CN114318397A - Molybdenum-based electrocatalyst, preparation method thereof, bifunctional electrolytic cell and application thereof - Google Patents
Molybdenum-based electrocatalyst, preparation method thereof, bifunctional electrolytic cell and application thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum-based electrocatalyst and a preparation method thereof, a bifunctional electrolytic cell and application thereof, wherein the preparation method of the molybdenum-based electrocatalyst comprises the following steps: adding ammonium molybdate and polyethylene glycol into water, stirring uniformly, then continuously adding concentrated nitric acid, and stirring to obtain a mixed solution; putting the mixed solution into a reaction kettle for hydrothermal reaction, cooling after the reaction is finished, centrifuging, washing and drying the product to obtain the molybdenum-based electrocatalystα‑MoO3. The raw materials adopted by the preparation of the molybdenum-based electrocatalyst are easy to obtain, the cost is low, the preparation process is simple to operate, the prepared molybdenum-based electrocatalyst is used as a working electrode in the double-function electrolytic cell, the mixed solution of potassium hydroxide and urea is used as an electrolyte, the double-function electrolytic cell is applied to hydrogen production and urea wastewater degradation, the hydrogen production efficiency is improved, and urea pollutants are oxidized and degraded, so that the double-function electrolytic cell is green and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of hydrogen production, and particularly relates to a molybdenum-based electrocatalyst, a preparation method thereof, a bifunctional electrolytic cell and application thereof.
Background
In recent years, the global energy crisis and environmental pollution seriously jeopardize human survival. Therefore, the development of clean and renewable energy sources is very necessary. Hydrogen is widely noticed as a clean energy source, and among many hydrogen production modes, electrocatalytic decomposition of water is considered as a widely-used hydrogen production method, but the method is also limited by a water oxidation four-electron half reaction, has slow reaction kinetics and high overpotential, and requires application of high voltage, so that the method is challenging. Studies have shown that this limitation can be overcome by replacing the slow water oxidation half-reaction with a more oxidizable molecule.
The patent of the prior utility model: urea electrolysis a system for wastewater treatment and hydrogen supply from coal liquefaction (publication No. CN 208183082U) discloses obtaining high-purity hydrogen gas by urea electrolysis, but the process and apparatus used are complicated and costly. Patent application of the prior invention: an anode catalyst for electrolysis of water and urea and a method for preparing the same (publication No. CN 110237860A) disclose that the performance of electrolysis of water and urea is studied by using the catalyst, but the preparation of the catalyst requires the use of a raw material having a polluting property and does not investigate whether the cell voltage of an electrolytic cell is changed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a molybdenum-based electrocatalyst, a preparation method thereof, a bifunctional electrolytic cell and application thereof.
The invention provides the following technical scheme:
in a first aspect, there is provided a method for preparing a molybdenum-based electrocatalyst, comprising the steps of:
adding ammonium molybdate and polyethylene glycol into water, stirring uniformly, then continuously adding concentrated nitric acid, and stirring to obtain a mixed solution;
putting the mixed solution into a reaction kettle for hydrothermal reaction, cooling after the reaction is finished, centrifuging, washing and drying the product to obtain the molybdenum-based electrocatalystα-MoO3。
Further, the mass ratio of the ammonium molybdate to the polyethylene glycol is 2.9-3.1: 1.
further, the mass fraction of the concentrated nitric acid is 65-68%.
Further, adding ammonium molybdate and polyethylene glycol into water, stirring for 20-40 min, adding concentrated nitric acid, and stirring for 20-40 min.
Furthermore, the temperature of the hydrothermal reaction is 150-170 ℃, and the reaction time is 22-26 h.
In a second aspect, a molybdenum-based electrocatalyst prepared by the method for preparing the molybdenum-based electrocatalyst according to the first aspect is provided.
In a third aspect, a bifunctional electrolytic cell is provided, using the molybdenum-based electrocatalyst according to the second aspect as a working electrode.
In a fourth aspect, an application of the bifunctional electrolytic cell of the third aspect is provided, wherein the application is applied to hydrogen production and urea wastewater degradation.
Further, a mixed solution of potassium hydroxide and urea is added into the double-function electrolytic cell to serve as an electrolyte, and a platinum wire serves as another working electrode.
Further, a voltage of 1.3-1.6V is applied in the process of hydrogen production and urea wastewater degradation.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the molybdenum-based electrocatalyst provided by the invention has the advantages of easily available raw materials, low cost, environmental protection and simple preparation process operation;
(2) according to the double-function electrolytic cell provided by the invention, the prepared molybdenum-based electrocatalyst is used as a working electrode, the mixed solution of potassium hydroxide and urea is used as an electrolyte, compared with the traditional electrolytic water system, the voltage of the electrolytic cell is effectively reduced, the electrolysis efficiency is high, the hydrogen production efficiency is improved, and meanwhile, urea pollutants are oxidized and degraded, so that the double-function electrolytic cell is suitable for hydrogen production and urea wastewater degradation.
Drawings
FIG. 1 is a molybdenum-based electrocatalyst prepared in example 1α-MoO3XRD pattern of (a);
FIG. 2 is the molybdenum-based electrocatalyst prepared in example 1α-MoO3SEM picture of (1);
FIG. 3 is a drawing obtained in example 4α-MoO3Anodic oxidation reaction performance graphs in 1M KOH and 1M KOH + 0.5M urea electrolytic systems respectively;
FIG. 4 shows the results obtained in example 4α-MoO3Performance diagram of cathodic reduction reaction in 1M KOH and 1M KOH + 0.5M urea electrolysis systems, respectively.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
Adding 1.23g of ammonium molybdate and 0.4g of polyethylene glycol into a beaker containing 30mL of water at room temperature, and stirring for 30 min; then adding 5ml of nitric acid with the concentration of 65-68%, stirring for 30min, transferring into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 24h at the constant temperature of 160 ℃; after the reaction is completed, naturally cooling to room temperature, washing with ethanol and water, centrifuging and drying to obtain the molybdenum-based electrocatalystα-MoO3。
FIG. 1 is a photograph of a film prepared in this exampleα-MoO3X-ray diffraction (XRD) pattern of (A) and (B) As can be seen from the figure, the product prepared by the present example andα-MoO3standard card (JCPDS: 89-7112) was identical, indicating that the product prepared was phase pureα-MoO3An electrocatalyst.
FIG. 2 is a photograph of a film prepared in this exampleα-MoO3Scanning Electron Microscope (SEM) image of (A) prepared in this exampleα-MoO3The shape is a nanowire, the diameter is 200-300nm, and the length is 5-10 μm.
Example 2
Adding 1.2g of ammonium molybdate and 0.4g of polyethylene glycol into a beaker containing 30mL of water at room temperature, and stirring for 30 min; then adding 5ml of nitric acid with the concentration of 65-68%, stirring for 30min, transferring into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 24h at the constant temperature of 160 ℃; after the reaction is completed, naturally cooling to room temperature, washing with ethanol and water, centrifuging and drying to obtain the molybdenum-based electrocatalystα-MoO3The XRD pattern and SEM pattern were the same as in example 1.
Example 3
Adding 1.20g of ammonium molybdate and 0.387g of polyethylene glycol into a beaker filled with 28mL of water at room temperature, and stirring for 20 min; then adding 4.9ml of nitric acid with the concentration of 65-68%, stirring for 20min, transferring into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction for 22 hours at the constant temperature of 170 ℃; after the reaction is completed, naturally cooling to room temperature, washing with ethanol and water, centrifuging and drying to obtain the molybdenum-based electrocatalystα-MoO3The XRD pattern and SEM pattern were the same as in example 1.
Example 4
Prepared in example 1α-MoO3Mixing with acetylene black and polyvinylidene fluoride in a mass ratio of 8:1:1, dispersing in 1-methyl-2-pyrrolidone, and stirring to form uniform slurry; the slurry was coated on a nickel foam and then dried at room temperature for 24 hours with a coating area of 1cm × 1cm to obtainα-MoO3And an electrode.
Will be preparedα-MoO3The electrode is used as a working electrode, a platinum wire counter electrode and Ag/AgCl as a reference electrode to form the dual-functional electrolytic cell. In the three-electrode system, certain voltage is applied, and electrocatalytic performance test is respectively carried out in 1M KOH and 1M KOH (potassium hydroxide) + 0.5M urea.
As can be seen from fig. 3 and 4, the addition of urea greatly reduced the overpotential of the electrolyzed water.
As shown in FIG. 3, for anodic oxidation, in KOH electrolysis system, water oxidation requires a high pressure of 1.611V to reach 40mA/cm2While the KOH + urea electrolytic system can reach 40mA/cm only by 1.365V2。
As shown in FIG. 4, for the cathodic reduction reaction, the hydrogen evolution reaction of the electrolytic KOH system and the KOH + urea system required voltages of-0.319V and-0.246V to reach 40mA/cm, respectively2To reach 40mA/cm2The cell voltage of the KOH electrolytic system is 1.93V, while the cell voltage of the KOH + urea electrolytic system is only 1.611V, and the cell voltage is reduced by 16.53 percent, because the slow four-electron water oxidation half reaction is replaced by the urea oxidation reaction, the energy consumption of the electrolytic water is reduced, and the hydrogen production is promoted. Therefore, the design of the double-function electrolytic cell is energy-saving, and urea pollutants are degraded while the hydrogen is produced by low-pressure high-efficiency electrolysis of water.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a molybdenum-based electrocatalyst is characterized by comprising the following steps:
adding ammonium molybdate and polyethylene glycol into water, stirring uniformly, then continuously adding concentrated nitric acid, and stirring to obtain a mixed solution;
putting the mixed solution into a reaction kettle for hydrothermal reaction, cooling after the reaction is finished, centrifuging, washing and drying the product to obtain the molybdenum-based electrocatalystα-MoO3。
2. The method for preparing a molybdenum-based electrocatalyst according to claim 1, wherein the mass ratio of ammonium molybdate to polyethylene glycol is 2.9-3.1: 1.
3. the method for preparing a molybdenum-based electrocatalyst according to claim 1, wherein the mass fraction of the concentrated nitric acid is 65-68%.
4. The method for preparing a molybdenum-based electrocatalyst according to claim 1, wherein ammonium molybdate and polyethylene glycol are added to water and stirred for 20 to 40min, and concentrated nitric acid is added and stirred for 20 to 40 min.
5. The method for preparing a molybdenum-based electrocatalyst according to claim 1, wherein the hydrothermal reaction temperature is 150 to 170 ℃ and the reaction time is 22 to 26 hours.
6. A molybdenum-based electrocatalyst, characterized in that it is prepared by the method of any one of claims 1 to 5.
7. A bifunctional electrolytic cell characterized by using the molybdenum-based electrocatalyst according to claim 6 as a working electrode.
8. Use of the bifunctional electrolytic cell of claim 7 for hydrogen production and urea wastewater degradation.
9. Use of a bi-functional electrolytic cell according to claim 8, characterized in that a mixed solution of potassium hydroxide and urea is added to the bi-functional electrolytic cell as an electrolyte, with a platinum wire as a counter electrode.
10. The application of the bifunctional electrolytic cell according to claim 9, characterized in that a voltage of 1.3-1.6V is applied in the process of hydrogen production and urea wastewater degradation.
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| CN114941155A (en) * | 2022-05-07 | 2022-08-26 | 南京信息工程大学 | Preparation process of difunctional electrolytic cell |
| CN114959771A (en) * | 2022-04-19 | 2022-08-30 | 南京信息工程大学 | Nickel-based electrocatalyst and electrolytic cell for degrading formaldehyde wastewater by hydrogen production |
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