CN114807957A - Vanadium solution valence state rapid regulation and control method based on high-current pulse technology - Google Patents

Vanadium solution valence state rapid regulation and control method based on high-current pulse technology Download PDF

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CN114807957A
CN114807957A CN202210464258.1A CN202210464258A CN114807957A CN 114807957 A CN114807957 A CN 114807957A CN 202210464258 A CN202210464258 A CN 202210464258A CN 114807957 A CN114807957 A CN 114807957A
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vanadium
valence state
electrode
current pulse
electrolyte
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蒲年文
赵锋
任华彬
刘磊
张忠裕
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Sichuan Xingming Energy Environmental Protection Technology Co ltd
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    • C25B9/60—Constructional parts of cells
    • C25B9/65—Means for supplying current; Electrode connections; Electric inter-cell connections
    • 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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Abstract

The invention discloses a method for quickly regulating and controlling the valence state of a vanadium solution based on a large-current pulse technology, and relates to the field of energy storage batteries. The method takes high-valence vanadium electrolyte, low-valence vanadium electrolyte and vanadium electrolyte with unbalanced valence as main raw materials, and adopts a pulse mode to carry out electrolysis in an electrolytic cell to prepare the electrolyte with the valence of vanadium ions conforming to that of a vanadium battery; the electrolytic cell consists of a positive half cell and a negative half cell, the two half cells are separated by a diaphragm, an electrode inserted into the positive half cell is connected with the positive pole of a direct current pulse power supply, an electrode inserted into the negative half cell is connected with the negative pole of the direct current pulse power supply, and pulse electrolysis parameters are controlled to carry out electrolysis. The method is simple and easy to operate, can quickly adjust the vanadium valence state of the electrolyte, can obtain the electrolyte with the specified vanadium valence state, can meet the use requirements under different conditions, and has very wide application prospect.

Description

Vanadium solution valence state rapid regulation and control method based on high-current pulse technology
Technical Field
The invention relates to the technical field of energy storage batteries, in particular to a method for quickly regulating and controlling the valence state of a vanadium solution based on a large-current pulse technology.
Background
An all-vanadium redox flow battery (vanadium battery) is a secondary energy system that utilizes redox reactions between vanadium ions of different valence states for energy storage and conversion. The method is characterized in that: no discharge pollution, adjustable capacity, long cycle life, deep heavy current density discharge, quick charge and high energy conversion rate. The vanadium battery is mainly applied to energy storage power supplies of power station peak shaving, large-scale photoelectric conversion and wind power generation as well as energy storage systems of remote areas, uninterrupted power supplies or emergency power supply systems.
Along with the charge and discharge of the vanadium battery, vanadium ion migration, divalent vanadium ion oxidation in the cathode electrolyte, hydrogen evolution of the cathode and the like can be generated between the anode electrolyte and the cathode electrolyte, so that the concentration and the valence state of the vanadium ion in the anode electrolyte and the cathode electrolyte are not matched. When the utilization rate of the electrolyte does not meet the design requirement, the vanadium electrolyte needs to be replaced by a new vanadium electrolyte, so that the energy storage cost of the vanadium battery is increased.
Currently, more valence state adjustment methods are used, including chemical reduction and oxidation, gas reduction and oxidation, and low current density direct current electrolysis (<200mA/cm 2 ) The method of (1). Impurity ions are easy to introduce by a chemical method, and the redox reaction degree of vanadium ions is not controlled; direct current electrolytic methods require a lower current density to control the end point of the electrochemical reaction, resulting in an excessively long conditioning time, a slow speed and an increase in cost to varying degrees.
Disclosure of Invention
In view of the above, the invention provides a method for rapidly regulating and controlling the valence state of a vanadium solution based on a large-current pulse technology, which overcomes the technical limitations of chemical reduction, low-current direct current electrolysis and other methods.
The invention discloses a method for quickly regulating and controlling the valence state of a vanadium solution based on a large-current pulse technology, which takes high-valence vanadium electrolyte, low-valence vanadium electrolyte and vanadium electrolyte with unbalanced valence state as main raw materials, and carries out electrolysis in an electrolytic cell by adopting a pulse mode to prepare the electrolyte with the valence state of vanadium ions conforming to that required by a vanadium battery; the electrolytic cell consists of a positive half cell and a negative half cell, the two half cells are separated by a diaphragm, an electrode inserted into the positive half cell is connected with the positive pole of a direct current pulse power supply, an electrode inserted into the negative half cell is connected with the negative pole of the direct current pulse power supply, and pulse electrolysis parameters are controlled to carry out electrolysis.
Further, during electrolysis, when the valence state of the vanadium solution needs to be raised, the positive half pool is the vanadium solution, and the negative half pool is the sulfuric acid solution; when the valence state of the vanadium solution needs to be reduced, the negative half pool is the vanadium solution, and the positive half pool is the sulfuric acid solution.
Further, the high valence vanadium electrolyte comprises VO 2 + And VO 2+ (ii) a The low-valence vanadium electrolyte comprises V 3+ And V 2 + (ii) a V in the vanadium electrolyte with the valence state unbalance 3+ And VO 2+ The ratio of (A) deviates from 1: 1.
Further, the positive electrode and the negative electrode both adopt graphite electrodes or size-stable electrodes; the concentration of the sulfuric acid solution in the positive half pool and the negative half pool is 2-8 mol/L.
Further, the electrolysis mode adopts constant current pulse electrolysis, and the average current density is 200-2000 mA/cm 2 The frequency is 200-2000 Hz, and the duty ratio is 20-80%.
Further, the positive electrode is any one of a platinum electrode, a gold electrode, a titanium-based lead dioxide electrode, a titanium-based noble metal oxide coating electrode, a titanium-based platinum electrode, and a titanium suboxide electrode.
Further, the electrode material of the negative electrode comprises at least one of a metal material, a carbon material and a conductive ceramic material; wherein the metal material comprises at least one of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, niobium, tantalum, zirconium, tungsten, cerium, aluminum, bismuth, rhenium, barium, osmium, tin, lead, gold, silver, platinum, palladium, iridium, rhodium, molybdenum and ruthenium; the carbon material comprises any one of graphite, glassy carbon, boron-doped diamond, activated carbon, graphene, carbon fiber, carbon nanotube, carbon sponge, carbon felt and graphite felt.
Further, the electrode shape of the positive electrode and the negative electrode includes any one of a sheet, a rod, a filament, a granule, a sponge, a mesh, and a porous structure.
Further, the stirring manner is mechanical stirring or air stirring.
Due to the adoption of the technical scheme, the invention has the following advantages: (1) the method is simple and easy to operate, can quickly adjust the vanadium valence state of the electrolyte, obtain the electrolyte with various vanadium valence states, and can meet the use requirements under different conditions; (2) the invention adopts a pulse electrolysis mode to carry out high valence state (VO) 2 + 、VO 2+ ) Lower valence state (V) 3+ 、V 2+ ) Vanadium electrolyte, valence state unbalance (V) 3+ ：VO 2+ The valence state adjustment of the vanadium electrolyte deviating from 1:1), compared with the traditional technology, the method has the advantages of high adjustment speed, high current efficiency, simple process method, low operation cost and wide application prospect.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments described in the embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings.
Fig. 1 is a schematic diagram of a rapid adjustment and control of a valence state of a vanadium solution based on a high current pulse technique according to an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, it being understood that the examples described are only some of the examples and are not intended to limit the invention to the embodiments described herein. All other embodiments available to those of ordinary skill in the art are intended to be within the scope of the embodiments of the present invention.
Example 1:
regulation of tetravalent Vanadium (VO) 2+ ) Solution to V 3+ ：VO 2+ The solution 1:1 is specifically: adding 2.0mol/L sulfuric acid solution into a positive half pool of an electrolytic cell, wherein a negative half pool is sulfuric acid aqueous solution with tetravalent vanadium of 2.0mol/L +2.0mol/L, the volumes of the two half pools are both 50mL, the positive half pool adopts a DSA electrode, the negative half pool adopts a graphite electrode, the effective electrode area is 10cm 2 At 600mA/cm 2 The average current density of (2) was electrolyzed at a frequency of 500Hz, a duty ratio of 20% and an electrolysis adjustment time of 0.3 hour. And (3) measuring the concentration of the electrolyte passing through the negative half cell to show that the trivalent vanadium ions in the solution: the concentration ratio of tetravalent vanadium ions is 1: 1. if direct current electrolysis is used, 1.44h is required.
Graphite felt is used as a positive electrode material and a negative electrode material, the positive electrode solution and the negative electrode solution are electrolyte which is prepared by electrolysis and contains vanadium ions with the concentration of 2.0mol/L, and the charge-discharge current density is 100mA/cm 2 The energy efficiency is 82 percent and is 150mA/cm 2 The energy efficiency was 76%.
Example 2:
regulation of trivalent vanadium (V) 3+ ) Solution to V 3+ ：VO 2+ The solution 1:1 is specifically: adding 3.0mol/L sulfuric acid solution into a negative half pool of an electrolytic cell, wherein the positive half pool is sulfuric acid aqueous solution with trivalent vanadium of 2.2mol/L +3.0mol/L, the volumes of the two half pools are both 50mL, the positive half pool adopts a platinum electrode, the negative half pool adopts a graphite felt electrode, and the effective electrode area is 10cm 2 At 1000mA/cm 2 The electrolysis was carried out at a frequency of 800Hz, a duty ratio of 30% and an electrolysis time of 0.23 hours. And (3) measuring the concentration of the negative half-cell electrolyte to show that the concentration of the trivalent vanadium ions: the concentration ratio of tetravalent vanadium ions is 1: 1. if direct current electrolysis is used, 159h is required.
Graphite felt is used as a positive electrode material and a negative electrode material, the positive electrode solution and the negative electrode solution are electrolyte which is prepared by electrolysis and contains vanadium ions with the concentration of 2.2mol/L, and the charge-discharge current density is 100mA/cm 2 The energy efficiency is 80 percent and is 150mA/cm 2 The energy efficiency was 75%.
Example 3:
adjusting pentavalent Vanadium (VO) 2 + ) Solution to V 3+ ：VO 2+ The solution 1:1 is specifically: in thatAdding 4.0mol/L sulfuric acid solution into a positive half pool of an electrolytic cell, wherein a negative half pool is sulfuric acid aqueous solution with pentavalent vanadium of 1.8mol/L +3.0mol/L, the volume of the two half pools is 50mL, the positive half pool adopts a gold electrode, the negative half pool adopts a glassy carbon electrode, and the effective electrode area is 10cm 2 At 1500mA/cm 2 The electrolysis was carried out at a frequency of 1200Hz, a duty ratio of 30% and an electrolysis time of 0.185 hours. And (3) measuring the concentration of the negative half-cell electrolyte to show that the concentration of the trivalent vanadium ions: the concentration ratio of tetravalent vanadium ions is 1: 1. if direct current electrolysis is used, 1.95h is required.
Graphite felt is used as a positive electrode material and a negative electrode material, the positive electrode solution and the negative electrode solution are electrolyte which is prepared by electrolysis and contains vanadium ions with the concentration of 1.8mol/L, and the charge-discharge current density is 100mA/cm 2 The energy efficiency is 85 percent and is 150mA/cm 2 The energy efficiency was 79%.
Example 4:
regulating V 3+ ：VO 2+ 2:1 solution to V 3+ ：VO 2+ The solution 1:1 is specifically: adding 3.0mol/L sulfuric acid solution into a negative half pool of an electrolytic cell, wherein the positive half pool is sulfuric acid aqueous solution with trivalent vanadium of 1.2mol/L, tetravalent vanadium of 0.6mol/L and 3.0mol/L, the volumes of the two half pools are both 50mL, the half pool adopts a platinum-plated electrode, the negative half pool adopts a carbon felt electrode, and the concentration of the carbon felt electrode is 2000mA/cm 2 The electrolysis was carried out at a frequency of 1500Hz, a duty ratio of 20% and an electrolysis time of 0.07 hours. And (3) measuring the concentration of the positive half cell electrolyte to show that the trivalent vanadium ions: the concentration ratio of tetravalent vanadium ions is 1: 1. if direct current electrolysis is used, 0.87h is required.
Graphite felt is used as a positive electrode material and a negative electrode material, the positive electrode solution and the negative electrode solution are electrolyte which is prepared by electrolysis and contains vanadium ions with the concentration of 1.8mol/L, and the charge-discharge current density is 100mA/cm 2 The energy efficiency is 86 percent and is 150mA/cm 2 The energy efficiency was 79%.
Example 5:
regulation of pentavalent (VO) 2 + ) Vanadium ion: quadrivalence (VO) 2+ ) The vanadium ion ratio is 3: 1 vanadium solution to tetravalent (VO) 2+ ) The vanadium ion solution specifically comprises: adding 3.0mol/L sulfuric acid solution into the negative half pool of the electrolytic cellThe positive half pool is sulfuric acid aqueous solution with trivalent vanadium of 1.5mol/L, tetravalent vanadium of 0.5mol/L and 3.0mol/L, the volumes of the two half pools are both 50mL, the half pool adopts a platinum-plated electrode, the negative half pool adopts a carbon felt electrode at 2000mA/cm 2 The electrolysis was carried out at a frequency of 1500Hz, a duty ratio of 20% and an electrolysis time of 0.15 hours. And (3) measuring the concentration of the positive half cell electrolyte to show that the trivalent vanadium ions: the concentration ratio of tetravalent vanadium ions is 1: 1. if direct current electrolysis is used, it takes 2.16 h.
Graphite felt is used as a positive electrode material and a negative electrode material, the positive electrode solution and the negative electrode solution are electrolyte which is prepared by electrolysis and contains vanadium ions with the concentration of 1.8mol/L, and the charge-discharge current density is 100mA/cm 2 The energy efficiency is 86 percent and is 150mA/cm 2 The energy efficiency was 79%.
Example 6:
regulation of pentavalent (VO) 2 + ) Vanadium solution to trivalent (V) 3+ ) The vanadium solution specifically comprises: adding 3.0mol/L sulfuric acid solution into a positive half pool of an electrolytic cell, wherein a negative half pool is sulfuric acid aqueous solution with pentavalent vanadium of 1.6mol/L and 3.0mol/L, the volume of the two half pools is 50mL, the half pool adopts a platinum-plated electrode, the negative half pool adopts a carbon felt electrode, and the concentration of the carbon felt electrode is 2000mA/cm 2 The electrolysis was carried out at a frequency of 1200Hz, a duty ratio of 20% and an electrolysis time of 0.144 hours. And the concentration of the positive half cell electrolyte is measured, which shows that the trivalent vanadium ion is 1.6 mol/L. If direct current electrolysis is used, it takes 2.3 h.
Example 7:
regulation of quadrivalence (VO) 2+ ) Vanadium solution to divalent (V) 2+ ) The vanadium solution specifically comprises: adding 3.0mol/L sulfuric acid solution into a positive half pool of an electrolytic cell, wherein a negative half pool is sulfuric acid aqueous solution with tetravalent vanadium of 2.0mol/L and 3.0mol/L, the volume of the two half pools is 50mL, a platinum-plated electrode is adopted in the half pool, a carbon felt electrode is adopted in the negative half pool, and the concentration of the carbon felt electrode is 1600mA/cm 2 The electrolysis was carried out at a frequency of 1500Hz, a duty ratio of 20% and an electrolysis time of 0.225 hours. And the concentration of the positive half cell electrolyte is measured, and the divalent vanadium ions are 2.0 mol/L. If direct current electrolysis is used, 2.88h is required.
Example 8:
see FIG. 1, modulation of bivalent (V) 2+ ) Vanadium solution to pentavalent (VO) 2 + ) The vanadium solution specifically comprises: adding 3.0mol/L sulfuric acid solution into a negative half pool of an electrolytic cell, wherein the positive half pool is aqueous solution of divalent vanadium of 1.5mol/L and 3.0mol/L sulfuric acid, the volume of the two half pools is 50mL, the half pool adopts a platinum-plated electrode, the negative half pool adopts a carbon felt electrode, and the concentration of the carbon felt electrode is 1200mA/cm 2 The electrolysis was carried out at a frequency of 1500Hz, a duty ratio of 30% and an electrolysis time of 0.77 hours. And the concentration of the positive half cell electrolyte is measured, and the pentavalent vanadium ions are 1.5 mol/L. If direct current electrolysis is used, it takes 6.48 h.
The embodiment result shows that the method for rapidly regulating and controlling the valence state of the vanadium solution based on the large-current pulse technology can perform rapid electrolysis under a larger current density, has simple process and short time consumption, and is easy to form industrialization.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.

Claims (9)

1. A vanadium solution valence state rapid regulation and control method based on a large current pulse technology is characterized in that high valence state vanadium electrolyte, low valence state vanadium electrolyte and vanadium electrolyte with unbalanced valence state are used as main raw materials, electrolysis is carried out in an electrolytic cell by adopting a pulse mode, and electrolyte with vanadium ion valence state meeting the requirement of a vanadium battery is prepared; the electrolytic cell consists of a positive half cell and a negative half cell, the two half cells are separated by a diaphragm, an electrode inserted into the positive half cell is connected with the positive pole of a direct current pulse power supply, an electrode inserted into the negative half cell is connected with the negative pole of the direct current pulse power supply, and pulse electrolysis parameters are controlled to carry out electrolysis.
2. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein during electrolysis, when the valence state of the vanadium solution needs to be raised, the positive half tank is the vanadium solution, and the negative half tank is the sulfuric acid solution; when the valence state of the vanadium solution needs to be reduced, the negative half pool is the vanadium solution, and the positive half pool is the sulfuric acid solution.
3. The method for rapidly regulating and controlling the valence state of a vanadium solution based on a high-current pulse technology as claimed in claim 1, wherein the high-valence vanadium electrolyte comprises VO 2 + And VO 2+ (ii) a The low-valence vanadium electrolyte comprises V 3+ And V 2+ (ii) a V in the vanadium electrolyte with the valence state unbalance 3+ And VO 2+ The ratio of (A) deviates from 1: 1.
4. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein the positive electrode and the negative electrode both adopt graphite electrodes or size-stable electrodes; the concentration of the sulfuric acid solution in the positive half pool and the negative half pool is 2-8 mol/L.
5. The method for rapidly regulating and controlling the valence state of a vanadium solution based on a high-current pulse technology as claimed in claim 1, wherein the electrolysis mode adopts constant-current pulse electrolysis, and the average current density is 200-2000 mA/cm 2 The frequency is 200-2000 Hz, and the duty ratio is 20-80%.
6. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein the positive electrode is any one of a platinum electrode, a gold electrode, a titanium-based lead dioxide electrode, a titanium-based noble metal oxide coating electrode, a titanium-based platinum electrode and a titanium suboxide electrode.
7. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein the electrode material of the negative electrode comprises at least one of a metal material, a carbon material and a conductive ceramic material; wherein the metal material comprises at least one of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, niobium, tantalum, zirconium, tungsten, cerium, aluminum, bismuth, rhenium, barium, osmium, tin, lead, gold, silver, platinum, palladium, iridium, rhodium, molybdenum and ruthenium; the carbon material comprises any one of graphite, glassy carbon, boron-doped diamond, activated carbon, graphene, carbon fiber, carbon nanotube, carbon sponge, carbon felt and graphite felt.
8. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein the shapes of the positive electrode and the negative electrode include any one of a sheet, a rod, a filament, a granule, a sponge, a net and a porous structure.
9. The method for rapidly regulating and controlling the valence state of the vanadium solution based on the high-current pulse technology as claimed in claim 1, wherein the stirring manner is mechanical stirring or air stirring.
CN202210464258.1A 2022-04-29 2022-04-29 Vanadium solution valence state rapid regulation and control method based on high-current pulse technology Pending CN114807957A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115655383A (en) * 2022-12-27 2023-01-31 杭州德海艾科能源科技有限公司 Method and system for detecting valence state imbalance state of electrolyte of all-vanadium redox flow battery

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812698A (en) * 2009-02-23 2010-08-25 中国科学院金属研究所 Pulse electrolytic preparation method of all vanadium ion redox flow battery electrolyte
CN103762377A (en) * 2014-01-27 2014-04-30 中国东方电气集团有限公司 Vanadium redox battery and electrolyte rebalancing method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812698A (en) * 2009-02-23 2010-08-25 中国科学院金属研究所 Pulse electrolytic preparation method of all vanadium ion redox flow battery electrolyte
CN103762377A (en) * 2014-01-27 2014-04-30 中国东方电气集团有限公司 Vanadium redox battery and electrolyte rebalancing method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115655383A (en) * 2022-12-27 2023-01-31 杭州德海艾科能源科技有限公司 Method and system for detecting valence state imbalance state of electrolyte of all-vanadium redox flow battery
CN115655383B (en) * 2022-12-27 2023-04-07 杭州德海艾科能源科技有限公司 Method and system for detecting valence state imbalance state of electrolyte of all-vanadium redox flow battery

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