CN109346729B - Water system semi-flow battery - Google Patents
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Abstract
The invention belongs to the field of electrochemistry, and particularly relates to a phenanthroline iron complex-water system semi-liquid flow battery with a carbon nanohorn/polyimide compound as a solid cathode. The battery system includes: the composite material comprises a carbon nanohorn/polyimide composite negative electrode with low negative potential, a phenanthroline iron complex positive electrode with high positive potential, a perfluorinated sulfonic acid-polytetrafluoroethylene copolymer diaphragm and an acetic acid aqueous solution electrolyte. The water system flow battery has the advantages of high working voltage, energy density, power density, safety performance and the like, and has good market application prospect when being used as an energy storage device in a new energy power generation process and in the field of power grid peak regulation.
Description
Technical Field
The invention belongs to the field of new energy, and particularly relates to a water system semi-flow battery.
Background
With the rapid development of economy, the demand of energy sources, especially the demand of electric energy, has increased dramatically in various countries. At present, not only various electrical equipment is available, but also the new energy electric automobile has severe impact on the traditional fossil fuel automobile. However, the traditional thermal power generation and water conservancy power generation have great limitations in the aspects of environmental friendliness and sustainable development, so that great attention is paid to the utilization of renewable energy sources such as solar energy, wind energy, tidal energy and the like. The renewable energy sources have the defects of obvious instability, locality and the like, so that the renewable energy sources are difficult to safely incorporate into a power grid, and therefore, the development of a high-efficiency energy storage device matched with the renewable energy sources is extremely important. At present, the electrochemical energy storage systems which are used more mainly comprise electrochemical secondary batteries, super capacitors, redox flow batteries and the like. The flow battery is an energy storage element, has the advantages of large energy storage scale, long cycle life, high safety performance and the like, but has lower energy density<50Wh kg-1)。
Flow batteries are mainly classified into aqueous flow batteries and nonaqueous flow batteries. For nonaqueous flow batteries, the ion/electron migration rate of the organic electrolyte is low, and the problem of safety is easily caused. In the aqueous flow battery, since an aqueous electrolyte is used, safety is no longer a major concern, but the charge/discharge potential is not high due to the problems of water decomposition and hydrogen evolution and oxygen evolution, and thus, the current research on the aqueous electrode material is relatively small.
Disclosure of Invention
In order to improve the energy density of a redox flow battery and simultaneously solve the technical problem that a charge-discharge potential of the aqueous flow battery is not high due to the problems of hydrogen evolution and oxygen evolution caused by water decomposition, the invention provides an aqueous semi-flow battery which has high energy density and is formed by combining a solid cathode taking a carbon nanohorn/polyimide compound as an active material and a water-soluble phenanthroline iron complex anode.
The invention provides a water system semi-flow battery, which takes a water-soluble phenanthroline iron complex with high positive potential as a positive electrode, a carbon nanohorn/polyimide complex with low negative potential as a solid negative electrode, an acetic acid aqueous solution as an electrolyte and a perfluorosulfonic acid-polytetrafluoroethylene copolymer as a diaphragm.
In the present invention, a carbon nanohorn/polyimide composite solid negative electrode includes: active material carbon nanohorn/polyimide, conductive agent graphene, adhesive polyvinylidene fluoride and current collector. The preparation method comprises the following steps: firstly, uniformly mixing an active material polyimide, a conductive agent graphene and a binder polyvinylidene fluoride according to a certain mass ratio, and then combining with a current collector in a rolling manner;
wherein, the content of the active substance carbon nanohorn/polyimide is 20-90% of the total mass of the negative electrode.
The content of the conductive agent graphene is 5-30% of the total mass of the negative electrode.
The content of the polyvinylidene fluoride binder accounts for 1-20% of the total mass of the negative electrode.
The adopted current collector has high conductivity and can be one or a compound of a plurality of carbon cloth, a conductive graphite net and a stainless steel net.
The preparation method of the active substance carbon nanohorn/polyimide comprises the following steps: acid dianhydride, amine and carbon nanohorns are used as raw materials, and carbon nanohorns/polyimides with different chemical structures are prepared in a one-step polymerization mode.
Wherein the acid dianhydride is one or more of naphthalene tetracarboxylic dianhydride, 3 ', 4, 4' -benzophenone tetracarboxylic dianhydride, cyclopentanetetracarboxylic dianhydride and biphenyl tetracarboxylic dianhydride.
The amine is one or a compound of more of urea, ethylenediamine, melamine, triethylamine, diethylenetriamine and isophorone diamine.
The specific preparation process of the carbon nanohorn/polyimide comprises the following steps: firstly, acid dianhydride and amine with equal molar ratio are added into a strong polar solvent NMP together, then 2% -20% of high-conductivity carbon nanohorns are added, and then heating reflux is carried out for 2-10 hours at 150-220 ℃. And repeatedly washing and filtering the reactants after cooling, carrying out vacuum drying, then carrying out heat treatment for 5-15 h at 200-400 ℃ under the protection of nitrogen, and cooling to obtain the carbon nanohorn/polyimide.
According to the invention, the carbon nanohorn is added into the raw material for synthesizing the polyimide, and the nanohorn/polyimide is prepared by adopting a one-step method, so that the dispersion of the carbon nanohorn in the product is facilitated, the prepared product is more uniform, and the performance is better.
Wherein, the preparation process of the carbon nanohorn comprises the following steps: the carbon nanohorn is prepared by adopting a plasma electrolysis method, namely the carbon quantum dot in ethanol or acetone solution is electrolyzed at constant potential by using the plasma electrolysis method to prepare the carbon nanohorn. Specifically, 50mg of high-purity graphite is taken and 200mL of 3mol L of high-purity graphite is added-1HNO of (2)3Reflux at 180 deg.C for 12 h. After multiple centrifugations and washings, the prepared carbon quantum dots are dispersed in ethanol or acetone solution. The platinum sheet is used as an electrode, and the high-dispersity carbon nanohorn is prepared by utilizing the high-temperature and large-amount free electron characteristics of plasma.
To increase Fe2+Adding acetic acid into the positive electrolyte to ensure that the pH value of the solution is 2-6, wherein the complexing ability of the complex with phenanthroline (phen) and the solubility of phenanthroline iron complex.
The water system semi-liquid flow battery provided by the invention has the advantages that under an acidic condition, the solubility of the positive electrode electroactive substance is high, the electron transfer speed is high, and the current density is higher, so that the positive electrode electroactive substance and the negative electrode electroactive substance have better electrochemical reversibility under the acidic condition, the assembled water system semi-liquid flow battery has high potential and specific energy, and the water system semi-liquid flow battery has wide application prospects in the fields of new energy grid connection, power grid peak regulation and the like.
The invention has the beneficial effects that:
the liquid flow battery utilizes the characteristics of good electrochemical reversibility and high potential of an electroactive water-soluble phenanthroline iron complex anode and good electric pair low potential of the carbon nanohorn/polyimide complex solid cathode, combines the water-soluble phenanthroline iron complex anode and the polyimide solid cathode to greatly improve the performance of an electrochemical energy storage battery system, and simultaneously, the anode of the water-based semi-liquid flow battery is the redox reaction between phenanthroline ferric iron and phenanthroline ferrous iron, the cathode is the redox reaction between polyimide and polyimide anions, and the carbon nanohorn plays a role of a conductive agent and can accelerate the transmission speed of electrons in the polyimide. The anode and cathode materials selected by the invention have appropriate electrode potentials, so that not only can a high potential be obtained, but also the problems of hydrogen evolution and oxygen evolution caused by water decomposition can be avoided.
The water system semi-liquid flow battery designed by the invention has the advantages of simple manufacturing process, safety, environmental protection, low price and high specific capacity, and is widely applied to the fields of large-scale electricity storage of new energy power generation and peak shaving of a power grid.
Drawings
FIG. 1 is a cyclic voltammogram of the phenanthroline iron complex of example 1 at different sweeping rates.
FIG. 2 is a cyclic voltammogram of the phenanthroline iron complex of example 1 at various pH values.
Fig. 3 is a cyclic voltammogram of the carbon nanohorn/polyimide composite negative electrode of example 2.
Fig. 4 is a capacity plot for the assembled water-based energy storage cell of example 3 at different current densities.
Fig. 5 is a capacity map of the assembled water-based hybrid energy storage cell in the comparative example at different current densities.
Detailed Description
Example 1
Preparation of water-soluble phenanthroline iron complex positive electrode and electrochemical performance test
0.3mol L of the mixture is prepared respectively-1And 0.1mol L of phenanthroline solution-1The pH value of the ferrous sulfate solution is adjusted to be 6 by sodium acetate-acetic acid. Slowly dripping the phenanthroline solution into the ferrous sulfate solution under the condition of continuously stirring, and continuously reacting for 2 hours to ensure that ferrous ions can be completely complexed with the phenanthroline to obtain the phenanthroline iron complex.
Pouring the phenanthroline ferrous solution into a 20mL electrolytic cell, introducing nitrogen for 10 minutes, taking a glassy carbon electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum sheet electrode as a counter electrode, and testing the electrochemical performance of phenanthroline ferrous in a three-electrode system.
FIG. 1 is a cyclic voltammogram of phenanthroline iron complex at different sweeping speeds. As the sweep rate increases, the redox current increases continuously, while the oxidation and reduction potentials remain substantially unchanged, exhibiting good electrochemical reversibility. Meanwhile, the difference value between the oxidation potential and the reduction potential is about 58mV, which further shows that the positive electrode of the phenanthroline iron complex has good electrochemical performance.
FIG. 2 is a cyclic voltammogram of phenanthroline iron complexes at different pH values. As can be seen from the figure, the phenanthroline iron complex has a good electrochemical peak in the electrolyte with the pH value of 2-6.
Example 2
Preparation and electrochemical performance test of carbon nanohorn/polyimide composite cathode
0.1mol of naphthalenetetracarboxylic dianhydride, 0.1mol of ethylenediamine and 0.005mol of carbon nanohorn were collectively added to 50mL of NMP as a solvent, and heated under reflux at 220 ℃ for 10 hours. And then repeatedly washing and filtering the reactants after cooling, carrying out vacuum drying, then carrying out heat treatment for 15h at 400 ℃ under the protection of nitrogen, and cooling to obtain the carbon nanohorn/polyimide.
The carbon nanohorn/polyimide composite negative electrode includes: active material carbon nanohorn/polyimide, conductive agent graphene, adhesive polyvinylidene fluoride and current collector. Firstly, uniformly mixing an active substance carbon nanohorn/polyimide, a conductive agent graphene and a binder polyvinylidene fluoride according to a certain mass ratio, and then combining with a current collector in a rolling manner; wherein the content of the active substance carbon nanohorn/polyimide compound is 90 percent of the total mass of the negative electrode, and the use amounts of the conductive agent graphene and the adhesive polyvinylidene fluoride are both 5 percent.
Fig. 3 is a cyclic voltammogram of a carbon nanohorn/polyimide composite negative electrode. The prepared carbon nanohorn/polyimide composite negative electrode has a pair of good oxidation-reduction peaks, and the reduction peaks are positioned at about-0.7V.
Example 3
Assembly of aqueous energy storage cells
And constructing a cathode based on the carbon nanohorn/polyimide compound and a water system energy storage battery based on the anode of the water-soluble phenanthroline iron complex electric pair. The water-soluble phenanthroline iron complex used in example 1 is used as a flow positive electrode, the carbon nanohorn/polyimide composite used in example 2 is used as a solid positive electrode, the pretreated perfluorosulfonic acid-polytetrafluoroethylene copolymer membrane is used as an ion exchange membrane of a flow battery, and an acetic acid aqueous solution with the pH of 6 is used as a battery electrolyte. And (3) carrying out charge and discharge tests on the assembled water system half flow battery by using a LAND battery test system.
In order to prevent the reduction products of the positive and negative electrodes from being oxidized by oxygen in the air during charging and discharging, the whole battery test period is carried out under the protection of nitrogen so as to isolate the air. In order to study the electrochemical performance of the assembled water system half-flow battery, we tested the battery at different current densities (50-400 mA/cm)2) Then, charging and discharging are carried out in a constant current mode, the voltage range of charging and discharging is 0V-1.7V, and the flow rate of the electrolyte is 100 mL/min.
Fig. 4 is a capacity plot of assembled water-based energy storage cells at different current densities. The voltage of the assembled flow battery was 1.7V and the energy density was 320.8Wh/L, calculated from the discharge time.
Example 4
Preparation of carbon nanohorn/polyimide composite negative electrode
0.1mol of 3,3 ', 4, 4' benzophenone tetracarboxylic dianhydride, 0.1mol of triethylamine and 0.01mol of carbon nanohorn are added into 50mL of NMP solvent together, and heated and refluxed for 8h at 200 ℃. And then repeatedly washing and filtering the reactants after cooling, carrying out vacuum drying, then carrying out heat treatment for 15h at 300 ℃ under the protection of nitrogen, and cooling to obtain the carbon nanohorn/polyimide.
The carbon nanohorn/polyimide composite negative electrode includes: active material carbon nanohorn/polyimide, conductive agent graphene, adhesive polyvinylidene fluoride and current collector. Firstly, uniformly mixing an active substance carbon nanohorn/polyimide, a conductive agent graphene and a binder polyvinylidene fluoride according to a certain mass ratio, and then combining with a current collector in a rolling manner; wherein the content of the active substance carbon nanohorn/polyimide compound is 80 percent of the total mass of the negative electrode, and the use amounts of the conductive agent graphene and the adhesive polyvinylidene fluoride are both 10 percent.
Example 5
Assembly of aqueous energy storage cells
And constructing a cathode based on the carbon nanohorn/polyimide compound and a water system energy storage battery based on the anode of the water-soluble phenanthroline iron complex electric pair.
The assembled aqueous semi-flow cell was subjected to charge and discharge tests using the water-soluble phenanthroline iron complex used in example 1 as a flow positive electrode, the carbon nanohorn/polyimide composite used in example 4 as a solid positive electrode, the pretreated perfluorosulfonic acid-polytetrafluoroethylene copolymer membrane as an ion exchange membrane of the flow cell, and an aqueous acetic acid solution having a pH of 6 as a cell electrolyte, using a LAND cell test system. The test method was the same as in example 3, and the assembled flow battery had a voltage of 1.7V and an energy density of 267.5 Wh/L.
Example 6
Preparation of carbon nanohorn/polyimide composite negative electrode
0.1mol of biphenyl tetracarboxylic dianhydride, 0.1mol of diethylenetriamine and 0.015mol of carbon nanohorn are added into 50mL of solvent NMP together, and heated and refluxed for 10h at 180 ℃. And then repeatedly washing and filtering the reactants after cooling, carrying out vacuum drying, then carrying out heat treatment for 15h at 300 ℃ under the protection of nitrogen, and cooling to obtain the carbon nanohorn/polyimide.
The carbon nanohorn/polyimide composite negative electrode includes: active material carbon nanohorn/polyimide, conductive agent graphene, adhesive polyvinylidene fluoride and current collector. Firstly, uniformly mixing an active substance carbon nanohorn/polyimide, a conductive agent graphene and a binder polyvinylidene fluoride according to a certain mass ratio, and then combining with a current collector in a rolling manner; the content of the active substance carbon nanohorn/polyimide compound is 50% of the total mass of the negative electrode, the using amount of the conductive agent graphene is 30%, and the using amount of the binder polyvinylidene fluoride is 20%.
Example 7
Assembly of aqueous energy storage cells
And constructing a cathode based on the carbon nanohorn/polyimide compound and a water system energy storage battery based on the anode of the water-soluble phenanthroline iron complex electric pair.
The assembled aqueous semi-flow cell was subjected to charge and discharge tests using the water-soluble phenanthroline iron complex used in example 1 as a flow positive electrode, the carbon nanohorn/polyimide composite used in example 6 as a solid positive electrode, the pretreated perfluorosulfonic acid-polytetrafluoroethylene copolymer membrane as an ion exchange membrane of the flow cell, and an aqueous acetic acid solution having a pH of 6 as a cell electrolyte, using a LAND cell test system. The test method was the same as in example 3, and the assembled flow battery had a voltage of 1.7V and an energy density of 310.4 Wh/L.
Comparative example
Construction of Metal Complex Mn based on Trans-1, 2-cyclohexanediaminetetraacetic acid (CyDTA) complexation(III)CyAnd the water system hybrid energy storage battery comprises a DTA positive electrode and a poly (1, 4-anthraquinone) negative electrode.
Poly (1, 4-anthraquinone) P (1,4-AQ) is taken as a negative electrode, and a water-soluble metal complex Mn(III)CyDTA is a flow positive electrode, a pretreated Nafion membrane is used as an ion exchange membrane of the flow battery, and 1M NaNO is added3As a negative electrolyte, the assembled water system half flow battery is charged by using a LAND battery test systemAnd (5) discharging and testing. Fig. 5 is a capacity diagram of the assembled water-based hybrid energy storage cell in the comparative example at different currents. The assembled flow battery had a voltage of 1.7V and an energy density of 108.8 Wh/L.
Claims (6)
1. An aqueous half-flow battery characterized in that: the water system semi-flow battery takes a water-soluble phenanthroline iron complex with high positive potential as a positive electrode, a carbon nanohorn/polyimide complex with low negative potential as a solid negative electrode, an acetic acid aqueous solution as an electrolyte and a perfluorosulfonic acid-polytetrafluoroethylene copolymer as a diaphragm;
the carbon nanohorn/polyimide composite solid negative electrode includes: carbon nanohorns/polyimide, graphene, polyvinylidene fluoride and a current collector;
the preparation method of the carbon nanohorn/polyimide comprises the following steps: acid dianhydride, amine and carbon nanohorns are used as raw materials, and carbon nanohorns/polyimide is prepared in a one-step polymerization mode;
the carbon nanohorn is prepared by adopting a plasma electrolysis method, and specifically, 50mg of high-purity graphite is firstly added into 200mL of 3mol L-1HNO of (2)3Refluxing for 12h at 180 ℃, centrifuging and washing for many times, dispersing the prepared carbon quantum dots in an ethanol or acetone solution, electrolyzing the carbon quantum dots in the ethanol or acetone solution by using a plasma electrolysis method at constant potential by taking a platinum sheet as an electrode, and preparing the high-dispersity carbon nanohorn by using the high-temperature and large-amount free electron characteristics of the plasma;
and adding acetic acid into the positive electrolyte to ensure that the pH value of the solution is 2-6.
2. The aqueous semi-flow battery of claim 1, wherein: the preparation method of the carbon nanohorn/polyimide composite solid negative electrode comprises the following steps: uniformly mixing the carbon nanohorn/polyimide, the graphene and the polyvinylidene fluoride according to the mass ratio, and then combining the mixture with a current collector in a rolling manner; wherein the content of the carbon nanohorn/polyimide is 90% of the total mass of the negative electrode, the content of the graphene is 5% of the total mass of the negative electrode, and the content of the polyvinylidene fluoride is 5% of the total mass of the negative electrode; the current collector is one or a compound of a plurality of carbon cloth, conductive graphite net or stainless steel net.
3. The aqueous semi-flow battery of claim 1, wherein: the preparation method of the carbon nanohorn/polyimide comprises the following steps: firstly, acid dianhydride and amine with equal molar ratio are added into a solvent NMP together, then 2% -20% of carbon nanohorns are added, and then heating reflux is carried out for 2-10 h at 150-220 ℃; and repeatedly washing and filtering the reactants after cooling, carrying out vacuum drying, then carrying out heat treatment for 5-15 h at 200-400 ℃ under the protection of nitrogen, and cooling to obtain the carbon nanohorn/polyimide.
4. The aqueous semi-flow battery of claim 3, wherein: the acid dianhydride is one or more of naphthalene tetracarboxylic dianhydride, 3,4, 4' -benzophenone tetracarboxylic dianhydride, cyclopentanetetracarboxylic dianhydride, biphenyl tetracarboxylic dianhydride and maleic anhydride.
5. The aqueous half-flow battery according to claim 4, characterized in that: the amine is one or a compound of more of urea, ethylenediamine, melamine, triethylamine, diethylenetriamine and isophorone diamine.
6. Use of an aqueous semi-flow battery according to claim 1, characterized in that: the water system semi-flow battery is used in the fields of new energy grid connection and power grid peak regulation.
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| CN113737213A (en) * | 2021-09-01 | 2021-12-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of flexible polyimide carbon cloth composite electrode material, product and application thereof |
| CN113980311B (en) * | 2021-11-26 | 2022-06-21 | 江苏清大际光新材料有限公司 | Heat dissipation film containing carbon nanohorns, preparation method and application |
| CN117586316B (en) * | 2023-10-24 | 2024-08-06 | 哈尔滨工业大学 | Iron complex, preparation method thereof and application thereof in solid energy storage material of flow battery |
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| CN102119458B (en) * | 2008-05-22 | 2014-10-22 | 株式会社Pi技术研究所 | Conductive agent for battery electrode, electrode containing the same, and battery |
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