CN109449470A - Utilize the method for sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte - Google Patents
Utilize the method for sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte Download PDFInfo
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- CN109449470A CN109449470A CN201811279118.7A CN201811279118A CN109449470A CN 109449470 A CN109449470 A CN 109449470A CN 201811279118 A CN201811279118 A CN 201811279118A CN 109449470 A CN109449470 A CN 109449470A
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- sulfuric acid
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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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- 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
Abstract
The method that the present invention relates to the use of sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte, 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 using sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte includes the following steps: that VOSO is added into electrolyte liquid4Aqueous solution, H2SO4With water to get regenerating electrolytes, the 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 sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte, belongs to vanadium electricity
Pond field.
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 sides using sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte
Method, to solve the problems, such as that existing failure V electrolyte recycling technique is cumbersome, utilization rate is low.
The present invention provides the methods using sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte, including such as
Lower step: VOSO is added into electrolyte liquid4Aqueous solution, H2SO4With water to get regenerating electrolytes, the vanadium cell is with sulfuric acid
For supporting electrolyte, wherein determine VOSO according to following methods4Aqueous solution, 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, VOSO needed for being determined according to the volume V1 of electrolyte liquid4Substance amount n1, n1 calculation formula are as follows: n1=
2*V1*C1*(3.5-M1)；
C, according to required VOSO4Substance amount and the VOSO4The vanadium ion concentration C0 of aqueous solution, which is determined, is added VOSO4
The volume V0:V0=n1/C0 of aqueous solution；
D, the vanadium ion concentration C2 according to needed for regeneration V electrolyte determines the volume V2:V2=(V1* of regeneration V electrolyte
C1+n1)/C2；
E, the sulfate concentration Cs2 according to needed for regeneration V electrolyte, which is determined, is added H2SO4Substance amount n2, n2 meter
Calculate formula are as follows: n2=V2*Cs2-V1*Cs1-n1；
F, water is added and the volume of electrolyte is adjusted to V2.
Further, step a is detected using chemical titration.
Further, the VOSO4The vanadium ion concentration C0 of aqueous solution is 0.1~8.0mol/L.
Wherein, work as VOSO4When vanadium ion concentration is lower than 0.1mol/L in aqueous solution, when regeneration, needs to be added a large amount of VOSO4Water
Solution, then re-evaporation moisture can be only achieved regenerated vanadium ion concentration requirement, not only make complicated for operationization, but also will lead to again
The cost of raw V electrolyte increases.
Further, the water is deionized water.
It is main to have the present invention provides the method using sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte
There is 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.
It is main logical the present invention provides the method using sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte
It crosses and tetravalence oxygen vanadium sulphate solution and H is added in failure 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 four
Valence oxygen vanadium sulphate solution improves vanadium ion average valence, so that V electrolyte reaches requirement again.
In addition, regeneration method of the present invention is primarily directed to using sulfuric acid as the V electrolyte of supporting electrolyte, using sulfuric acid oxygen
Vanadium solution adjusts vanadium ion valence state, can avoid the introducing of other impurity components to the full extent, guarantee the pure of V electrolyte
Degree, to improve the electro-chemical activity of regenerating electrolytes as far as possible.
Setting three tetravalent vanadium ion molar concentration rates in regeneration V electrolyte, as 1:1, vanadium ion average valence is+3.5.Tool
For body, the present invention determines VOSO according to following methods4Aqueous solution, H2SO4With 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, vanadic sulfate (VOSO needed for being determined according to the volume V1 of failure cathode V electrolyte4) substance amount n1；n1
Calculation formula are as follows:
N1=2*V1*C1* (3.5-M1) (1)
3, according to required vanadic sulfate (VOSO4) substance amount and the VOSO4The vanadium ion concentration C0 of aqueous solution is determined
The volume V0 of tetravalence oxygen vanadium sulphate solution is added:
V0=n1/C0 (2)
4, 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+n1)/C2 (3)
5, 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-n1 (4)
6, the desired amount of tetravalence sulfuric acid oxygen is added into failure electrolyte liquid according to the calculated result of step 3 and step 5
Vanadium solution, H2SO4With water (volume of solution is adjusted to V2) to get regeneration 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, vanadium ion concentration C0 is 0.1~8.0mol/L in tetravalence vanadic sulfate aqueous solution.
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+
3.4；Measuring sulfate concentration in failure cathode V electrolyte is 4.3mol/L；The volume of failure electrolyte liquid is 20.0L.Four
Vanadium ion concentration is 4.0mol/L in valence oxygen vanadium sulphate solution.The vanadium ion concentration of regenerating electrolytes is 1.6mol/L, sulfate radical
Concentration is 4.4mol/L.Therefore, the amount n1 that the substance of required vanadic sulfate is calculated according to formula (1) is 6.0mol, according to
The volume that formula (2) calculates required 4.0mol/L tetravalence oxygen vanadium sulphate solution is 1.5L, calculates regeneration electricity according to formula (3)
The volume V2 for solving liquid is 22.5L, is 7.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (4).Finally according to meter
It calculates as a result, the tetravalence vanadic sulfate that addition 1.5L vanadium ion concentration is 4.0mol/L into 20.0L failure cathode V electrolyte is molten
Liquid and 7.0mol sulfuric acid, then the volume of solution is transferred to 22.5L with deionized water, it is 1.6mol/L that vanadium ion concentration, which can be obtained,
The regenerating electrolytes for being 4.4mol/L with sulfate concentration.
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 and discharge energy of regenerating electrolytes slightly improve.From fig. 4, it can be seen that compared with original electrolyte,
The coulombic efficiency of regenerating electrolytes slightly improves, and energy efficiency does not change substantially.Illustrate that regenerating electrolytes reach to reuse
Requirement.
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 1.5mol/L, average valence is+
2.8；Measuring sulfate concentration in failure cathode V electrolyte is 4.0mol/L；The volume of failure electrolyte liquid is 20.0L.Four
Vanadium ion concentration is 6.0mol/L in valence oxygen vanadium sulphate solution.The vanadium ion concentration of regenerating electrolytes is 1.6mol/L, sulfate radical
Concentration is 4.4mol/L.Therefore, the amount n1 that the substance of required vanadic sulfate is calculated according to formula (1) is 42.0mol, according to
The volume that formula (2) calculates required 6.0mol/L tetravalence sulfate sulfatase vanadyl solution is 7.0L, is calculated again according to formula (3)
The volume V2 of raw electrolyte is 45.0L, is 76.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (4).Last root
According to calculated result, the tetravalence sulfuric acid oxygen that 7.0L vanadium ion concentration is 6.0mol/L is added into 20.0L failure cathode V electrolyte
Vanadium solution and 76.0mol sulfuric acid, then the volume of solution is transferred to 45.0L with deionized water, vanadium ion concentration, which can be obtained, is
The regenerating electrolytes that 1.6mol/L and sulfate concentration are 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+
3.2；Measuring sulfate concentration in failure cathode V electrolyte is 4.1mol/L；The volume of failure electrolyte liquid is 20.0L.Four
Vanadium ion concentration is 1.5mol/L in valence oxygen vanadium sulphate solution.The vanadium ion concentration of regenerating electrolytes is 1.6mol/L, sulfate radical
Concentration is 4.3mol/L.Therefore, the amount n1 that the substance of required vanadic sulfate is calculated according to formula (1) is 24.0mol, according to
The volume that formula (2) calculates required 1.5mol/L tetravalence sulfate sulfatase vanadyl solution is 16.0L, is calculated according to formula (3)
The volume V2 of regenerating electrolytes is 40.0L, is 66.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (4).Finally
According to calculated result, the tetravalence sulfuric acid that 16.0L vanadium ion concentration is 1.5mol/L is added into 20.0L failure cathode V electrolyte
Vanadyl solution and 66.0mol sulfuric acid, then the volume of solution is transferred to 40.0L with deionized water, vanadium ion concentration, which can be obtained, is
The regenerating electrolytes that 1.6mol/L and sulfate concentration are 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 2.0mol/L, average valence is+
2.5；Measuring sulfate concentration in failure cathode V electrolyte is 4.1mol/L；The volume of failure electrolyte liquid is 20.0L.Four
Vanadium ion concentration is 2.0mol/L in valence oxygen vanadium sulphate solution.The vanadium ion concentration of regenerating electrolytes is 1.5mol/L, sulfate radical
Concentration is 4.3mol/L.Therefore, the amount n1 that the substance of required vanadic sulfate is calculated according to formula (1) is 80.0mol, according to
The volume that formula (2) calculates required 2.0mol/L tetravalence sulfate sulfatase vanadyl solution is 40.0L, is calculated according to formula (3)
The volume V2 of regenerating electrolytes is 80.0L, is 182.0mol according to the amount that the substance of required sulfuric acid is calculated in formula (4).Most
Afterwards according to calculated result, the tetravalence sulphur that 40.0L vanadium ion concentration is 2.0mol/L is added into 20.0L failure cathode V electrolyte
Sour vanadyl solution and 182.0mol sulfuric acid, then the volume of solution is transferred to 80.0L with deionized water, vanadium ion concentration can be obtained
The regenerating electrolytes for being 4.3mol/L for 1.5mol/L and sulfate concentration.
Embodiment 5 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+
3.4；Measuring sulfate concentration in failure cathode V electrolyte is 4.1mol/L；The volume of failure electrolyte liquid is 20.0L.Four
Vanadium ion concentration is 2.0mol/L in valence oxygen vanadium sulphate solution.The vanadium ion concentration of regenerating electrolytes is 1.6mol/L, sulfate radical
Concentration is 4.3mol/L.Therefore, the amount n1 that the substance of required vanadic sulfate is calculated according to formula (1) is 7.2mol, according to
The volume that formula (2) calculates required 2.0mol/L tetravalence sulfate sulfatase vanadyl solution is 3.6L, is calculated again according to formula (3)
The volume V2 of raw electrolyte is 27.0L, is 26.9mol according to the amount that the substance of required sulfuric acid is calculated in formula (4).Last root
According to calculated result, the tetravalence sulfuric acid oxygen that 3.6L vanadium ion concentration is 2.0mol/L is added into 20.0L failure cathode V electrolyte
Vanadium solution and 26.9mol sulfuric acid, then the volume of solution is transferred to 27.0L with deionized water, vanadium ion concentration, which can be obtained, is
The regenerating electrolytes that 1.6mol/L and sulfate concentration are 4.3mol/L.
Claims (4)
1. using the method for sulfuric acid system vanadium cell failure electrolyte liquid regeneration V electrolyte, it is characterized in that: including following step
It is rapid: VOSO is added into electrolyte liquid4Aqueous solution, H2SO4With water to get regenerating electrolytes, the vanadium cell is branch with sulfuric acid
Hold electrolyte, wherein determine VOSO according to following methods4Aqueous solution, 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, VOSO needed for being determined according to the volume V1 of electrolyte liquid4Substance amount n1, n1 calculation formula are as follows: n1=2*V1*
C1*(3.5-M1)；
C, according to required VOSO4Substance amount and the VOSO4The vanadium ion concentration C0 of aqueous solution, which is determined, is added VOSO4It is water-soluble
The volume V0:V0=n1/C0 of liquid；
D, the vanadium ion concentration C2 according to needed for regeneration V electrolyte determines the volume V2:V2=(V1*C1+ of regeneration V electrolyte
n1)/C2；
E, the sulfate concentration Cs2 according to needed for regeneration V electrolyte, which is determined, is added H2SO4Substance amount n2, n2 calculating it is public
Formula are as follows: n2=V2*Cs2-V1*Cs1-n1；
F, 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: the VOSO4The vanadium ion concentration C0 of aqueous solution
For 0.1~8.0mol/L.
4. regeneration method as described in claim 1, it is characterized in that: the water is deionized water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113964358A (en) * | 2021-11-06 | 2022-01-21 | 江西钒业科技有限公司 | Novel method for preparing vanadyl sulfate electrolyte by using vanadium coal mine |
| CN116130692A (en) * | 2023-02-28 | 2023-05-16 | 安徽海螺洁能科技有限公司 | Recycling method of waste 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
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Patent Citations (3)
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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 |
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| 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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| CN113964358A (en) * | 2021-11-06 | 2022-01-21 | 江西钒业科技有限公司 | Novel method for preparing vanadyl sulfate electrolyte by using vanadium coal mine |
| CN116130692A (en) * | 2023-02-28 | 2023-05-16 | 安徽海螺洁能科技有限公司 | Recycling method of waste vanadium battery electrolyte |
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