CN115418653A - Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction - Google Patents

Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction Download PDF

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CN115418653A
CN115418653A CN202211113675.8A CN202211113675A CN115418653A CN 115418653 A CN115418653 A CN 115418653A CN 202211113675 A CN202211113675 A CN 202211113675A CN 115418653 A CN115418653 A CN 115418653A
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solution
electrolysis
reaction
vanadium
preparing
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张东彬
滕艾均
代宇
刘天豪
尹翔鹭
彭显著
曾泽华
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Ansteel Beijing Research Institute
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/50—Processes
    • 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
    • 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
    • H01M2300/0088—Composites
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    • 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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Abstract

The invention provides a method for preparing vanadium battery electrolyte by coupled reaction electrolysis, which comprises the following steps: step 1: weighing high-valence vanadium sulfuric acid solution to prepare solution A with the vanadium ion concentration of 1-5 mol/L under the condition of continuous stirring; step 2: preparing a sulfuric acid solution with the same concentration as the solution A, and adding a corresponding reaction substrate according to the type of the coupling reaction to prepare a solution B; and step 3: the prepared solution A is used as a cathode electrolyte, the solution B is used as an anode electrolyte, a Nafion membrane is used as a proton exchange membrane, and the solution A is prepared by electrolysis under an inert electrode material. Half reactions such as urea oxidation, methanol/ethanol oxidation, hydroxylamine oxidation and the like with low reaction electrode potential and low reaction energy barrier are used for replacing acid OER half reactions in the process of preparing the vanadium electrolyte by the traditional electrolytic method, so that the voltage value required in the whole electrolytic reaction process is reduced, the energy barrier in the electrolytic process is reduced, and the purpose of saving cost is achieved.

Description

Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction
Technical Field
The invention relates to the technical field of electrolyte, in particular to a method for preparing vanadium battery electrolyte by utilizing coupled reaction electrolysis.
Background
The electrolyte is an important component of the vanadium battery, and not only can be used as conductor ions but also can be used as an energy storage medium, so that the development of the vanadium battery electrolyte with low cost and high performance plays an important role in promoting the development of the vanadium battery industry and improving the energy storage performance of the vanadium battery. At present, the preparation method of the vanadium battery electrolyte mainly comprises a chemical reduction method and an electrolysis method. Wherein, the chemical reduction method mainly utilizes reducing substances such as oxalic acid and the like to reduce a pentavalent vanadium source for preparation; the electrolytic reduction method is to dissolve pentavalent vanadium source in sulfuric acid and reduce the solution into quadrivalent or tri-quadrivalent mixed electrolyte at cathode. The Chinese patent with publication number CN103490086 discloses a method for preparing 3.5-valent electrolyte by an electrolytic method. Meanwhile, the research result of the Chinese invention patent CN104577173 shows that the concentration of vanadium ions in the electrolyte prepared by the electrolytic method can be higher than that of the electrolyte prepared by the chemical method, and the electrical property is better, namely, the electrolyte prepared by the electrolytic method is more suitable for the requirements of vanadium batteries. However, in the case of the existing electrolytic processes, V occurs in the cathodic compartment 5+ To V 3+ /V 4+ To obtain an electrolyte, the anodic compartment then undergoing an oxygen evolution reaction (OER, 2H) in an acidic system (sulfuric acid) 2 O-4e - ＝4H + +O 2 ×) in the table ×. Since the OER reaction is a reaction involving four electrons, the reaction electrode has high potential, high reaction energy barrier and slow reaction rate, and higher voltage is required to initiate OER and V 5+ The reduction reaction of (2) causes a large energy consumption required in the electrolyte preparation process and an increase in the preparation cost. Therefore, there is an urgent need to develop a vanadium battery electrolyte with easier reaction and lower costA novel method for preparing liquid electrolysis.
Disclosure of Invention
In order to solve the technical problems provided by the background art, the invention provides a method for preparing vanadium battery electrolyte by coupled reaction electrolysis, which utilizes half reactions with low reaction energy barrier and low reaction electrode potential, such as urea oxidation (UOR, thermodynamic overpotential is 0.37V, which is about 0.9V lower than OER), methanol/ethanol oxidation, hydroxylamine oxidation and the like to replace acidic OER half reactions in the process of preparing vanadium electrolyte by the traditional electrolysis method, thereby reducing the required voltage value in the whole electrolysis reaction process, reducing the energy barrier in the electrolysis process and achieving the purpose of saving cost. The method has the advantages of low energy consumption, high efficiency, strong operability and the like, is favorable for further optimizing the electrolytic preparation process route of the vanadium battery electrolyte, and promotes the further development of the vanadium battery electrolyte industry.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing vanadium battery electrolyte by coupled reaction electrolysis comprises the following steps:
step 1: weighing a high-valence vanadium sulfuric acid solution with a set amount under the condition of continuous stirring to prepare an A solution with the vanadium ion concentration of 1-5 mol/L and the sulfuric acid concentration of 1-6 mol/L;
step 2: preparing a sulfuric acid solution with the same concentration as the solution A, and adding a corresponding reaction substrate according to the type of the coupling reaction to prepare a solution B;
adding a urine-containing substance when coupling UOR half reaction, adding an organic alcohol when coupling alcohol oxidation half reaction, and adding a hydroxylamine compound when coupling hydroxylamine oxidation half reaction;
and step 3: the prepared solution A is used as a catholyte, the solution B is used as an anolyte, a Nafion membrane is used as a proton exchange membrane, and the solution A is prepared by electrolysis under an inert electrode material.
Further, in the step 1, the high valence vanadium sulfuric acid solution is V with a set weight 2 O 5 Dissolved in sulfuric acid solution or waste high-valence vanadium electrolyte.
Further, in the step 2, the urine-containing substance is one or more of urea, hexamethylene tetramine, or urine.
Further, in the step 2, the organic alcohol is one or more of methanol and ethanol.
Further, in the step 2, the hydroxylamine compound is hydroxylamine hydrochloride or hydroxylamine sulfate.
Further, in the step 2, the concentration of the added reaction substrate is 0.5-3 mol/L.
Further, in the step 3, the inert electrode is one of a titanium mesh, a platinum mesh and a graphite sheet/rod.
Furthermore, in the step 3, the electrolysis mode is constant voltage or constant current electrolysis, the current is 0.1-5A, the voltage is 1-5V, and the electrolysis end point is 1-1.5 times of the theoretical electric quantity.
Compared with the prior art, the invention has the beneficial effects that:
1) According to the method for preparing the vanadium battery electrolyte by utilizing the coupled reaction electrolysis, the anode half reaction with lower electrode potential is utilized to couple the cathode high-valence (pentavalent) vanadium reduction reaction, so that the reaction energy barrier of the electrolysis full reaction is reduced, the voltage value required by the full reaction process is reduced, and the purpose of reducing energy consumption is achieved. The electrolyte prepared by the method has higher concentration and electrochemical performance, and can be used as the electrolyte of a vanadium flow battery.
2) On the basis of keeping the original equipment for preparing vanadium battery electrolyte by an electrolytic method, the method of the invention improves the efficiency of electrolytic reduction of high-valence vanadium ions by coupling the anode half-reaction with low energy barrier. By coupling half reactions such as UOR, alcohol electrooxidation, hydroxylamine oxidation and the like, the full electrolysis reaction potential is reduced, the energy consumption in the electrolyte preparation process is reduced, and the purpose of energy conservation is achieved.
3) The preparation method of the electrolyte has the advantages of simple operation, high efficiency and strong popularization, the prepared electrolyte has good electrochemical performance, the limitations of high energy consumption and the like of the vanadium battery electrolyte prepared by the existing electrolytic method can be greatly improved, and the further development of the vanadium battery and the vanadium battery electrolyte industry can be promoted.
Drawings
FIG. 1 is a plot of linear voltammetric scans (LSV) during preparation according to the methods of the present invention example 1 (plot a) and comparative example 1 (plot b);
FIG. 2 is a constant current electrolysis curve during the preparation of the method of example 1 (curve a) and comparative example 1 (curve b) according to the present invention;
FIG. 3 shows UV-VIS absorption spectrum test of electrolytes (positive 4-valent) prepared by the methods of example 1 (curve a) and comparative example 1 (curve b) according to the present invention;
FIG. 4 is a plot of the linear voltammetric sweep (LSV) during preparation according to the methods of the present invention example 2 (plot a) and comparative example 1 (plot b);
FIG. 5 is a plot of the linear voltammetric scan (LSV) during preparation according to the methods of the present invention example 3 (plot a) and comparative example 1 (plot b).
Detailed Description
The following detailed description of the present invention is provided in connection with the accompanying drawings.
The method for preparing the vanadium battery electrolyte by utilizing the coupling reaction electrolysis specifically comprises the step of coupling the reduction reaction of cathode high-valence vanadium (pentavalent vanadium) by utilizing anode half reaction with lower electrode potential, so that the voltage value required by the whole reaction process is reduced, and the purpose of reducing energy consumption is achieved. Potential E = E due to electrolytic reaction Yang (Yang) +E Yin (kidney) +η，E Yang (Yang) To anodic potential, E Yin (kidney) At cathodic potential and eta at overpotential for reaction, by selecting appropriate E Yang (Yang) The minimization of E can be achieved. The method has the characteristics of simple operation, low energy consumption and high universality. The electrolyte prepared by the method has higher concentration and electrochemical performance, and can be used as the electrolyte of a vanadium flow battery.
The method for preparing the vanadium battery electrolyte by utilizing the coupled reaction electrolysis comprises the following specific steps:
1) Weighing a set amount of high-valence vanadium (pentavalent vanadium) sulfuric acid solution under the condition of continuous stirring to prepare a solution with the vanadium ion concentration of 1-5 mol/L,The concentration of the sulfuric acid is 1 to 6mol/L. The high-valence vanadium sulfuric acid solution can be weighed to set the mass V 2 O 5 Dissolved in sulfuric acid solution or used as waste high-valence vanadium electrolyte.
2) Preparing a sulfuric acid solution with the same concentration as the solution A, and adding a corresponding reaction substrate according to the type of the coupling reaction to prepare a solution B. In particular, when coupling UOR half reaction, adding urea, hexamethylene tetramine, or urine containing substances; when coupling alcohol oxidation half reaction, adding organic alcohol such as methanol and ethanol; when coupling hydroxylamine oxidation half reaction, hydroxylamine hydrochloride, hydroxylamine sulfate and other hydroxylamine compounds are added. The concentration of the added reaction substrate is 0.5-3 mol/L.
3) The prepared solution A is used as a catholyte, the solution B is used as an anolyte, a Nafion membrane is used as a proton exchange membrane, and the solution A is prepared by electrolysis under inert electrode materials. The inert electrode is a titanium mesh, a platinum mesh, a graphite flake/bar and the like, the electrolysis mode is constant voltage or constant current electrolysis, the current is 0.1-5A, the voltage is 1-5V, and the electrolysis end point is 1-1.5 times of the theoretical electric quantity.
Example 1
1) 30mL1.6mol/L of pentavalent vanadium battery electrolyte (the concentration of sulfuric acid is 1.6 mol/L) is weighed as the solution A.
2) 3.34g of hydroxylamine hydrochloride is weighed and quickly added into 1.6mol/L sulfuric acid solution, and the solution is continuously stirred until the solution is completely dissolved, so that 30mL1.6mol/L hydroxylamine hydrochloride-sulfuric acid solution is prepared, and the solution B can be obtained.
3) In the electrolytic cell, a carbon rod is used as a cathode and anode electrolytic electrode, the solution A is used as a cathode cell solution, the solution B is used as an anode cell solution, and a Nafion proton exchange membrane is used as a diaphragm to carry out electrolytic reaction.
4) And carrying out constant current electrolysis at the current of 0.1A, wherein the electrolysis end point is 1.1 times of the theoretical electric quantity, and the cathode tank solution after electrolysis is the corresponding vanadium battery electrolyte.
Example 2
1) Weighing 8.74gV 2 O 5 The solution was dissolved in sulfuric acid at a concentration of 1.6mol/L to prepare 30mL1.6mol/L pentavalent vanadium sulfuric acid solution as solution A.
2) 2.88g of urea is weighed and quickly added into 1.6mol/L sulfuric acid solution, and is continuously stirred until the urea is completely dissolved, 30mL1.6mol/L urea-sulfuric acid solution is prepared, and then the B solution can be obtained.
3) In the electrolytic bath, a titanium mesh is used as a cathode and anode electrolytic electrode, the solution A is used as a cathode bath solution, the solution B is used as an anode bath solution, and a Nafion proton exchange membrane is used as a diaphragm, so that the electrolytic reaction is carried out.
4) And carrying out constant current electrolysis at the voltage of 3V, wherein the electrolysis end point is 1.5 times of the theoretical electric quantity, and the cathode bath solution is the corresponding vanadium battery electrolyte after electrolysis.
Example 3
1) 30mL1.6mol/L of pentavalent vanadium battery electrolyte (the concentration of sulfuric acid is 1.6 mol/L) is weighed as the solution A.
2) Weighing 4mL of absolute ethyl alcohol, adding the absolute ethyl alcohol into 1.6mol/L sulfuric acid solution, and preparing 30mL2.29mol/L ethanol-sulfuric acid solution to obtain solution B.
3) In the electrolytic cell, a carbon rod is used as a cathode and anode electrolytic electrode, the solution A is used as a cathode cell solution, the solution B is used as an anode cell solution, and a Nafion proton exchange membrane is used as a diaphragm to carry out electrolytic reaction.
4) And carrying out constant current electrolysis at the current of 0.1A, wherein the electrolysis end point is 1.3 times of the theoretical electric quantity, and the cathode tank solution after electrolysis is the corresponding vanadium battery electrolyte.
Comparative example 1
1) 30mL1.6mol/L of pentavalent vanadium battery electrolyte (the concentration of sulfuric acid is 1.6 mol/L) is weighed as the solution A.
2) A30mL1.6mol/L sulfuric acid solution was prepared as the B solution.
3) In the electrolytic cell, a carbon rod is used as a cathode and anode electrolytic electrode, the solution A is used as a cathode cell solution, the solution B is used as an anode cell solution, and a Nafion proton exchange membrane is used as a diaphragm to carry out electrolytic reaction.
4) And carrying out constant current electrolysis at the current of 0.1A, wherein the electrolysis end point is 1.1 times of the theoretical electric quantity, and the cathode tank solution after electrolysis is the corresponding vanadium battery electrolyte.
FIG. 1 is a plot of linear voltammetric scans (LSV) during preparation according to the methods of the present invention example 1 (plot a) and comparative example 1 (plot b); as can be seen from fig. 1, the method of example 1 has a larger current at the same potential, indicating better electrolytic performance, compared to comparative example 1.
FIG. 2 is a constant current electrolysis curve during the preparation of the method of example 1 (curve a) and comparative example 1 (curve b) according to the present invention; as can be seen from FIG. 2, the voltage value required by the method of example 1 under the condition of 0.1A current is only 2.3V, and compared with 2.8V required by comparative example 1, the energy consumption is expected to be saved by 18%.
FIG. 3 shows UV-VIS absorption spectrum test of electrolytes (positive 4-valent) prepared by the methods of example 1 (curve a) and comparative example 1 (curve b) according to the present invention; as can be seen from fig. 3, the uv-vis absorption spectra curves of the electrolytes obtained in example 1 and comparative example 1 are similar, both show the characteristic absorption peak of typical vanadium valence 4, and the corresponding peak intensities and peak areas are equivalent, which indicates that the electrolyte states after electrolysis are substantially the same, and the result further indicates that the electrolysis efficiency is higher by using the method of example 1.
FIG. 4 is a plot of the linear voltammetric sweep (LSV) during preparation according to the methods of the present invention example 2 (plot a) and comparative example 1 (plot b); as can be seen from fig. 4, the method of example 2 has a larger electrolytic current at the same potential, indicating better electrolytic performance, compared to comparative example 1.
FIG. 5 is a plot of the linear voltammetric sweep (LSV) during preparation according to the method of the present invention in example 3 (curve a) and comparative example 1 (curve b); as can be seen from fig. 5, the method of example 3 has a larger electrolytic current at the same potential, indicating better electrolytic performance, compared to comparative example 1.
The above embodiments are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the above embodiments. The methods used in the above examples are conventional methods unless otherwise specified.

Claims (9)

1. A method for preparing vanadium battery electrolyte by coupled reaction electrolysis is characterized by comprising the following steps:
step 1: weighing a set amount of high-valence vanadium sulfuric acid solution under the condition of continuous stirring to prepare solution A with the vanadium ion concentration of 1-5 mol/L;
and 2, step: preparing a sulfuric acid solution with the same concentration as the solution A, and adding a corresponding reaction substrate according to the type of the coupling reaction to prepare a solution B;
adding a urine-containing substance when coupling UOR half reaction, adding an organic alcohol when coupling alcohol oxidation half reaction, and adding a hydroxylamine compound when coupling hydroxylamine oxidation half reaction;
and step 3: the prepared solution A is used as a catholyte, the solution B is used as an anolyte, a Nafion membrane is used as a proton exchange membrane, and the solution A is prepared by electrolysis under an inert electrode material.
2. The method for preparing the vanadium redox battery electrolyte by electrolysis through the coupling reaction according to claim 1, wherein in the step 1, the sulfuric acid concentration in the solution A is 1-6 mol/L.
3. The method for preparing the vanadium redox battery electrolyte by coupled reaction electrolysis as claimed in claim 1, wherein in the step 1, the high valence vanadium sulfuric acid solution is V with a set weight 2 O 5 Dissolved in sulfuric acid solution or waste high-valence vanadium electrolyte.
4. The method for preparing the vanadium redox battery electrolyte by using the coupled reaction electrolysis as claimed in claim 1, wherein in the step 2, the urine-containing substance is one or more of urea, hexamethylenetetramine or urine.
5. The method for preparing the vanadium redox battery electrolyte by coupling reaction electrolysis according to claim 1, wherein in the step 2, the organic alcohol is one or more of methanol and ethanol.
6. The method for preparing the vanadium redox battery electrolyte by electrolysis through a coupling reaction according to claim 1, wherein in the step 2, the hydroxylamine compound is hydroxylamine hydrochloride or hydroxylamine sulfate.
7. The method for preparing the vanadium battery electrolyte by electrolysis through the coupling reaction according to claim 1, wherein in the step 2, the concentration of the added reaction substrate is 0.5-3 mol/L.
8. The method for preparing the vanadium battery electrolyte by electrolysis through a coupling reaction according to claim 1, wherein in the step 3, the inert electrode is one of a titanium mesh, a platinum mesh and a graphite sheet/rod.
9. The method for preparing the vanadium redox battery electrolyte by coupled reaction electrolysis as claimed in claim 1, wherein in the step 3, the electrolysis mode is constant voltage or constant current electrolysis, the current is 0.1-5A, the voltage is 1-5V, and the electrolysis end point is 1-1.5 times of the theoretical electric quantity.
CN202211113675.8A 2022-09-14 2022-09-14 Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction Pending CN115418653A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115992357A (en) * 2023-02-13 2023-04-21 华秦储能技术有限公司 Preparation method of electrolyte of all-vanadium redox flow battery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115992357A (en) * 2023-02-13 2023-04-21 华秦储能技术有限公司 Preparation method of electrolyte of all-vanadium redox flow battery

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