WO2015111815A1 - Composition électrolytique contenant un acide organique et batterie rédox la comprenant - Google Patents

Composition électrolytique contenant un acide organique et batterie rédox la comprenant Download PDF

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Publication number
WO2015111815A1
WO2015111815A1 PCT/KR2014/008245 KR2014008245W WO2015111815A1 WO 2015111815 A1 WO2015111815 A1 WO 2015111815A1 KR 2014008245 W KR2014008245 W KR 2014008245W WO 2015111815 A1 WO2015111815 A1 WO 2015111815A1
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acid
electrolyte
redox flow
flow battery
active material
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English (en)
Korean (ko)
Inventor
설용건
이진구
박세준
조용일
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University Industry Foundation UIF of Yonsei University
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University Industry Foundation UIF of Yonsei University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/20—Indirect fuel cells, e.g. fuel cells with redox couple being irreversible
    • 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
    • H01M8/02—Details
    • 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
    • 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
    • H01M2300/0002—Aqueous electrolytes
    • H01M2300/0005—Acid 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

Definitions

  • the present invention relates to an electrolyte composition and a redox flow battery using the same.
  • Redox flow battery is a very efficient technology for power storage because it can increase the amount of power storage by a simple method of increasing the amount of electrolyte.
  • the redox flow battery is charged and discharged by supplying a positive electrolyte solution and a negative electrolyte solution to a battery cell having a separator interposed between the positive electrode and the negative electrode.
  • a positive electrolyte solution an aqueous solution containing a water-soluble metal ion in which the valence is typically changed by redox is used, and this metal ion is used as an electrode active material.
  • Such redox flow batteries may be of a kind such as Cr / Cr, V / Sn, V / Fe, and V / V, depending on the redox couple.
  • Redox flow batteries have the ability to store intermittent energy supply and demand, like other batteries, but have a small change in the capacity to store energy over time, and have the advantage of producing electricity by reacting as needed.
  • the redox flow battery has been disadvantageous in that it is large, expensive, and difficult to control at an appropriate temperature.However, through the vanadium redox flow battery (VRB), the life, reaction time and charge / discharge Attempts have been made at various angles to solve the efficiency problem.
  • VRB vanadium redox flow battery
  • the existing vanadium redox flow battery uses sulfuric acid or hydrochloric acid as a solvent of an electrolyte solution.
  • sulfuric acid or hydrochloric acid having such a high acidity tends to corrode the cell, thereby degrading battery performance.
  • secondary acidity may occur due to high acidity when the electrolyte flows out, resulting in low battery stability.
  • An object of the present invention is to provide an electrolyte solution composition comprising an active material and an organic acid having at least one carboxyl group.
  • Another object of the present invention is to provide an electrolyte composition for a redox flow battery comprising an active material and an organic acid having at least one carboxyl group.
  • Still another object of the present invention is to provide a redox flow battery having improved cell corrosion and charging capacity, including the electrolyte composition.
  • an electrolyte composition comprising an organic acid having at least one carboxyl group.
  • It provides an electrolyte solution composition for a redox flow battery comprising an organic acid having at least one carboxyl group.
  • a positive electrode cell including a positive electrode and a positive electrolyte
  • a negative electrode cell including a negative electrode and a negative electrolyte
  • a separator separating the positive cell and the negative cell
  • At least one of the positive electrode electrolyte and the negative electrode electrolyte provides a redox flow battery including an organic acid including at least one carboxyl group.
  • the electrolyte composition according to the present invention may improve the corrosion of the cell by including an organic acid having one or more carboxyl groups, instead of including inorganic acids such as sulfuric acid or hydrochloric acid having high acidity, and may improve the stability of the battery when the electrolyte flows out. have.
  • an organic acid having one or more carboxyl groups instead of including inorganic acids such as sulfuric acid or hydrochloric acid having high acidity
  • inorganic acids such as sulfuric acid or hydrochloric acid having high acidity
  • FIG. 1 is a structural diagram showing the structure of a redox flow battery according to an embodiment of the present invention.
  • FIGS. 2 and 3 are graphs showing a cyclic voltage current curve (CV) of a redox flow battery using an electrolyte according to an embodiment and a comparative example of the present invention.
  • FIGS. 4 and 5 are graphs of a cyclic voltage current curve (CV) of a redox flow battery using an electrolyte according to another exemplary embodiment of the present invention.
  • FIG. 6 is a graph showing a change in battery voltage with charge and discharge time of a redox flow battery using an electrolyte according to an embodiment and a comparative example of the present invention.
  • FIG. 7 is a graph showing the charge and discharge capacity of the redox flow battery using an electrolyte according to an embodiment and a comparative example of the present invention.
  • FIG. 8 is a graph showing the coulombic efficiency and energy efficiency of the redox flow battery using the electrolyte according to an embodiment and a comparative example of the present invention.
  • V battery voltage
  • h cycle time
  • the present invention is an active material; Provided is an electrolyte composition comprising an organic acid having at least one carboxyl group.
  • organic acid electrolyte means an electrolyte containing an organic acid as a main component as an acidic component, and an existing electrolyte containing an inorganic acid such as sulfuric acid or hydrochloric acid as a main component as an acidic component. Contrast with.
  • “contains as a main component” means that the content of the corresponding organic acid with respect to the total acidic component is 95% or more, 99% or more, or 99.9% or more.
  • the active material according to the present invention may use any conventional metal compound used in a redox flow battery without limitation.
  • the active material may use a vanadium compound of + 2-valent to + 5-valent.
  • formic acid formic acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, hexanoic acid, heptanoic acid, heptanoic acid ), Caprylic acid, nonanoic acid, decanoic acid, undecylenic acid, lauric acid, tridecylic acid, myristic acid linear saturated carboxylic acids having one carboxyl group such as myristic acid, pentadecanoic acid, and palmitic acid; Oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, Saturated aliphatic dicarboxylic acids such as azelaic acid, or sebacic acid; Unsaturated aliphatic dicarboxylic acids such as maleic acid, fumaric acid, glutaconic acid, traumatic acid, or muconic acid
  • unsaturated aliphatic dicarboxylic acids such as maleic acid, fumaric acid, glutaconic acid, glutaconic acid, traumatic acid, or muconic acid; Three or more carboxyl groups such as citric acid, isocitric acid, aconitic acid, carballylic acid, tribasic acid, or melictic acid Carboxylic acid having; Or oxalic acid, malonic acid, malic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid Saturated aliphatic dicarboxylic acids, such as azelaic acid, or sebacic acid, may be used, more specifically maleic acid, citric acid or oxalic acid. It may be used, and more specifically oxalic acid may be used.
  • the organic acid according to the present invention may form a chelate structure with vanadium ions in the electrolyte composition, and the chelate structure may serve to increase the charge / discharge capacity of the battery. Moreover, the said organic acid can aim at the improvement of stability and reactivity of vanadium ion, suppression of side reaction, reduction of internal resistance, etc.
  • the organic acid is not particularly limited in form, but may have a form of a solution dissolved in an organic solvent or water.
  • acetone for example, methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, etc.
  • IPA isopropyl alcohol
  • the concentration of the organic acid in the electrolyte composition may be 1 to 5 M, 1 to 3 M or 1 to 2 M.
  • the pH of the electrolyte composition may be in the range of 2 to 5, for example.
  • the pH of the electrolyte composition when the pH of the electrolyte composition is within the above range, the corrosion resistance is low, the cell stability is excellent, and the efficiency of the battery such as the charge / discharge capacity is not impaired.
  • the present invention is an active material; It provides an electrolyte solution composition for a redox flow battery comprising an organic acid having at least one carboxyl group.
  • the electrolyte composition for a flow battery according to the present invention includes organic acids having at least one carboxyl group instead of inorganic acids such as sulfuric acid or hydrochloric acid having high acidity, thereby improving corrosion of the cell, and improving battery stability when the electrolyte is leaked. You can. In addition to the charge and discharge capacity of the redox flow battery, it is excellent in the effect of reducing the corrosion of the ion exchange membrane and the current collector to improve the life of the battery.
  • the present invention is a positive electrode cell comprising a positive electrode and a positive electrode electrolyte
  • a negative electrode cell including a negative electrode and a negative electrolyte
  • a separator separating the positive cell and the negative cell
  • At least one of the positive electrode electrolyte and the negative electrode electrolyte provides a redox flow battery including an organic acid including at least one carboxyl group.
  • the cathode electrolyte may include an organic acid including a cathode active material and one or more carboxyl groups, and the cathode active material may include vanadium ions having an oxidation number of +4 to +5.
  • the positive electrode active material may be (VO 2 ) SO 4 , VO (SO 4 ) or a combination thereof.
  • the cathode active material may be present in a cathode electrolyte composition at a concentration of 1 M to 10 M.
  • concentration of the positive electrode active material is included in the range, there is an advantage that can implement a high energy density and high power density. If the concentration of the positive electrode active material is lower than 1 M, the amount of positive electrode active material per unit volume may be low, and the energy density may be reduced. If the concentration of the positive electrode active material is higher than 10 M, the viscosity of the positive electrode active material may increase rapidly, and the oxidation / reduction reaction rate may be significantly reduced. The power density may be reduced.
  • the negative electrode electrolyte may include an organic acid including a negative electrode active material and one or more carboxyl groups, and the negative electrode active material may include vanadium ions having an oxidation number of +2 to +4.
  • the negative electrode active material may be a + 2-valent to + trivalent vanadium-based compound, and examples of the negative electrode active material include VSO 4 , VO 2 (SO 4 ) 3, or a combination thereof.
  • the negative electrode active material may be present in a negative electrode electrolyte composition at a concentration of 1 M to 10 M.
  • concentration of the negative electrode active material is included in the range, there is an advantage that can implement a high energy density and high power density. If the concentration of the negative electrode active material is lower than 1 M, the amount of the negative electrode active material per unit volume may be low, and the energy density may be reduced. If the concentration of the negative electrode active material is higher than 10 M, the viscosity of the negative electrode active material is rapidly increased, and the oxidation / reduction reaction rate is significantly reduced. The power density may be reduced.
  • the electrolyte composition according to the present invention may further contain other metal ions other than the vanadium metal component, thereby improving the utilization rate of vanadium ions.
  • the redox flow battery according to the present invention includes an organic acid having one or more carboxyl groups in any one or more of the positive electrode electrolyte and the negative electrode electrolyte, thereby improving the charge and discharge capacity of the redox flow battery and the life of the battery, solar light It can be usefully used in power storage devices used in the energy field, such as generators, wind generators.
  • the redox flow battery 100 typically includes a power generation unit (eg, a solar generator, a wind generator, and other general power plants) through an AC / DC converter. And a load such as a power system or a consumer, are charged using the power generation unit as a power supply source, and discharged using the load as a power supply target.
  • a power generation unit eg, a solar generator, a wind generator, and other general power plants
  • a load such as a power system or a consumer
  • the following battery system including the redox flow battery 100 and a circulation mechanism (tank, pipe, pump) for circulating the electrolyte in the battery 100 is constructed.
  • the redox flow battery 100 includes a cathode cell 20 incorporating the anode electrode 21, a cathode cell 30 incorporating the cathode electrode 31, and a separation membrane separating the two cells 20 and 30.
  • the ion exchange membrane 40 which selectively permeates ions is provided.
  • a positive electrode electrolyte tank 50 is connected to the positive cell 20 via a pipe 51.
  • a negative electrode electrolyte tank 60 is connected to the negative electrode cell 30 through a pipe 61.
  • the pipes 51 and 61 are provided with pumps 52 and 62 for circulating the electrolyte at each pole.
  • the redox flow battery 100 uses the piping 51 and 61 and the pumps 52 and 62, and the anode cell 20 (anode electrode 21) and the cathode cell 30 (cathode electrode 31) are used. ], The anode electrolyte of the tank 50 and the cathode electrolyte of the tank 60 are circulated and supplied, respectively, and charge / discharge is performed according to the valence change reaction of the metal ion used as the electrode active material in the electrolyte of each electrode.
  • the ion exchange membrane 40 of the redox flow secondary battery 100 may be formed of nafion.
  • the cathode electrode 31 and the anode electrode 21 may be used that the carbon layer is uniformly coated on the porous metal surface, for example, carbon felt may be used, platinum as a counter electrode (counter electrode) Can be used.
  • An electrolyte was prepared in the same manner as in Example 1, except that 12 g of maleic acid powder was used instead of oxalic acid powder. At this time, the pH of the electrolyte solution prepared in Example 2 is 3.7.
  • An electrolyte was prepared in the same manner as in Example 1, except that 19.2 g of citric acid powder was used instead of oxalic acid powder. At this time, the pH of the electrolyte solution prepared in Example 2 is 3.6.
  • An electrolyte was prepared in the same manner as in Example 1, except that an aqueous sulfuric acid solution was used instead of an organic acid solution. At this time, the pH of the electrolyte solution prepared in Comparative Example 1 is 0.5.
  • Measurement 1 Using the electrolyte solution obtained in Examples 1 to 3 and Comparative Example 1, the potential scan rate was 100 mV / s at room temperature, and the potential scan range was 0 to 1.65 V. The change was measured.
  • the cell for measuring the cyclic voltammogram curve used silver-silver chloride electrode (Ag / AgCl) as the reference electrode, graphite electrode as the working electrode, and anion exchange membrane as the ion exchange membrane. Used. Cyclic voltammograms (CV) for the cells measured under these conditions are shown in FIGS.
  • Measurement 2 Cyclic Voltammetry by using carbon felt as working electrode and carrying out under the same conditions as the measurement 1 except that the potential scanning range was 0 to 1.3 V. , CV) was measured, and the results are shown in FIG. 5.
  • the electrolyte according to Example 1 of the present invention is superior to Comparative Example 1 using inorganic acid sulfuric acid as a solvent of the electrolyte, it is excellent in the redox characteristics of the electrolyte regardless of the type of electrode You can check it.
  • Measurement 1 The electrolyte solution prepared in Example 1 was charged in 10 mL portions of the positive and negative electrode electrolyte tanks, and purged with nitrogen to block contact with external air and seal it.
  • the electrolyte solution which is blocked from contact with the sealed external air at room temperature conditions, is controlled at a constant rate of 3 to 4 mL / min, and the inflow rate is controlled to flow into 3 cm * 3 cm carbon felt (electrode reaction area of 9 cm 2).
  • the current scan rate to adjust the charge and discharge rate of the redox flow battery was constantly adjusted to about 250 mA. Furthermore, as shown in FIG.
  • Charging and discharging were performed using a low current scanning rate of 50 mA / cm 2 or less, and the current scanning rate controlling the charging and discharging speed of the redox flow battery was measured, and the voltage, the discharge capacity, and the charging capacity were measured. In addition, under the same conditions, voltage, discharge capacity, and charge capacity during charge and discharge of the redox flow battery including the electrolyte solution prepared in Comparative Example 1 were measured.
  • Voltage efficiency (%) (average voltage at discharge / average voltage at charge) ⁇ 100
  • the redox flow battery including the electrolyte solution prepared in Example 1 has a larger charge / discharge capacity than the battery including the electrolyte solution prepared in Comparative Example 1, and It can be seen that the charging time is faster. In addition, it can be seen that the energy efficiency is excellent due to this. From these results, it can be seen that the electrolyte composition according to the present invention can significantly improve the charge and discharge capacity and energy efficiency of the redox flow battery.
  • the redox flow battery including the electrolyte solution prepared in Example 1 was confirmed to maintain a constant charge / discharge voltage even after repeated charging and discharging. From these results, it can be seen that the electrolyte solution composition according to the present invention improves battery life when used in a redox flow battery.
  • the electrolyte composition according to the present invention includes organic acids having at least one carboxyl group instead of inorganic acids such as sulfuric acid or hydrochloric acid having high acidity, thereby improving corrosion of the cells and improving stability of the battery when the electrolyte is leaked. Can be.
  • organic acids having at least one carboxyl group instead of inorganic acids such as sulfuric acid or hydrochloric acid having high acidity, thereby improving corrosion of the cells and improving stability of the battery when the electrolyte is leaked.
  • inorganic acids such as sulfuric acid or hydrochloric acid having high acidity

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

La présente invention concerne une composition électrolytique contenant un matériau actif et un acide organique comportant un ou plusieurs groupes acide carboxylique, et une batterie rédox l'utilisant. La composition électrolytique selon la présente invention contient l'acide organique comportant un ou plusieurs groupes acide carboxylique à la place d'un acide inorganique ayant une acidité élevée tel qu'un acide sulfurique et un acide chlorhydrique, ce qui permet d'améliorer la corrosion des piles et d'améliorer la stabilité de la batterie en cas de fuite de l'électrolyte. De plus, quand elle est appliquée à la batterie rédox, la composition électrolytique améliore la capacité de charge et de décharge et augmente également la durée de vie de la batterie par réduction de la corrosion d'une membrane échangeuse d'ions et d'un collecteur de courant.
PCT/KR2014/008245 2014-01-23 2014-09-03 Composition électrolytique contenant un acide organique et batterie rédox la comprenant Ceased WO2015111815A1 (fr)

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KR10-2014-0008449 2014-01-23
KR1020140008449A KR101577888B1 (ko) 2014-01-23 2014-01-23 유기산을 포함하는 전해액 조성물 및 이를 포함하는 레독스 플로우 전지

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Cited By (2)

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CN111653799A (zh) * 2020-07-16 2020-09-11 盐城工学院 一种锡基碱性液流电池锡负极的预处理方法
CN112599827A (zh) * 2020-12-08 2021-04-02 贵州聚能世纪科技有限责任公司 一种提高钒电池低温稳定性的电解液外加剂及其制备方法

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KR20250136550A (ko) * 2024-03-08 2025-09-16 스탠다드에너지(주) 바나듐 전해액, 이의 제조방법, 및 이를 포함하는 이차전지

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US20130095362A1 (en) * 2011-10-14 2013-04-18 Deeya Energy, Inc. Vanadium flow cell
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CN111653799A (zh) * 2020-07-16 2020-09-11 盐城工学院 一种锡基碱性液流电池锡负极的预处理方法
CN111653799B (zh) * 2020-07-16 2022-03-15 盐城工学院 一种锡基碱性液流电池锡负极的预处理方法
CN112599827A (zh) * 2020-12-08 2021-04-02 贵州聚能世纪科技有限责任公司 一种提高钒电池低温稳定性的电解液外加剂及其制备方法
CN112599827B (zh) * 2020-12-08 2021-11-26 贵州聚能世纪科技有限责任公司 一种提高钒电池低温稳定性的电解液外加剂及其制备方法

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