A preparation method for hexagonal h-WO3 vertically interlaced micron disks for water treatment
By preparing the hexagonal phase h-WO3 vertically interspersed micron disk, the problems of low reserves of existing materials and insufficient catalytic activity are solved, and high-efficiency electrocatalytic water oxidation is achieved to generate high current density oxygen.
Patent Information
- Application Number
- CN202310966255.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-02
- Publication Date
- 2025-09-02
- Estimated Expiration
- 2043-08-02
AI Technical Summary
Due to the low reserves and high prices of existing IrO2 and RuO2-based materials, the electrocatalytic water oxidation efficiency is limited. The existing h-WO3 materials lack catalytic activity in electrolytic water, making it difficult to meet the demand for efficient electrocatalytic water oxidation.
By dispersing H2WO4 into a mixed solution of hydrogen peroxide and NaNO3 and heated to prepare a hexagonal phase h-WO3 vertically interspersed micron disk, it is applied to electrocatalytic water oxidation reaction to form an IrO2/WO3 complex to improve catalytic activity.
The production of oxygen at a high current density at a lower overpotential is achieved, showing high catalytic capacity, the current density reaches 10mA/cm2 and the overpotential is 250-400mV.
Smart Images
Figure HDA0004373729990000011
Abstract
Description
Technical Field
[0001] The invention relates to a method for preparing hexagonal phase h-WO3 vertically interlaced micron disks for water treatment, belonging to the field of material preparation and application. Background Art
[0002] Due to the energy crisis caused by the extensive use of fossil fuels, the development of green energy has become a hot topic in the world. Hydrogen energy has become a focus of attention due to its advantages such as high energy density and pollution-free combustion. There are many ways to produce hydrogen, among which electrocatalytic decomposition of water to produce hydrogen and oxygen is an effective path. Electrocatalytic water oxidation is a half-reaction of water electrolysis, and its slow kinetics seriously restricts the efficiency of water electrolysis. IrO2 and RuO2-based materials can effectively catalyze water oxidation, but the disadvantages of these materials are low reserves and high prices. Therefore, there is an urgent need to develop highly active and stable non-precious metal materials to improve the efficiency of electrocatalytic water oxidation.
[0003] The wide bandwidth makes WO3 have high catalytic activity. At present, WO3 mainly includes the thermodynamically stable phase m-WO3 and the thermodynamically metastable phase h-WO3. Among them, h-WO3 contains a large channel, and the structure is constructed by [WO6] octahedron. Electrocatalytic water splitting mainly focuses on m-WO3 catalysts, while h-WO3 electrolysis of water is rarely involved. Yang's team will (NH4) 10 [H2W 12 O 42 ]·xH2O was calcined at 350℃ for 120min to obtain WO3 material, which was then dispersed into H2IrCl6·6H2O solution and calcined at 400℃ for 240min to obtain IrO2 / WO3 composite. WO3 had almost no activity in the electrocatalytic water oxidation reaction, and the current density of the IrO2 / WO3 material was 13.9mA / cm at 450mV. 2 (Int J Hydrogen Energy 2019;44:31082-93). Dai's team constructed a WO3@F-GS material using CF3(CF2)6COOH, W, and graphite sheets. The addition of F enhanced the catalytic water oxidation performance, with a current density of 10 mA / cm at 298 mV. 2 (Chem Eng J 2023; 451: 138590). Liang's team found that h-WO3 had almost no water oxidation activity. After combining it with rGO, they obtained WO3 / rGO, which had a current density of 5 mA / cm at 570 mV. 2 (EnergyEnviron Mater 2021;4:681-6).
[0004] Recent studies have shown that modifying the morphology, size, and composition of materials can increase the number of active sites on the catalyst, thereby enhancing its electrocatalytic activity. Therefore, it is of great significance to modify the WO3 crystal structure and morphology to achieve efficient catalytic water oxidation. Summary of the Invention
[0005] The present invention aims to provide a method for preparing hexagonal h-WO3 vertically interlaced micron disks for water treatment.
[0006] Based on the above objectives, the technical solutions involved in the present invention are as follows:
[0007] (1) Preparation of hexagonal h-WO3 vertically interspersed microdisks: 0.3g-0.4mg of H2WO4 was dispersed in 10-15mL of commercial hydrogen peroxide (30% by mass), and 0.3-0.9g of NaNO3 was added. After mixing, the mixture was heated at 110-130°C for 6-24h to obtain hexagonal h-WO3 vertically interspersed microdisks. The hexagonal h-WO3 prepared in the above method is classified as JCPDS#33-1387, and the diameter of the hexagonal h-WO3 vertically interspersed microdisks is 1.8-4μm.
[0008] (2) Application of the hexagonal h-WO3 vertically interlaced micron disks prepared by the above-mentioned preparation method in water treatment reaction; electrocatalytic water oxidation produces oxygen at a KOH concentration of 1 mol / L, and the reaction current density is 10 mA / cm 2 , the overpotential is 250-400mV.
[0009] The present invention has the following advantages:
[0010] 1) A new synthesis route for vertically interlaced hexagonal h-WO3 microdisks is provided.
[0011] 2) Hexagonal h-WO3 vertically interspersed microdisks exhibit high catalytic ability in electrocatalytic water oxidation to produce oxygen. BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Figure 1 These are the XRD and SEM characterization results of hexagonal h-WO3 vertically interspersed micro-disks. DETAILED DESCRIPTION
[0013] The following examples are intended to further illustrate the present invention but are not intended to limit the present invention.
[0014] Example 1
[0015] Preparation of hexagonal h-WO3 vertically interspersed micron disks: 0.3g H2WO4 was dispersed in 10mL of commercial hydrogen peroxide (mass fraction of 30%), and then 0.3g NaNO3 was added. After mixing, the mixture was heated at 110°C for 6h to obtain hexagonal h-WO3 vertically interspersed micron disks. In the above preparation method, the hexagonal h-WO3 belongs to the standard card JCPDS#33-1387, and the diameter of the hexagonal h-WO3 vertically interspersed micron disks is 1.8-3μm. The prepared hexagonal h-WO3 vertically interspersed micron disks were used for water treatment; when the KOH concentration was 1mol / L, the electrocatalytic water oxidation produced oxygen, and the reaction current density was 10mA / cm 2 , the overpotential is 400mV.
[0016] Example 2
[0017] Preparation of hexagonal h-WO3 vertically interlaced micron disks: 0.4mg H2WO4 was dispersed in 15mL commercial hydrogen peroxide (mass fraction of 30%), and then 0.9g NaNO3 was added. After mixing, the mixture was heated at 130°C for 24h to obtain hexagonal h-WO3 vertically interlaced micron disks. In the above preparation method, the hexagonal h-WO3 belongs to the standard card JCPDS#33-1387, and the diameter of the hexagonal h-WO3 vertically interlaced micron disks is 2-4μm. The prepared hexagonal h-WO3 vertically interlaced micron disks were used for water treatment; when the KOH concentration was 1mol / L, the electrocatalytic water oxidation produced oxygen, and the reaction current density was 10mA / cm 2 , the overpotential is 300mV.
[0018] Example 3
[0019] Preparation of hexagonal h-WO3 vertically interlaced micron disks: 0.35g mg of H2WO4 was dispersed in 12mL of commercial hydrogen peroxide (mass fraction of 30%), and then 0.6g of NaNO3 was added. After mixing, the mixture was heated at 120°C for 10h to obtain hexagonal h-WO3 vertically interlaced micron disks. In the above preparation method, the hexagonal h-WO3 belongs to the standard card JCPDS#33-1387, and the diameter of the hexagonal h-WO3 vertically interlaced micron disks is 1.8-3.4μm. The prepared hexagonal h-WO3 vertically interlaced micron disks were used for water treatment; when the KOH concentration was 1mol / L, the electrocatalytic water oxidation produced oxygen, and the reaction current density was 10mA / cm 2 , the overpotential is 250mV.
Claims
1. A method for preparing hexagonal h-WO3 vertically interlaced micro-disks, characterized in that: The following steps are involved: 0.3g-0.4mg H2WO4 is dispersed in 10-15mL of commercial hydrogen peroxide with a mass fraction of 30%, and then 0.3-0.9NaNO3 is added. After mixing, it is heated at 110-130°C for 6-24h to obtain hexagonal h-WO3 vertically interspersed micron disks; the hexagonal h-WO3 is classified according to the standard card JCPDS#33-1387, and the diameter of the hexagonal h-WO3 vertically interspersed micron disks is 1.8-4μm.
2. An application of a hexagonal h-WO3 vertically interlaced micron disk prepared by the preparation method of claim 1 in a water treatment reaction; electrocatalytic water oxidation produces oxygen at a KOH concentration of 1 mol / L, with a reaction current density of 10 mA / cm 2 , the overpotential is 250-400mV.