CN110970646A - Application of additive in negative electrode electrolyte of all-vanadium redox flow battery - Google Patents
Application of additive in negative electrode electrolyte of all-vanadium redox flow battery Download PDFInfo
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- CN110970646A CN110970646A CN201811145979.6A CN201811145979A CN110970646A CN 110970646 A CN110970646 A CN 110970646A CN 201811145979 A CN201811145979 A CN 201811145979A CN 110970646 A CN110970646 A CN 110970646A
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- 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
An application of an additive in an all-vanadium redox flow battery negative electrode electrolyte. The invention relates to a flow battery negative electrode electrolyte containing an additive, wherein the additive is C containing at least one carboxyl and at least one hydroxylxHyOzAt least one organic substance, wherein x is 2-10, and the organic substance comprises one or more of malic acid, p-hydroxybenzoic acid, salicylic acid, hydroxypropionic acid, hydroxybutyric acid, gentisic acid, gallic acid and protocatechuic acid; the concentration of the additive is 0.01 wt% -5 wt%. The preferred concentration of the additive is 0.05 wt% to 1 wt%. The material used in the invention is used as the negative electrolyte additive, so that the low-temperature stability of the di-trivalent vanadium ions can be effectively improved, the low-temperature stability of the negative electrolyte can be improved, the capacity retention rate of the battery in a long-term circulation process at low temperature can be effectively improved, and the stable operation of the battery at low temperature can be realized. The preparation process disclosed by the invention is simple to operate, energy-saving, environment-friendly and low in cost, and can realize stable operation of the electrolyte in the battery.
Description
Technical Field
The invention relates to application of electrolyte stability in the technical field of energy storage of all-vanadium redox flow batteries, in particular to an additive-containing all-vanadium redox flow battery electrolyte.
Background
With the continuous depletion of fossil energy and the continuous enhancement of people's environmental protection consciousness all over the world, renewable energy power generation technology is more and more favored by people. Renewable energy sources mainly include wind energy, solar energy, biomass energy, ocean energy, and the like, which are generally converted into electric energy for use. The renewable energy power generation is obviously discontinuous and unstable under the influence of conditions such as regions, weather and the like. In order to smooth and stabilize the power generation output of renewable energy sources, solve the time difference contradiction between power generation and power utilization, and improve the power quality and the reliability of a power grid, a high-efficiency energy storage technology must be developed. The full-vanadium redox flow battery (VFB) has the outstanding advantages of mutually independent and adjustable system capacity and power, rapid response, safety, reliability, environmental friendliness, long cycle life, easiness in maintenance and regeneration and the like, so that the VFB becomes one of the most promising technologies in large-scale energy storage such as renewable energy power generation, peak clipping and valley filling of a power grid, emergency and standby power stations and the like.
The electrolyte is an important component of the all-vanadium redox flow battery, the concentration and the volume of the electrolyte directly determine the capacity of the battery, and the stability of the electrolyte directly influences the reliability and the stability of the VFB in the long-term operation process. In practice, however, during operation, the solubility and stability of the vanadium ions in the supporting electrolyte is limited: when the temperature is low, low-valence vanadium ions in the negative electrolyte are easy to precipitate, so that the application of the all-vanadium redox flow battery system in a low-temperature environment is limited. Therefore, improving the medium-low temperature thermal stability of the VFB negative electrode electrolyte is particularly important for the stability and application range of the battery system. For the problem of low-valence vanadium ion precipitation in the electrolyte, the low-temperature stability of the low-valence vanadium ion can be improved by adding a small amount of additive into the electrolyte, so that the low-valence vanadium ion can exist stably at a lower temperature.
Disclosure of Invention
The invention aims to solve the problems and provides the all-vanadium redox flow battery negative electrode electrolyte containing the additive so as to improve the low-temperature stability of the all-vanadium redox flow battery negative electrode electrolyte.
In order to achieve the purpose, the invention adopts the technical scheme that:
an all-vanadium redox flow battery negative electrode electrolyte containing an additive, wherein the additive is C containing at least one carboxyl and at least one hydroxylxHyOzAt least one organic substance, wherein x is 1-10, y is 4-22, z is 3-20, and the organic substance comprises one or more of malic acid, p-hydroxybenzoic acid, salicylic acid, hydroxypropionic acid, hydroxybutyric acid, gentisic acid, gallic acid and protocatechuic acid, preferably one or more of p-hydroxybenzoic acid, salicylic acid, gentisic acid, gallic acid and protocatechuic acid; the concentration of the additive is 0.01 wt% -5 wt%. The preferred concentration of the additive is 0.05 wt% to 1 wt%.
The main component of the vanadium battery electrolyte applicable to the invention is a lower valence (di-or tri-valent) vanadyl-sulfuric acid system. Vanadium ion (containing V) in the negative electrode electrolyte2+，V3+One or two of them) is 0.5 to 3mol/L, sulfate radical (containing SO)4 2-And HSO4 -One or two) at a concentration of 1 to 7 mol/L. The preferable concentration of vanadium ions in the negative electrode electrolyte is 1-2 mol/L, and the preferable concentration of sulfate radicals is 3-5 mol/L.
Vanadium ion (containing V) in positive electrode electrolyte4+，V5+One or two of them) is 0.5 to 3mol/L, sulfate radical (containing SO)4 2-And HSO4 -One or two) at a concentration of 1 to 7 mol/L.
The running temperature of the all-vanadium redox flow battery adopting the cathode electrolyte is 10-minus 20 ℃.
When the positive electrode and the negative electrode both contain the additive, the additive can reduce the high-valence vanadium ions of the positive electrode, and the additive can adversely affect the stability of the positive electrolyte and the battery.
The beneficial results of the invention are:
the cathode electrolyte containing the additive used in the invention can effectively improve the low-temperature stability of the di-trivalent vanadium ions, improve the low-temperature stability of the cathode electrolyte, effectively improve the capacity retention rate of the battery in a long-term circulation process at low temperature, and realize the stable operation of the battery at low temperature. The preparation process disclosed by the invention is simple to operate, energy-saving, environment-friendly and low in cost, and can ensure that the battery can efficiently and stably run for a long time.
Drawings
Fig. 1 discharge capacity curves for cell No. 1 and cell No. 2 in example 6.
Fig. 2 discharge capacity curves for cell No. 3 and cell No. 4 of example 7.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1
Preparing 1.5M divalent vanadium solution by adopting an electrolysis method, respectively adding 0.01 wt%, 0.05 wt%, 0.5 wt%, 1 wt% and 10 wt% of malic acid, salicylic acid, gallic acid and hydrochloric acid into 10mL of divalent vanadium solution, sealing, fully mixing, uniformly stirring, placing the mixture and a blank 1.5M divalent vanadium solution sample in a thermostat at minus 10 ℃, observing the state of the solution, and investigating the influence of different additives and contents on the low-temperature stability of the cathode electrolyte. The low-temperature stability means that the electrolyte maintains a homogeneous liquid state at a certain temperature, and no solid is precipitated, no gas is volatilized, and the like.
TABLE 1 influence of different contents of additives on electrolyte stability
Note: the stabilization time means a time taken from the time when the electrolyte is put into a low-temperature environment to the time when the precipitation of solids is observed.
As can be seen from Table 1, the stability time of the electrolyte containing the additive of malic acid, salicylic acid and gallic acid is obviously prolonged compared with that of the blank sample, which shows that the additive can improve the low-temperature stability of the divalent vanadium ions. And when the content of the additive is 0.05 wt% -0.5 wt%, the low-temperature stability of the electrolyte is better. And when the additive content is increased to 10 wt%, the electrolyte stability is remarkably lowered. And the addition of the inorganic hydrochloric acid has no obvious influence on the low-temperature stability time of the electrolyte. The stabilization time was not significantly prolonged for the samples with formic acid or ethanol added. The reason may be that the vanadium ion of the negative electrode interacts with the hydroxyl group and the carboxyl group together to form a certain complex, which can exist more stably at low temperature. And pure hydroxyl or carboxyl is lack of the mutual interaction with vanadium ions, so that the low-temperature stability of the vanadium ion is not obviously improved.
Example 2
Preparing 1.6M cathode electrolyte by adopting an electrolytic method, wherein the concentration of di-and trivalent vanadium ions is 0.9M and 0.7M respectively, the concentration of sulfate radical is 3.2mol/L, adding 0.02 wt%, 0.1 wt%, 0.4 wt%, 0.8 wt% and 5 wt% of gentisic acid, hydroxypropionic acid, p-hydroxybenzoic acid and nitric acid into 20mL of cathode electrolyte respectively, sealing, stirring uniformly after fully mixing, placing the mixture and a blank 1.6M cathode electrolyte sample in a thermostat at minus 15 ℃, observing the state of the solution, and inspecting the influence of different additives and contents on the low-temperature stability of the cathode electrolyte. The low-temperature stability means that the electrolyte maintains a homogeneous liquid state at a certain temperature, and no solid is precipitated, no gas is volatilized, and the like.
TABLE 2 influence of different additive contents on electrolyte stability
Note: the stabilization time means a time taken from the time when the electrolyte is put into a low-temperature environment to the time when the precipitation of solids is observed.
As can be seen from Table 2, the stability time of the electrolyte containing the additive of gentisic acid, hydroxypropionic acid and p-hydroxybenzoic acid is obviously prolonged compared with that of the blank sample, which shows that the additive can improve the low-temperature stability of vanadium ions in the negative electrolyte. And when the content of the additive is 0.1-0.4 wt%, the low-temperature stability of the electrolyte is better. And when the additive content is increased to 5 wt%, the electrolyte stability is remarkably lowered. And the addition of inorganic nitric acid has no obvious influence on the low-temperature stability time of the electrolyte.
Example 3
Preparing 1.5M low-valence vanadium solution by adopting an electrolytic method, wherein the sulfate radical concentration is 3mol/L, the concentration of di-and trivalent vanadium ions is 0.75M respectively, adding 0.01 wt%, 0.05 wt%, 0.5 wt%, 1 wt% and 10 wt% of malic acid, salicylic acid, gallic acid and polyacrylic acid into 10mL of the low-valence vanadium solution respectively, sealing, fully mixing, stirring uniformly, placing the mixture and a blank 1.5M low-valence vanadium solution sample in a thermostat at minus 10 ℃, observing the state of the solution, and inspecting the influence of different additives and contents on the low-temperature stability of the cathode electrolyte. The low-temperature stability means that the electrolyte maintains a homogeneous liquid state at a certain temperature, and no solid is precipitated, no gas is volatilized, and the like.
TABLE 3 influence of different additive contents on electrolyte stability
Note: the stabilization time means a time taken from the time when the electrolyte is put into a low-temperature environment to the time when the precipitation of solids is observed.
It can be seen from table 3 that the electrolyte stability time containing the additive of malic acid, salicylic acid and gallic acid is significantly longer than that of the blank sample, which indicates that the additive can improve the low-temperature stability of vanadium ions in the negative electrode electrolyte. And when the content of the additive is 0.05 wt% -0.5 wt%, the low-temperature stability of the electrolyte is better. And when the additive content is increased to 10 wt%, the electrolyte stability is remarkably lowered. While the samples with polyacrylic acid added have a somewhat prolonged stabilization time, the effect is almost negligible.
Example 4
Preparing 1.8M divalent vanadium solution by adopting an electrolytic method, wherein the sulfate radical concentration is 3.6mol/L, adding 0.05 wt%, 0.12 wt%, 0.4 wt%, 1 wt% and 6 wt% of hydroxy propionic acid, salicylic acid and p-hydroxybenzoic acid into 10mL divalent vanadium solution respectively, sealing, fully mixing, stirring uniformly, placing the mixture and a blank 1.8M divalent vanadium solution sample in a thermostat at minus 20 ℃, observing the state of the solution, and inspecting the influence of different additives and contents on the low-temperature stability of the cathode electrolyte. The low-temperature stability means that the electrolyte maintains a homogeneous liquid state at a certain temperature, and no solid is precipitated, no gas is volatilized, and the like.
TABLE 4 influence of different additive contents on electrolyte stability
Note: the stabilization time means a time taken from the time when the electrolyte is put into a low-temperature environment to the time when the precipitation of solids is observed.
As can be seen from Table 4, the stability time of the electrolyte containing the hydroxypropionic acid, salicylic acid and p-hydroxybenzoic acid additive was significantly longer than that of the blank sample, indicating that the additive can improve the low temperature stability of the divalent vanadium ions. And when the content of the additive is 0.12-0.4 wt%, the low-temperature stability of the electrolyte is better. And when the additive content is increased to 6 wt%, the electrolyte stability is remarkably lowered.
Example 5
Preparing a 1.8M trivalent vanadium solution by adopting an electrolytic method, wherein the sulfate radical concentration is 3.6mol/L, adding 0.02 wt%, 0.1 wt%, 0.5 wt%, 1 wt% and 5 wt% of malic acid, hydroxypropionic acid and p-hydroxybenzoic acid into 50mL of the divalent vanadium solution, sealing, fully mixing, uniformly stirring, placing the mixture and a blank 1.8M trivalent vanadium solution sample in a thermostat at minus 15 ℃, observing the state of the solution, and investigating the influence of different additives and contents on the low-temperature stability of the trivalent vanadium electrolyte. The low-temperature stability means that the electrolyte maintains a homogeneous liquid state at a certain temperature, and no solid is precipitated, no gas is volatilized, and the like.
TABLE 5 influence of different additive contents on electrolyte stability
Note: the stabilization time means a time taken from the time when the electrolyte is put into a low-temperature environment to the time when the precipitation of solids is observed.
As can be seen from Table 5, the electrolyte stability time containing the malic acid, hydroxypropionic acid and p-hydroxybenzoic acid additive was significantly longer than the blank, indicating that the additive can improve the low temperature stability of the trivalent vanadium ions. And when the content of the additive is 0.1 wt% -1 wt%, the low-temperature stability of the electrolyte is better. And when the additive content is increased to 5 wt%, the electrolyte stability is remarkably lowered.
Example 6
Preparing four parts of electrolyte with the same components and the total vanadium concentration of 1.5M (the trivalent vanadium concentration is 0.75M, the tetravalent vanadium concentration is 0.75M), wherein the sulfate radical concentration is 3mol/L, one part is used for a positive electrode, the other part is used for a negative electrode, 1 wt% gentisic acid is added into the electrolyte for the negative electrode, the all-vanadium redox flow battery is assembled, a diaphragm is made of Nafion115, and an electrode is a 5mm carbon felt, and the all-vanadium redox flow battery is defined as a No. 1 battery.
And assembling the other two parts of electrolyte, wherein one part of the electrolyte is used for a positive electrode, the other part of the electrolyte is used for a negative electrode (blank comparison), and the all-vanadium redox flow battery is defined as a No. 2 battery, wherein a diaphragm is made of Nafion115, and an electrode is a 5mm carbon felt.
Meanwhile, the two batteries are placed in a thermostat at 0 ℃ for battery charging and discharging, the discharging curve is shown in figure 1, and it can be obviously seen that the discharge capacity attenuation of the No. 1 battery is obviously smaller than that of the No. 2 battery, which shows that the electrolyte containing the additive shows smaller capacity attenuation due to the improvement of low-temperature stability, and the capacity retention rate is improved.
Example 7
Preparing four parts of electrolyte with the same components and the total vanadium concentration of 1.7M (the trivalent vanadium concentration is 0.85M, the tetravalent vanadium concentration is 0.85M), wherein the sulfate radical concentration is 3.4mol/L, one part is used for a positive electrode, the other part is used for a negative electrode, 1 wt% of gallic acid is added into the electrolyte for the negative electrode, the all-vanadium flow battery is assembled, a diaphragm is made of Nafion115, and an electrode is a 5mm carbon felt, and the all-vanadium flow battery is defined as a No. 3 battery.
And the other two parts of electrolyte, wherein one part of the electrolyte is used as a positive electrode, the other part of the electrolyte is used as a negative electrode (blank comparison), 1 wt% of gallic acid is added into the positive electrode and the negative electrode, the all-vanadium redox flow battery is assembled, the diaphragm is Nafion115, and the electrode is a 5mm carbon felt, and is defined as a No. 4 battery.
Meanwhile, the two batteries are placed in a thermostat at 5 ℃ for battery charging and discharging, the discharging curve is shown in figure 2, and it can be obviously seen that the discharging capacity attenuation of the No. 3 battery is obviously smaller than that of the No. 4 battery, which shows that the electrolyte containing the additive shows smaller capacity attenuation due to the improvement of low-temperature stability, and the capacity retention rate is improved. Meanwhile, the capacity of the No. 4 battery initially decreases and then increases, because the hydroxyl in the additive reduces the high-valence vanadium ions V (V), so that the concentration of the active substance is reduced, and the capacity is obviously reduced. When all hydroxyl groups were completely reacted, the concentration of the active material increased, and the discharge capacity was increased temporarily. Thus, the additive is not suitable for being added to the positive electrode.
Claims (9)
1. The application of the additive in the cathode electrolyte of the all-vanadium redox flow battery is characterized in that: the additive is C containing at least one carboxyl and at least one hydroxylxHyOzAt least one of organic substances, wherein x is 2-10, y is 4-22, and z is 3-20.
2. Use according to claim 1, characterized in that: the additive is C2-C10At least one hydroxy acid of (a).
3. Use according to claims 1 and 2, characterized in that: the additive comprises one or more of malic acid, p-hydroxybenzoic acid, salicylic acid, hydroxypropionic acid, hydroxybutyric acid, gentisic acid, gallic acid, and protocatechuic acid.
4. Use according to claim 3, characterized in that: the additive is preferably one or more of p-hydroxybenzoic acid, salicylic acid, gentisic acid, gallic acid and protocatechuic acid.
5. Use according to claim 1, characterized in that: the concentration of the additive is 0.01 wt% -5 wt%; the preferred concentration of the additive is 0.05 wt% to 1 wt%.
6. Use according to claim 1, characterized in that: the electrolyte of the negative electrolyte comprises vanadium ions and sulfate radicals, and the vanadium ions in the negative electrolyte comprise V2+，V3+One or two of them, the concentration is 0.5-3 mol/L; sulfate radical containing SO4 2-And HSO4 -One or two of the above (1-7) mol/L, and the solvent is water.
7. Use according to claim 1 or 6, characterized in that: the preferable concentration of vanadium ions in the negative electrode electrolyte is 1-2 mol/L, and the preferable concentration of sulfate radicals is 3-5 mol/L.
8. Use according to claim 1 or 6, characterized in that: the vanadium ion in the positive electrode electrolyte contains V4+，V5+One or two of them, the concentration is 0.5-3 mol/L, the sulfate radical contains SO4 2-And HSO4 -One or two of the above (1-7) mol/L, and the solvent is water.
9. Use according to any one of claims 1 to 8, wherein: the running temperature of the all-vanadium redox flow battery adopting the cathode electrolyte is 10-minus 20 ℃.
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| CN116504994A (en) * | 2023-06-28 | 2023-07-28 | 杭州德海艾科能源科技有限公司 | All-vanadium redox flow battery negative electrode dual-function additive and preparation method and application thereof |
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