CN114865066A - Iron-chromium flow battery electrolyte containing complexing agent - Google Patents

Iron-chromium flow battery electrolyte containing complexing agent Download PDF

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CN114865066A
CN114865066A CN202210516829.1A CN202210516829A CN114865066A CN 114865066 A CN114865066 A CN 114865066A CN 202210516829 A CN202210516829 A CN 202210516829A CN 114865066 A CN114865066 A CN 114865066A
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complexing agent
chromium
iron
electrolyte
ions
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程元徽
牛世阳
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0563—Liquid materials, e.g. for Li-SOCl2 cells
    • 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
    • H01M2300/0017—Non-aqueous electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention discloses an iron-chromium flow battery electrolyte containing a complexing agent, belonging to the technical field of electrochemical energy storage. The electrolyte containing the complexing agent contains Cr at the negative electrode 3+ /Cr 2+ The ionic electrolyte and the positive electrode contain Fe 3+ /Fe 2+ Adding diethylenetriamine pentaacetic acid (DTPA) or salt thereof and bromide into the ionic electrolyte simultaneously to respectively obtain (Br) Cr (DTPA) 3+ /(Br)Cr(DTPA) 2+ And a negative electrode electrolyte containing (Br) Fe (DTPA) 3+ /(Br)Fe(DTPA) 2+ The positive electrode electrolyte of (1). The electrolyte used by the invention can effectively improve the reaction activity of the positive and negative redox couples and inhibit Cr 3+ Inactivating, increasing the size of the metal ion complex, avoiding cross contamination of electrolyte passing through the membrane, and improving the efficiency and service life of the iron-chromium flow battery.

Description

Iron-chromium flow battery electrolyte containing complexing agent
Technical Field
The invention relates to the technical field of electrochemical energy storage, in particular to an iron-chromium flow battery electrolyte containing a complexing agent.
Background
With the increasing world economy, people have increasingly increased demand for energy, and the shortage of energy is more serious. The environmental problems caused by the large consumption of traditional fossil energy are increasing day by day. Therefore, renewable energy is widely applied, but power generation by renewable energy such as wind energy, solar energy and the like has the characteristics of instability and discontinuity, and further development of the renewable energy is restricted. Therefore, there is a need for large-scale energy storage technology, especially long-term energy storage technology, to improve the power quality and reliability of renewable energy power generation.
The flow battery has the advantages of high safety, long cycle life, recyclable electrolyte, high life cycle cost performance, environmental friendliness and the like, is considered to be one of the first-choice technologies of large-scale energy storage technology, and has wide application prospects. The ferrochrome flow battery, as a first developed flow battery, has the advantages of low cost and the like, and becomes one of the most promising technologies in the large-scale energy storage such as renewable energy power generation.
The electrolyte is used as a key component of the iron-chromium flow battery, and the efficiency and stability of the battery are determined to a great extent. The electrolyte of the iron-chromium flow battery usually adopts an acidic solution containing iron ions, chromium ions and hydrochloric acid, and the iron ions and the chromium ions have small sizes and are easy to penetrate through a diaphragm. Meanwhile, CrCl is adopted as the cathode electrolyte of the traditional iron-chromium flow battery 3 Aqueous hydrochloric acid in the presence of Cr (H) 2 O) 6 3+ 、Cr(H 2 O) 5 Cl 2+ 、Cr(H 2 O) 4 Cl 2 + Three complexing ions, among which Cr (H) 2 O) 5 Cl 2+ And Cr (H) 2 O) 4 Cl 2 + Are electrochemically active ions, however Cl and Cr 3+ Weak ion binding force, easy to be converted into Cr (H) without electrochemical activity after long-term storage 2 O) 6 3+ Resulting in a decline in efficiency and capacity of the iron-chromium flow battery.
The regulation and control of the complex state of chromium ions in water is an effective way to improve the activity and stability of the chromium ions. The activity of CrDTPA in a 1M sulfuric acid solution is tested by a three-electrode system in the literature (Electrochimica Acta, 2013,94,336-343), the potential of a redox electrode is corrected to be about 0.2V vs SHE, the reversibility is poor, and the CrDTPA can not be used as a negative active electrode pair and is not applied to a battery. Rockschidmandin energy limited, usa, discloses (CN109461954A) an aqueous redox flow battery comprising a metal coordination compound, wherein one side comprises a metal-sulfonic catechol + other ligand as an electrolyte, the other ligand may be ethylene triamine pentaacetic acid (DTPA), wherein the sulfonic catechol is a bidentate ligand, the DTPA is a pentadentate ligand, and the saturated coordination of Cr is 6 coordination, both of which cannot be completely complexed with Cr ions, resulting in unstable Cr double complex structure, large steric hindrance of the double ligands, reduced electrochemical activity and reversibility, especially as can be seen in the examples, resulting in low voltage efficiency.
In conclusion, the complex state of chromium ions in water is regulated and controlled, so that the chromium ions and a ligand can form a stable hexa-coordination structure, and the problem of chromium ion inactivation is hopefully solved, but a single complexing agent is difficult to realize. The method adopts a pentadentate ligand DTPA and a monodentate ligand Br to simultaneously complex with Cr ions, so as to construct a Cr ion organic/inorganic composite complex system, and improve the efficiency and stability of the iron-chromium flow battery.
Disclosure of Invention
The invention develops the iron-chromium flow battery electrolyte containing the complexing agent, and solves the problems of inactivation of the cathode chromium electrolyte and cross contamination of the anode electrolyte and the cathode electrolyte of the iron-chromium flow battery, so that the energy conversion efficiency of the iron-chromium flow battery is improved, and the capacity retention rate is improved. The specific invention content is as follows:
the iron-chromium flow battery electrolyte containing complexing agents is characterized in that a negative electrolyte comprises trivalent chromium ions, divalent chromium ions, a first complexing agent, a second complexing agent, a supporting electrolyte and water, a positive electrolyte comprises iron ions, ferrous ions, the first complexing agent, the second complexing agent, the supporting electrolyte and water, the same first complexing agent and the same second complexing agent are adopted in the positive electrolyte and the negative electrolyte and are respectively complexed with the iron ions and the ferrous ions or the trivalent chromium ions and the divalent chromium ions, the first complexing agent is diethylenetriamine pentaacetic acid (DTPA) or salts thereof, and the second complexing agent is bromide.
The material containing trivalent chromium ions in the negative electrode electrolyte can be one or more than two of chromium trichloride, dichromium trithionate and chromium trinitrate, and the concentration is 0.1-2.0 mol/L.
The substance containing divalent chromium ions in the negative electrode electrolyte can be one or two of chromium dichloride and chromium sulfate, and the concentration is 0.1-2.0 mol/L.
The substance containing iron ions in the positive electrolyte can be one or more than two of ferric chloride, ferric sulfate and ferric nitrate, and the concentration is 0.1-2.0 mol/L.
The substance containing ferrous ions in the positive electrolyte can be one or more than two of ferrous chloride, ferrous sulfate and ferrous nitrate, and the concentration is 0.1-2.0 mol/L.
The first complexing agent is one or more than two of diethylenetriamine pentaacetic acid, diethylenetriamine pentaacetic acid pentasodium and diethylenetriamine pentaacetic acid pentapotassium, and the concentration is 0.1-3.0 mol/L.
The second complexing agent is one or more than two of hydrogen bromide, lithium bromide, potassium bromide, sodium bromide and ammonium bromide, and the concentration is 0.1-3.0 mol/L.
The concentration ratio of the total of the iron ions and the ferrous ions (or the total of the chromium ions and the sub-ions), the first complexing agent and the second complexing agent is 1:1 (0.1-2.5), preferably 1:1 (1.0-2.0), and more preferably 1:1: 1.
The supporting electrolyte is one or more than two of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and lithium hydroxide, and the concentration is 0.1-8 mol/L.
THE ADVANTAGES OF THE PRESENT INVENTION
Compared with the prior art, the invention has the following beneficial effects:
1. cr in the negative electrode electrolyte is added by an organic/inorganic composite complexing agent 3+ /Cr 2+ Ion conversion to (Br) Cr (DTPA) 3+ /(Br)Cr(DTPA) 2+ The problem of inactivation of the cathode electrolyte is solved, and the reaction activity and reversibility of the cathode electrolyte are improved, so that the efficiency and capacity retention rate of the battery are improved.
2. The positive and negative electrolytes adopt the same organic/inorganic composite complexing agent to form a solution containing (Br) Cr (DTPA) 3+ /(Br)Cr(DTPA) 2+ And a negative electrode electrolyte containing (Br) Fe (DTPA) 3+ /(Br)Fe(DTPA) 2+ The anode electrolyte increases the sizes of free chromium ions and free iron ions, solves the problems of electrolyte pollution, battery capacity attenuation and efficiency reduction caused by the fact that active ions of the anode electrolyte and the cathode electrolyte pass through the diaphragm, and accordingly improves the efficiency and prolongs the service life of the battery.
3. The electrolyte has low cost and simple operation, and can greatly improve the performance of the iron-chromium flow battery.
Drawings
Fig. 1 is a schematic diagram of an iron-chromium flow battery and a structure thereof. The negative current collector comprises a negative electrode liquid storage tank, a centrifugal pump, an end plate, a negative electrode current collector, a negative electrode, a diaphragm, a positive electrode current collector and a positive electrode liquid storage tank.
Fig. 2 is a graph comparing coulombic efficiency, voltage efficiency, and energy efficiency of the iron chromium flow batteries of example 1, example 2, and comparative example. As can be seen from fig. 2, the coulombic efficiency and the energy efficiency of examples 1 and 2 are higher than those of the comparative example. The energy efficiency of example 1 was as high as 82.1% compared to 4.8% for the comparative example. The energy efficiency of example 2 was as high as 78.9% which is 1.6% higher than the comparative example.
Fig. 3 is a graph comparing the capacity retention rate of the iron-chromium flow batteries according to the number of charge and discharge cycles in examples 1 and 2 and comparative examples. As can be seen from fig. 3, the capacity retention ratio of the batteries of examples 1 and 2 was stable and close to 100% in 100 charge/discharge cycles. In contrast, the capacity retention rate of the battery was only 28.4% in 100 charge/discharge cycles of the comparative example.
Detailed Description
Example 1
1. Preparation of electrolyte
1) Preparing a negative electrode electrolyte: 15.7g of diethylenetriaminepentaacetic acid was weighed into 150ml of deionized water and stirred uniformly to form a solution A. 6.3g of CrCl are subsequently weighed out 3 This was slowly added to solution a to obtain solution B. Subsequently, 10.7g of sodium carbonate and 2.4g of potassium bromide were added to the solution B to obtain a solution C. Transferring the solution C into a 200ml volumetric flask for constant volume to obtain 0.2mol/L CrCl cathode electrolyte containing complexing agent 3 +0.2mol/L DTPA+0.1mol/L KBr。
2) Preparing a positive electrolyte: 20.1g of diethylenetriaminepentaacetic acid are weighed out and added to 140ml of deionized water, followed by the further addition of 5.1g of FeCl 2 To obtain a solution A. Weighing 10.7g of sodium carbonate and 2.4g of potassium bromide, slowly adding the sodium carbonate and the potassium bromide into the solution A, completely dissolving, transferring into a 200ml volumetric flask for constant volume, and shaking up to obtain the anode electrolyte containing the complexing agent: 0.2mol/L FeCl 2 +0.2mol/L DTPA+0.1mol/L KBr。
2. Iron-chromium flow battery assembly
The iron-chromium flow battery is assembled by taking 70mL of the positive electrolyte and 70mL of the negative electrolyte respectively according to the form shown in FIG. 1. Wherein the ion exchange membrane is Nafion115 with an effective area of 9cm 2 . The positive and negative electrodes are carbon felts, and the thickness of the carbon felts is 3 mm. The positive and negative current collectors are carbon plates, and the connecting pipeline is an anti-corrosion pipeline with the inner diameter of 2 mm.
3. Iron-chromium flow battery performance test
At a current density of 40mA/cm 2 And carrying out constant current charge and discharge test under the temperature condition, wherein the charge cut-off condition is 1.65V or 30 minutes, and the discharge cut-off condition is 0.8V. And after the test is finished, obtaining the curve of the efficiency and the capacity of the battery along with the cycle number.
Example 2
1. Preparation of electrolyte
1) Preparing a negative electrode electrolyte: 201.2g of diethylenetriaminepentaacetic acid pentasodium and 106.6g of sodium carbonate were weighed into 150ml of deionized water and stirred uniformly to form solution A. 63.3g of CrCl were subsequently weighed 3 This was slowly added to the previous solution a to obtain solution B. Subsequently, 41.2g of sodium bromide was added to the solution B to obtain a solution C. Transferring the solution C into a volumetric flask of 200ml for constant volume to obtain the cathode electrolyte containing the complexing agent, wherein the volume of the cathode electrolyte is 2.0mol/L CrCl 3 +2.0mol/L DTPA+2.0mol/L NaBr。
2) Preparing a positive electrolyte: 201.2g of pentasodium diethylenetriaminepentaacetate are weighed out and added to 140ml of deionized water, followed by the further addition of 50.8g of FeCl 2 To obtain a solution A. Weighing 106.6g of sodium carbonate and 41.2g of sodium bromide, slowly adding the sodium carbonate and the sodium bromide into the solution A, completely dissolving, transferring the solution into a 200ml volumetric flask for constant volume, and shaking up to obtain the anode electrolyte containing the complexing agent: 2.0mol/L FeCl 2 +2.0mol/L DTPA+2.0mol/L NaBr。
2. Iron-chromium flow battery assembly
The iron-chromium flow battery is assembled by taking 70mL of the positive electrolyte and 70mL of the negative electrolyte respectively according to the form shown in FIG. 1. Wherein the ion exchange membrane is Nafion115 with an effective area of 9cm 2 . Is justThe negative electrode is a carbon felt, and the thickness of the carbon felt is 3 mm. The positive and negative current collectors are carbon plates, and the connecting pipeline is an anti-corrosion pipeline with the inner diameter of 2 mm.
3. Iron-chromium flow battery performance test
At a current density of 40mA/cm 2 And carrying out constant current charge and discharge test under the temperature condition, wherein the charge cut-off condition is 1.65V or 60 minutes, and the discharge cut-off condition is 0.8V. And after the test is finished, obtaining the curve of the efficiency and the capacity of the battery along with the cycle number.
Comparative example 1
1. Electrolyte solution preparation
1) Preparation of negative electrode electrolyte: 65ml of concentrated hydrochloric acid are weighed into 150ml of deionized water, followed by 47.5g of CrCl 3 After the solid is completely dissolved, transferring the solid into a 200ml volumetric flask for constant volume to obtain 1.5mol/L CrCl of the negative electrode electrolyte 3 +3.0mol/L HCl。
2) Preparing a positive electrolyte: 65ml of concentrated HCl was weighed into 150ml of deionized water, followed by 38.1g of FeCl 2 After the solid is completely dissolved, transferring the solid into a volumetric flask of 200ml for constant volume to obtain 1.5mol/L FeCl of the positive electrolyte 2 +3.0mol/L HCl。
2. Iron-chromium flow battery assembly
The iron-chromium flow battery is assembled by taking 70mL of the positive electrolyte and 70mL of the negative electrolyte respectively according to the form shown in FIG. 1. Wherein the ion exchange membrane is Nafion115 with an effective area of 9cm 2 . The positive and negative electrodes are carbon felts, and the thickness of the carbon felts is 3 mm. The positive and negative current collectors are carbon plates, and the connecting pipeline is an anti-corrosion pipeline with the inner diameter of 2 mm.
3. Iron-chromium flow battery performance test
At a current density of 40mA/cm 2 And carrying out constant current charge and discharge test under the temperature condition, wherein the charge cut-off condition is 1.6V, and the discharge cut-off condition is 0.8V. And after the test is finished, obtaining the curve of the efficiency and the capacity of the battery along with the cycle number.

Claims (8)

1. The iron-chromium flow battery electrolyte containing complexing agents is characterized in that a negative electrolyte comprises trivalent chromium ions, divalent chromium ions, a first complexing agent, a second complexing agent, a supporting electrolyte and water, a positive electrolyte comprises iron ions, ferrous ions, the first complexing agent, the second complexing agent, the supporting electrolyte and water, the same first complexing agent and the same second complexing agent are adopted in the positive electrolyte and the negative electrolyte and are respectively complexed with the iron ions and the ferrous ions or the trivalent chromium ions and the divalent chromium ions, the first complexing agent is diethylenetriamine pentaacetic acid (DTPA) or salt thereof, preferably diethylenetriamine pentaacetic acid (DTPA), and the second complexing agent is bromide, preferably potassium bromide.
2. The iron-chromium flow battery electrolyte containing the complexing agent as claimed in claim 1, wherein the material containing trivalent chromium ions can be one or more than two of chromium trichloride, dichromium trithioate and chromium trinitrate, and the concentration is 0.1-2.0 mol/L.
3. The iron-chromium flow battery electrolyte containing the complexing agent as claimed in claim 1, wherein the substance containing divalent chromium ions can be one or two of chromium dichloride and chromium sulfate, and the concentration is 0.1-2.0 mol/L.
4. The iron-chromium flow battery electrolyte containing the complexing agent as recited in claim 1, wherein the substance containing iron ions can be one or more than two of ferric chloride, ferric sulfate and ferric nitrate, and the concentration is 0.1-2.0 mol/L.
5. The iron-chromium flow battery electrolyte containing the complexing agent as claimed in claim 1, wherein the substance containing ferrous ions can be one or more than two of ferrous chloride, ferrous sulfate and ferrous nitrate, and the concentration is 0.1-2.0 mol/L.
6. The iron-chromium flow battery electrolyte containing the complexing agent as claimed in claim 1, wherein the first complexing agent is one or more than two of diethylenetriamine pentaacetic acid, diethylenetriamine pentaacetic acid pentasodium and diethylenetriamine pentaacetic acid pentapotassium, and the concentration is 0.1-3.0 mol/L.
7. The iron-chromium flow battery electrolyte containing the complexing agent as recited in claim 1, wherein the second complexing agent is one or more than two of hydrogen bromide, lithium bromide, potassium bromide, sodium bromide and ammonium bromide, and the concentration is 0.1-3.0 mol/L.
8. The iron-chromium flow battery electrolyte containing the complexing agent as claimed in claim 1, wherein the supporting electrolyte is one or more than two of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and lithium hydroxide, and the concentration is 0.1-8 mol/L.
CN202210516829.1A 2022-05-12 2022-05-12 Iron-chromium flow battery electrolyte containing complexing agent Pending CN114865066A (en)

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