CN115579502A - Aqueous semi-solid alkaline organic flow battery - Google Patents
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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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- H01M2300/0014—Alkaline electrolytes
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Abstract
The invention relates to the field of flow batteries, in particular to a water system semi-solid alkaline organic flow battery. The cathode active electrolyte of the battery is 2-hydroxy-3-pyrrole anthraquinone, the diaphragm is a cation conductive film, and the anode active electrolyte is an oxidation reduction active inorganic substance. The additive for improving the specific capacity of the negative electrolyte solution is one or a mixture of more of choline, cyclodextrin, nicotinamide and urea. The water system semi-solid alkaline organic flow battery has the advantages of low manufacturing cost, high capacity, long-term energy storage, safety, environmental protection and the like, and has wide application prospects in the fields of power grid peak shaving and large-scale storage of renewable energy sources.
Description
Technical Field
The invention relates to the field of flow batteries, in particular to a water system semi-solid alkaline organic flow battery.
Background
With the rapid development of distributed power generation technologies such as solar energy and wind energy, various large-scale energy storage technologies are needed to stabilize input and output of a power grid system, regulate shortage and reduce energy waste (adv.
Flow batteries achieve energy storage and conversion through valence state transitions between different redox active species. The redox active species is stored in an external storage tank and fed to the cell system by a circulation pump, so that its energy and power can be designed independently of each other (chem. Rev.2015, 115, 11533).
The unique battery structure based on the liquid electrolyte, namely the flow battery, has the advantages of easiness in expansion and modularization, and shows a huge application prospect in the fields of scale utilization of renewable energy sources, power grid peak regulation and the like (J.electrochem.Soc.2011, 158, R55; adv.Mater.2019, 31, 1902025).
In the existing flow battery system, the all-vanadium flow battery has good electrochemical reversibility and high power density, and is not limited by cross permeation of positive and negative active species, so that the all-vanadium flow battery becomes a water-based flow battery which is firstly commercially operated (int.j.energy res.2010, 34, 182, energy stor.mater.2020, 24, 529. However, the application of the all-vanadium redox flow battery is still restricted by high cost, the vanadium-based electrolyte has strong toxicity, and the solubility of vanadium oxide species of the positive electrode is in negative correlation with temperature, so that the working temperature range of the battery is limited (10-40 ℃) (J.Power Sources 2017, 360, 243 J.Electrochem.Soc.2011, 158, R55; CN 201780040304.2).
The mixed liquid flow battery uses a solid electrodeless (or organic) electrode material with high specific capacity to combine with a liquid redox electrolyte, can obviously improve energy density, and has the advantages of high power density and low cost.
However, solid electrode materials (such as zinc) are prone to morphology change, dendrite growth, passivation and parasitic side reactions during charge and discharge cycles, thereby affecting cycle life (CN 202011260954.8 j. Power sources,2008, 184, 610;).
In order to increase energy density and expand the application range of flow batteries, the Yet-Ming Chiang group developed a semi-solid lithium ion flow battery, i.e., the solubility limit of redox species was broken through by using a flowable "slurry" electroactive material on the positive electrode side (adv. However, such "slurry" fluids are generally of relatively high viscosity, resulting in a significant increase in the power consumption of the circulation pump.
Recently, the Yang shano-Horn group developed a zinc-manganese dioxide semi-solid flow battery (Joule, 2021,5, 2934). The power consumption of the circulating pump is reduced through the structural design, and compared with a lithium ion battery and a vanadium flow battery, the slurry type flow battery system has the obvious advantages of low cost and long-term energy storage, but the circulating life of the slurry type flow battery system still cannot meet the requirement of practical application.
Disclosure of Invention
The invention aims to provide a water system semi-solid alkaline organic flow battery with high specific capacity and low cost.
In order to achieve the purpose, the invention provides an aqueous semi-solid alkaline organic flow battery, which comprises a negative electrode electrolyte system, a diaphragm, a positive electrode electrolyte solution, a conductive electrode, a storage tank and a pump, wherein the negative electrode electrolyte system is a negative electrode electrolyte system with stable suspension state and contains anthraquinone derivatives with high negative potential, additives and alkaline supporting electrolyte.
The cathode electrolyte system contains 2-hydroxy-3-pyrrole anthraquinone as the electroactive material. The content of the 2-hydroxy-3-pyrrole anthraquinone is 0.1 to 1mol/L. The preferred content is 0.1 to 0.5mol/L.
The additive of the negative electrode electrolyte system is one or a mixture of choline, cyclodextrin, nicotinamide and urea. The preferred additive is choline. The content of the additive is 0.01-1 mol/L. The content of the additive is preferably 0.05 to 0.5mol/L.
The positive electrolyte solution is an aqueous solution comprising a redox active inorganic substance and an alkaline supporting electrolyte. Wherein the redox active inorganic substance is one or mixture of potassium ferrocyanide, sodium ferrocyanide and ammonium ferrocyanide. The concentration of the ferrocyanide in the positive electrolyte solution is 0.1-1.2 mol/L. The preferable concentration of ferrocyanide is 0.2 to 0.8mol/L.
Both the negative electrolyte system and the positive electrolyte solution comprise an alkaline supporting electrolyte. The alkaline supporting electrolyte is one of potassium hydroxide, sodium hydroxide and lithium hydroxide or a mixture of the potassium hydroxide, the sodium hydroxide and the lithium hydroxide. Preferably, the basic supporting electrolyte is potassium hydroxide. The concentration of the alkaline supporting electrolyte is 0.01-2 mol/L. The preferred concentration of the alkaline supporting electrolyte is 0.1 to 1mol/L.
Conductive electrodes include any carbon-based electrode such as carbon paper, carbon cloth, carbon felt. Titanium nitride electrodes may also be used. Other electrodes suitable for use are known in the art.
The membrane is a cation-conducting membrane that allows hydrated cations to pass through, but blocks larger sized anions or other redox active species from passing through. Examples are Nafion series membranes (i.e. perfluorosulfonic acid membranes).
The flow battery of the present invention may include additional components known in the art. The redox active substance dissolved or dispersed in the aqueous solution will be contained in a suitable reservoir. The cell also includes a circulation pump to deliver the aqueous solution to both electrode surfaces. The cell also includes a flow field plate and a metal current collector.
The beneficial results of the invention are: the redox active substance of the negative electrode used in the invention has stable chemical structure, and is beneficial to maintaining the stability of the battery in long-term charge-discharge circulation; the used additive can improve the effective concentration of anthraquinone redox substances and the stability of an electrolyte system, thereby improving the energy density of the battery. The battery has the advantages of simple process, low manufacturing cost, safety, environmental protection and universality and flexibility in the design of the electrolyte.
Description of the drawings:
FIG. 1 is a scheme for the synthesis of 2-hydroxy-3-pyrrolanthraquinone of example 1.
FIG. 2 is a nuclear magnetic resonance hydrogen spectrum of 2-hydroxy-3-pyrrol-anthraquinone of example 1: ( 1 H NMR) figure.
FIG. 3 is a cyclic voltammogram of 2-hydroxy-3-pyrrolidinone of example 1 (0.001 mol/L) at different sweep rates in a 1mol/LKOH solution on a glassy carbon electrode.
FIG. 4 is a 100mVs solution of 2-hydroxy-3-pyrrolidinoanthraquinone (0.001 mol/L) from example 1 in 1mol/LKOH solution on a glassy carbon electrode -1 Cyclic voltammogram at the lower 100 cycles.
FIG. 5 is a linear sweep voltammogram of 2-hydroxy-3-pyrrolidinone (0.001 mol/L) from example 1 at various electrode rotation speeds in a 1mol/LKOH solution on a glassy carbon electrode.
FIG. 6 (a) is a Koutecky-Levich plot of 2-hydroxy-3-pyrrolidinone of example 1 (0.001 mol/L) at 6 overpotentials in a 1mol/LKOH solution on a glassy carbon electrode; and (b) is a corresponding Tafel relationship diagram.
FIG. 7 (a) is a cyclic voltammogram of 2-hydroxy-3-pyrrolanthraquinone (0.001 mol/L) of example 1 in KOH solutions of different concentrations on a glassy carbon electrode; (b) Is the corresponding standard potential (E) 0 ) -pH dependence diagram.
Fig. 8 is a schematic diagram of an aqueous semi-solid alkaline organic flow cell based on a 2-hydroxy-3-pyrrolidinone (HPyAQ) catholyte negative electrolyte of example 3.
Fig. 9 is a graph of rate performance (a) and cycle life/efficiency for the aqueous semi-solid alkaline organic flow battery based on 2-hydroxy-3-pyrrolidinone (HpyAQ) negative electrode electrolyte (0.1 mol/L) of example 3.
Fig. 10 is a graph of rate performance (a) and cycle life/efficiency for the aqueous semi-solid alkaline organic flow battery of example 3 based on 2-hydroxy-3-pyrrolidinone (HpyAQ) negative electrode electrolyte (0.2 mol/L).
Detailed Description
The present invention will be described in detail with reference to specific examples.
EXAMPLE 1 Synthesis of 2-hydroxy-3-Pyrroloanthraquinone and its electrochemical Properties
2-amino-3-hydroxyanthraquinone (0.947g, 4.03mmol), 2, 5-dimethoxytetrahydrofuran (1.05mL, 8.06mmol), elemental iodine (0.102g, 0.40mmol), 90mL of N, N-Dimethylformamide (DMF), and 3.6mL of water were added to a three-necked flask in this order. Heating to 120 ℃, and refluxing for reaction for 3h. Cooling to room temperature, adding 300mL of water, stirring, precipitating, standing for 2h, performing suction filtration to obtain a yellow solid, washing with warm water for 3 times, and vacuum drying at 60 ℃ for 12h to obtain the product 2-hydroxy-3-pyrrole anthraquinone (yield 90%).
FIG. 1 is a scheme showing the synthesis of 2-hydroxy-3-pyrrolidinone (HpyAQ).
FIG. 2 is a schematic representation of 2-hydroxy-3-pyrrol-anthraquinone 1 H NMR spectrum (. Delta. (ppm): 11.77 (s, -OH), 8.17 (d, 1H), 7.99 (d, 2H), 7.91 (d, 2H), 7.77 (d, 1H), 7.34 (d, 2H), 6.31 (t, 2H)).
The electrochemical properties of 2-hydroxy-3-pyrrol-anthraquinone were tested using cyclic voltammetry techniques and a standard three-electrode system. The working electrode is a glassy carbon electrode, the counter electrode is a platinum sheet electrode, and the reference electrode is a mercury/mercury oxide electrode (MMO, 0.098V relative standard hydrogen electrode). The electrolyte solution is 0.001 mol/L2-hydroxy-3-pyrrole anthraquinone solution dissolved in 1mol/L KOH. Prior to testing, nitrogen was bubbled through the electrolyte solution to exclude dissolved oxygen. The test was carried out in a nitrogen atmosphere throughout the course of the test.
FIG. 3 shows 2-hydroxy-3-pyrrol-anthraquinone (0.001 mol/L) on glass at different sweep ratesCyclic voltammograms in 1mol/LKOH on carbon electrodes. FIG. 3 is a CV curve of 2-hydroxy-3-pyrrol-anthraquinone showing a pair of reversible redox peaks, the standard potential E of which 0 It was-0.59V.
FIG. 4 is a graph of 100mVs of 2-hydroxy-3-pyrrolanthraquinone (0.001 mol/L) in 1mol/L KOH on glassy carbon electrodes -1 Cyclic voltammogram for the next 100 cycles. 2-hydroxy-3-pyrrol-anthraquinone exhibits high redox stability.
FIG. 5 is a linear scanning voltammogram of 2-hydroxy-3-pyrrol-anthraquinone (0.001 mol/L) in 1mol/L KOH solution on a glassy carbon electrode at different electrode rotation speeds.
FIG. 6 (a) is a Koutecky-Levich plot of 2-hydroxy-3-pyrrol-anthraquinone (0.001 mol/L) at 6 overpotentials in 1mol/L KOH solution on a glassy carbon electrode, while FIG. 6 (b) is the corresponding Tafel relationship plot. The standard rate constant of 2-hydroxy-3-pyrrol-anthraquinone was 7.67X 10 -2 cm s -1 。
FIG. 7 (a) is a cyclic voltammogram of 2-hydroxy-3-pyrrol-anthraquinone (0.001 mol/L) in KOH solutions of different concentrations. FIG. 7 (b) shows the corresponding standard potential (E) 0 ) -pH diagram. E 0 The relationship with pH corresponds to the Nernst equation at pH>13.2 the electrochemical reaction of 2-hydroxy-3-pyrrole anthraquinone in the alkaline medium is a reversible 2 electron 1 proton process.
EXAMPLE 2 stability of 2-hydroxy-3-Pyrrolanthraquinone suspensions in alkaline systems
The solubility of 2-hydroxy-3-pyrrole anthraquinone in 1mol/L KOH at room temperature is about 0.04mol/L through the measurement of an ultraviolet spectroscopy technology. Solubility experiments, however, have shown that relatively stable suspensions can still be formed in 1mol/L KOH when the amount of 2-hydroxy-3-pyrrolidinone is slightly more than 0.04mol/L (Table 1). Respectively adding different additives into 2mL of KOH (1 mol/L) solution of 2-hydroxy-3-pyrrole anthraquinone, wherein the types and the concentrations of the additives are shown in Table 1, fully mixing, uniformly stirring by ultrasonic assistance, standing with a blank sample, observing the state of a suspension, and inspecting the influence of different additives on the stability of the 2-hydroxy-3-pyrrole anthraquinone suspension.
The results are shown in Table 1. When no additive is added, the stability time of the suspension is more than 72 hours when the concentration of the 2-hydroxy-3-pyrrole anthraquinone is 0.1 mol/L; as the concentration of 2-hydroxy-3-pyrrol-anthraquinone increased to 0.2 and 0.4mol/L, the stabilization time was shortened to 24 and about 6 hours, respectively. After 0.2mol/L choline is added into the suspension with the concentration of 0.2 mol/L2-hydroxy-3-pyrrol-anthraquinone, the stabilization time is improved from 24 hours to more than 72 hours, and other additives (cyclodextrin, nicotinamide and urea) have similar effects, which shows that the additive can effectively improve the dispersibility of the 2-hydroxy-3-pyrrol-anthraquinone.
TABLE 1 stability of 2-hydroxy-3-pyrrol-anthraquinone suspensions at room temperature
Note: the stabilization time is the time at which a large number of solid precipitates appear in the suspension.
Example 3
Additive-free aqueous semi-solid alkaline organic flow battery with 2-hydroxy-3-pyrrole anthraquinone cathode electrolyte
2-hydroxy-3-pyrrole anthraquinone suspension without additives is used as a negative electrolyte, potassium ferrocyanide solution is used as a positive electrolyte (supporting electrolytes of the positive electrolyte and the negative electrolyte are KOH), a carbon felt electrode is used as a conductive electrode, and a Nafion112 perfluorosulfonic acid film is used as a diaphragm, so that a single cell system of a semi-solid organic flow battery is constructed [ J.Mater.chem.A., 2021,9 and 26709; ACS Energy lett.2020,5,411; adv. Energy mater.2017,1702056; j. Power Sources 2018,386,40]. To prevent oxidation of the negative active species by oxygen in the air during charging and discharging, the cells were tested in a nitrogen-filled glove box at room temperature.
Fig. 8 is a schematic diagram of an aqueous semi-solid alkaline organic flow battery based on a 2-hydroxy-3-pyrrol anthraquinone (HpyAQ) negative electrolyte.
Fig. 9 is a graph (a) of rate performance and cycle life/efficiency of the aqueous semi-solid alkaline organic flow cell (0.1 mol/L). The negative electrode electrolyte was 7 ml of additive-free suspension of 2-hydroxy-3-pyrrol-anthraquinone (No. A1 (blank)), and the positive electrode electrolyte was 21 ml of 1mol/LKOH solution containing 0.1mol/L potassium ferrocyanide. Current density 40mA cm -2 The actual specific capacity of the negative electrode electrolyte is 4.5Ah L -1 . After 480 cycles, the discharge capacity retention rate (DCR) was 84.7%, and the capacity retention rate per cycle was 99.97%. The current efficiency was 96.6% and the energy efficiency was 69.4%.
Fig. 10 is a graph (a) of rate performance and cycle life/efficiency of an aqueous semi-solid alkaline organic flow battery (0.2 mol/L). The negative electrode electrolyte was 7 ml of additive-free 0.2 mol/L2-hydroxy-3-pyrrolidoneanthraquinone suspension (code A2 (blank)), and the positive electrode electrolyte was 21 ml of 1mol/LKOH solution containing 0.2mol/L potassium ferrocyanide. Current density 50mA cm -2 The actual specific capacity of the negative electrode electrolyte is 9.7Ah L -1 . After 1000 cycles, the discharge capacity retention rate (DCR) was 65.0%, and the capacity retention rate per cycle was 99.96%. The current efficiency is 99.2%, and the energy efficiency is 76.9%.
Comparative example 1 aqueous semi-solid alkaline organic flow cell containing additive-free 1, 8-dihydroxyanthraquinone negative electrode electrolyte
1, 8-dihydroxy anthraquinone suspension (0.1 mol/L) without additives is used as a negative electrolyte, potassium ferrocyanide solution (0.2 mol/L) is used as a positive electrolyte (supporting electrolytes of the positive and negative electrolytes are all 0.5 MKOH), and a Nafion112 membrane is used as a diaphragm, so that a single cell system of the semi-solid organic flow battery is constructed. The cell was protected with nitrogen. Current density 100mA cm -2 The actual specific capacity of the negative electrode electrolyte of the battery is only 1.86Ah L -1 . The battery system had a discharge capacity retention of 89% after 100 cycles, and a capacity retention of 99.88% per cycle.
Example 4 aqueous semi-solid alkaline organic flow cell with additive-containing 2-hydroxy-3-pyrrolequinone negative electrolyte
And (3) taking the suspension of the 2-hydroxy-3-pyrrole anthraquinone containing the additive as the negative electrolyte, and constructing a single cell of the semi-solid organic flow battery under the same conditions as in the example 3. The cells were tested in a nitrogen-filled glove box at room temperature. The results are shown in Table 2. As can be seen from the table, the addition of the additive (particularly choline) improves the specific capacity of the negative electrode electrolyte. The addition of cyclodextrin, niacinamide, and urea also helps to improve the current efficiency of the cell.
TABLE 2 comparison of Performance of aqueous semi-solid alkaline organic flow cell
| Serial number | Negative electrode electrolyte | Positive electrode electrolyte | Current efficiency (%) | Specific capacity of negative electrode solution (Ah L) -1 ) |
| 1 | A2 (blank) | 0.1mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 99.2 | 9.7 |
| 2 | A4 | 0.2mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 99.1 | 9.9 |
| 3 | A5 | 0.4mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 98.6 | 16.5 |
| 4 | A6 | 0.4mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 98.7 | 19.4 |
| 5 | A7 | 0.4mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 98.3 | 15.3 |
| 6 | A8 | 0.2mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 99.3 | 9.9 |
| 7 | A9 | 0.2mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 99.8 | 9.8 |
| 8 | A10 | 0.2mol/L K 4 [Fe(CN) 6 ]+1mol/L NaOH | 99.8 | 9.7 |
| 9 | A11 | 0.2mol/L K 4 [Fe(CN) 6 ]+1mol/L KOH | 99.1 | 9.8 |
。
Claims (9)
1. The flow battery is characterized by comprising a negative electrode electrolyte system, a diaphragm, a positive electrode electrolyte solution and a conductive electrode; wherein, the active substance in the negative electrode electrolyte system is low-solubility 2-hydroxy-3-pyrrole anthraquinone.
2. The aqueous semi-solid alkaline organic flow battery of claim 1, wherein the negative electrolyte system is comprised of 2-hydroxy-3-pyrrol-anthraquinone, additives, alkaline supporting electrolyte and water.
3. The aqueous semi-solid alkaline organic flow cell of claim 1, wherein the 2-hydroxy-3-pyrrol-anthraquinone is present in the negative electrolyte system in an amount of 0.1 to 1mol/L.
4. The water-based semi-solid alkaline organic flow battery of claim 2, wherein the additive is one or a mixture of choline, cyclodextrin, nicotinamide and urea, and the content of the additive in the negative electrode electrolyte system is 0.01-1 mol/L.
5. The aqueous semi-solid alkaline organic flow battery of claim 1, wherein the positive electrolyte solution is an aqueous solution comprising a redox active inorganic substance and an alkaline supporting electrolyte.
6. The aqueous semi-solid alkaline organic flow battery of claim 5, wherein the redox active inorganic substance is one or more of potassium ferrocyanide, sodium ferrocyanide and ammonium ferrocyanide, and the concentration of ferrocyanide in the positive electrolyte solution is 0.1-1.2 mol/L.
7. The aqueous semi-solid alkaline organic flow battery of claim 1, wherein the alkaline supporting electrolyte contained in the electrolyte solution of the negative electrode and the positive electrode is one or a mixture of potassium hydroxide, sodium hydroxide and lithium hydroxide, and the concentration of the alkaline supporting electrolyte is 0.01-2 mol/L.
8. The aqueous semi-solid alkaline organic flow cell of claim 1, wherein the separator is a cation conducting membrane.
9. The aqueous semi-solid alkaline organic flow cell of claim 1, wherein the conductive electrode is a carbon-based material.
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