of resource had been avoided, it not can cause environmental pollution again, and the electro-chemical activity of regenerating electrolytes and the electrolyte of vanadium redox battery of normal use are almost the same, have reached the requirement reused.
Description
Technical field
The method that the present invention relates to the use of the electrolyte liquid regeneration V electrolyte of failure vanadium cell, belongs to vanadium cell neck
Domain.
Background technique
Vanadium cell has power and capacity big, service life cycle is long, energy because its output power and capacity are mutually indepedent
It is high-efficient, the advantages that depth charge-discharge performance is good, and security performance is high, it is considered to be the most extensive energy storage of one of application prospect
Battery has been to be concerned by more and more people.Can be generated with the charge and discharge of vanadium cell, between positive and negative anodes electrolyte vanadium ion migration,
Divalent vanadium ion oxidation, cathode liberation of hydrogen etc. in electrolyte liquid lead in positive and negative anodes electrolyte the concentration of vanadium ion and valence state not
Match, when requirement when design is not achieved in the utilization rate of electrolyte, needs replacing new V electrolyte.Therefore, it produces
Fail V electrolyte.With the large-scale application of vanadium cell, need to recycle the V electrolyte largely to fail.
Currently, mainly recycle vanadium therein obtains vanadic anhydride or sulfuric acid oxygen to the reuse method of failure V electrolyte
Then vanadic anhydride or vanadic sulfate are further prepared into electrolyte by vanadium.However, this method technics comparing is cumbersome multiple
Miscellaneous, recovery efficiency is low, regenerating electrolytes it is at high cost.
Summary of the invention
The purpose of the present invention is to provide the methods of the electrolyte liquid regeneration V electrolyte using failure vanadium cell, with solution
Certainly existing failure V electrolyte recycles the problem that technique is cumbersome, utilization rate is low.
The present invention provides the methods of the electrolyte liquid regeneration V electrolyte using failure vanadium cell, including walk as follows
It is rapid: vanadic anhydride and H being added into electrolyte liquid2SO4, sufficiently react, be separated by solid-liquid separation, collect liquid phase, be diluted with water, i.e.,
Regenerating electrolytes are obtained, the failure vanadium cell is using sulfuric acid as supporting electrolyte, wherein determines five oxidations two according to following methods
Vanadium, H2SO4With the additional amount of water:
A, vanadium ion concentration C1, vanadium ion average valence M1, sulfate concentration Cs1 in electrolyte liquid are detected；
B, the calculation formula that the amount n1, n1 of substance of vanadic anhydride is added is determined according to the volume V1 of electrolyte liquid
Are as follows: n1=V1*C1* (3.5-M1)/3；
C, the vanadium ion concentration C2 according to needed for regenerating electrolytes determines the volume V2 of regenerating electrolytes:
V2=(V1*C1+2n1)/C2；
D, the sulfate concentration Cs2 according to needed for regenerating electrolytes, which is determined, is added H2SO4Substance amount n2, n2 calculating
Formula are as follows: n2=V2*Cs2-V1*Cs1；
E, water is added and the volume of electrolyte is adjusted to V2.
Further, step a is detected using chemical titration.
Further, reaction temperature is 40~100 DEG C.
Further, reaction temperature is 70~100 DEG C.
Further, the water is deionized water.
The present invention provides the methods of the electrolyte liquid regeneration V electrolyte using failure vanadium cell, mainly have following
Advantage:
1, the rate of recovery of failure vanadium redox battery negative pole electrolyte can achieve 100%, not only avoid the waste of resource, but also will not
It pollutes the environment.
2, the electro-chemical activity of regenerating electrolytes and the electrolyte of vanadium redox battery of normal use are almost the same, and reached makes again
It is required that.
3, present invention process is very simple, easily operated, is suitable for large-scale promotion application.
Detailed description of the invention
Fig. 1 is the cyclic voltammetry curve figure of regenerating electrolytes and original electrolyte in embodiment 1；
Fig. 2 is the discharge capacity of the cell figure of regenerating electrolytes and original electrolyte in embodiment 1；
Fig. 3 is the battery discharging energy figure of regenerating electrolytes and original electrolyte in embodiment 1；
Fig. 4 is the battery efficiency figure of regenerating electrolytes and original electrolyte in embodiment 1.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
The present invention provides the methods of the electrolyte liquid regeneration V electrolyte using failure vanadium cell, mainly by losing
It imitates and vanadic anhydride and H is added in cathode V electrolyte2SO4To regenerate V electrolyte.
The failure of V electrolyte refers to that V electrolyte utilization rate is lower, causes the capacity of battery and energy lower, is not achieved
The phenomenon that setting value, mainly since the valence state of vanadium ion in electrolyte is not achieved caused by requirement.When putting down for vanadium ion
When equal valence state deviates+3.5, V electrolyte can will be reduced using capacity, with the increase of bias, be got over using capacity reduction amount
Greatly, the electro-chemical activity of electrolyte is remarkably decreased at this time.Inventor is detected by the electrolyte liquid to failure vanadium cell
It was found that the vanadium ion in solution mainly will appear following several situations: (1) trivalent vanadium ion；(2) trivalent vanadium ion and tetravalence
Vanadium ion mixing；(3) mixing of trivalent vanadium ion and divalent vanadium ion.For above situation, inventor considers by being added five
V 2 O improves vanadium ion average valence, so that V electrolyte reaches requirement again.
In addition, regeneration method of the present invention is aoxidized primarily directed to using sulfuric acid as the V electrolyte of supporting electrolyte using five
Two vanadium adjust vanadium ion valence state, can avoid the introducing of other impurity components to the full extent, guarantee the purity of V electrolyte,
To improve the electro-chemical activity of regenerating electrolytes as far as possible.
Set regeneration V electrolyte in three tetravalent vanadium ion molar concentration rates be 1: 1, vanadium ion average valence be+3.5.Tool
For body, the present invention determines vanadic anhydride, H according to following methods2SO4With the additional amount of water:
1, the concentration C 1 and average valence M1 of vanadium ion in failure cathode V electrolyte are determined, and is measured in failure electrolyte
Sulfate concentration Cs1；
2, the amount n1 of the substance of vanadic anhydride needed for being determined according to the volume V1 of failure cathode V electrolyte；The calculating of n1
Formula are as follows:
N1=V1*C1* (3.5-M1)/3 (1)
3, the volume V2 of regeneration V electrolyte is calculated in the vanadium ion concentration C2 according to needed for regeneration V electrolyte:
V2=(V1*C1+2n1)/C2 (2)
4, the sulfate concentration Cs2 according to needed for regeneration V electrolyte, is calculated required H2SO4Substance amount n2；N2's
Calculation formula are as follows:
N2=V2*Cs2-V1*Cs1 (3)
5, the desired amount of vanadic anhydride is added into failure electrolyte liquid according to the calculated result of step 2 and step 4
And H2SO4, heating stirring, temperature is controlled at 40~100 DEG C, and after vanadic anhydride in solution sufficiently reacts, filtering obtains three
The filtrate that tetravalent vanadium ion molar concentration rate is 1: 1.
6, three tetravalent vanadium ion molar concentration rates be 1: 1 filtrate in be added water by the volume of solution be adjusted to V2 to get
Regenerate V electrolyte.
Wherein, C1, C2, Cs1, Cs2 are substance withdrawl syndrome.Step 1 preferably uses chemical titration.It is preferably added to
Ionized water.Preferably, reaction temperature is 70~100 DEG C.
Embodiment 1 prepares electrolyte of vanadium redox battery using the method for the present invention
Using chemical titration, measuring vanadium ion concentration in failure cathode V electrolyte is 1.5mol/L, average valence is+
3.2；Measuring sulfate concentration in failure cathode V electrolyte is 4.0mol/L；The volume of failure electrolyte liquid is 20.0L.Again
The vanadium ion concentration of raw electrolyte is 1.6mol/L, sulfate concentration 4.4mol/L.Therefore, it is calculated according to formula (1)
The amount n1 of the substance of required vanadic anhydride is 2.0mol, is according to the volume V2 that formula (2) calculates regenerating electrolytes
22.5L is 19.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (3).Finally according to calculated result, to 20.0L
3.0mol vanadic anhydride and 19.0mol sulfuric acid is added in failure cathode V electrolyte, solution is heated to 85 DEG C and is stirred simultaneously
It mixes, after vanadic anhydride reacts completely, the filtrate that three tetravalent vanadium ion molar concentration rates are 1: 1 is obtained by filtration, then by filtrate
Volume be transferred to 22.5L with deionized water, can be obtained that vanadium ion concentration is 1.6mol/L and sulfate concentration is 4.4mol/L
Regenerating electrolytes.
The electrolyte (original electrolyte) for the vanadium cell for capableing of normal use is taken respectively and regeneration that embodiment 1 obtains is electrolysed
Liquid measures its cyclic voltammetry curve and its battery performance, the result is shown in Figure 1~4.
It will be seen from figure 1 that the cyclic voltammetry curve of regenerating electrolytes and original electrolyte is substantially coincident, illustrate again
The electro-chemical activity of raw electrolyte is substantially consistent with original electrolyte.From figures 2 and 3, it will be seen that with original electrolysis
Liquid phase ratio, the discharge capacity of regenerating electrolytes slightly improve, and discharge energy does not change substantially.From fig. 4, it can be seen that with original
Electrolyte is compared, and the coulombic efficiency of regenerating electrolytes slightly improves, and energy efficiency does not change substantially.Illustrate that regenerating electrolytes reach
To the requirement reused.
Embodiment 2 prepares electrolyte of vanadium redox battery using the method for the present invention
Using chemical titration, measuring vanadium ion concentration in failure cathode V electrolyte is 1.8mol/L, average valence is+
2.8；Measuring sulfate concentration in failure cathode V electrolyte is 3.8mol/L；The volume of failure electrolyte liquid is 20.0L.Again
The vanadium ion concentration of raw electrolyte is 1.6mol/L, sulfate concentration 4.4mol/L.Therefore, it is calculated according to formula (1)
The amount n1 of the substance of required vanadic anhydride is 8.4mol, is according to the volume V2 that formula (2) calculates regenerating electrolytes
34.25L is 67.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (3).Finally according to calculated result, to
8.4mol vanadic anhydride and 67.0mol sulfuric acid is added in 20.0L failure cathode V electrolyte, solution is heated to 90 DEG C simultaneously together
When stir, after vanadic anhydride reacts completely, be obtained by filtration three tetravalent vanadium ion molar concentration rates be 1: 1 filtrate, then will
The volume of filtrate is transferred to 34.25L with deionized water, can be obtained that vanadium ion concentration is 1.6mol/L and sulfate concentration is
The regenerating electrolytes of 4.4mol/L.
Embodiment 3 prepares electrolyte of vanadium redox battery using the method for the present invention
Using chemical titration, measuring vanadium ion concentration in failure cathode V electrolyte is 2.0mol/L, average valence is+
2.9；Measuring sulfate concentration in failure cathode V electrolyte is 3.9mol/L；The volume of failure electrolyte liquid is 30.0L.Again
The vanadium ion concentration of raw electrolyte is 1.6mol/L, sulfate concentration 4.3mol/L.Therefore, it is calculated according to formula (1)
The amount n1 of the substance of required vanadic anhydride is 12.0mol, is according to the volume V2 that formula (2) calculates regenerating electrolytes
52.5L is 108.75mol according to the amount that the substance of required sulfuric acid is calculated in formula (3).Finally according to calculated result, to
12.0mol vanadic anhydride and 108.75mol sulfuric acid is added in 30.0L failure cathode V electrolyte, solution is heated to 80 DEG C
And stir simultaneously, after vanadic anhydride reacts completely, the filtrate that three tetravalent vanadium ion molar concentration rates are 1: 1 is obtained by filtration,
The volume of filtrate is transferred to 52.5L with deionized water again, can be obtained that vanadium ion concentration is 1.6mol/L and sulfate concentration is
The regenerating electrolytes of 4.3mol/L.
Embodiment 4 prepares electrolyte of vanadium redox battery using the method for the present invention
Using chemical titration, measuring vanadium ion concentration in failure cathode V electrolyte is 1.4mol/L, average valence is+
2.8；Measuring sulfate concentration in failure cathode V electrolyte is 4.4mol/L；The volume of failure electrolyte liquid is 30.0L.Again
The vanadium ion concentration of raw electrolyte is 1.6mol/L, sulfate concentration 4.3mol/L.Therefore, it is calculated according to formula (1)
The amount n1 of the substance of required vanadic anhydride is 9.8mol, is according to the volume V2 that formula (2) calculates regenerating electrolytes
38.5L is 67.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (3).Finally according to calculated result, to 30.0L
8.4mol vanadic anhydride and 33.55mol sulfuric acid is added in failure cathode V electrolyte, solution is heated to 90 DEG C and is stirred simultaneously
It mixes, after vanadic anhydride reacts completely, the filtrate that three tetravalent vanadium ion molar concentration rates are 1: 1 is obtained by filtration, then by filtrate
Volume be transferred to 38.5L with deionized water, can be obtained that vanadium ion concentration is 1.6mol/L and sulfate concentration is 4.3mol/L
Regenerating electrolytes.
Claims (5)
1. the method for the electrolyte liquid regeneration V electrolyte using failure vanadium cell, it is characterized in that: including the following steps: to negative
Vanadic anhydride and H are added in the electrolyte of pole2SO4, sufficiently react, be separated by solid-liquid separation, collect liquid phase, be diluted with water to get regeneration electricity
Liquid is solved, the failure vanadium cell is using sulfuric acid as supporting electrolyte, wherein determines vanadic anhydride, H according to following methods2SO4With
The additional amount of water:
A, vanadium ion concentration C1, vanadium ion average valence M1, sulfate concentration Cs1 in electrolyte liquid are detected；
B, the calculation formula that the amount n1, n1 of substance of vanadic anhydride is added is determined according to the volume V1 of electrolyte liquid are as follows: n1=
V1*C1*(3.5-M1)/3；
C, the vanadium ion concentration C2 according to needed for regenerating electrolytes determine the volume V2:V2=(V1*C1+2n1) of regenerating electrolytes/
C2；
D, the sulfate concentration Cs2 according to needed for regenerating electrolytes, which is determined, is added H2SO4Substance amount n2, n2 calculation formula
Are as follows: n2=V2*Cs2-V1*Cs1；
E, water is added and the volume of electrolyte is adjusted to V2.
2. the method for regeneration V electrolyte as described in claim 1, it is characterized in that: step a is detected using chemical titration.
3. the method for regeneration V electrolyte as described in claim 1, it is characterized in that: reaction temperature is 40~100 DEG C.
4. the method for regeneration V electrolyte as described in claim 1, it is characterized in that: reaction temperature is 70~100 DEG C.
5. regeneration method as described in claim 1, it is characterized in that: the water is deionized water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111509247A (en) * | 2020-04-03 | 2020-08-07 | 武汉科技大学 | Method for regenerating electrolyte of failure vanadium battery |
| CN112993361A (en) * | 2019-12-17 | 2021-06-18 | 江苏泛宇能源有限公司 | Preparation method of vanadium electrolyte |
| CN116914171A (en) * | 2023-09-05 | 2023-10-20 | 南阳汉鼎高新材料有限公司 | Recycling method of failure vanadium battery electrolyte |
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| CN106410250A (en) * | 2016-11-11 | 2017-02-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling ineffective electrolyte of vanadium redox battery |
| CN106450371A (en) * | 2016-11-11 | 2017-02-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling failed vanadium electrolyte |
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2018
- 2018-10-30 CN CN201811279104.5A patent/CN109461948A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106340657A (en) * | 2016-11-11 | 2017-01-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium electrolytic solution |
| CN106410250A (en) * | 2016-11-11 | 2017-02-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling ineffective electrolyte of vanadium redox battery |
| CN106450371A (en) * | 2016-11-11 | 2017-02-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling failed vanadium electrolyte |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112993361A (en) * | 2019-12-17 | 2021-06-18 | 江苏泛宇能源有限公司 | Preparation method of vanadium electrolyte |
| CN112993361B (en) * | 2019-12-17 | 2022-06-17 | 江苏泛宇能源有限公司 | Preparation method of vanadium electrolyte |
| CN111509247A (en) * | 2020-04-03 | 2020-08-07 | 武汉科技大学 | Method for regenerating electrolyte of failure vanadium battery |
| CN116914171A (en) * | 2023-09-05 | 2023-10-20 | 南阳汉鼎高新材料有限公司 | Recycling method of failure vanadium battery electrolyte |
| CN116914171B (en) * | 2023-09-05 | 2024-03-12 | 南阳汉鼎高新材料有限公司 | Recycling method of failure vanadium battery electrolyte |
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