CN109201038B - V-shaped groove2O3/VO2Composite electrocatalyst and method of making - Google Patents
V-shaped groove2O3/VO2Composite electrocatalyst and method of making Download PDFInfo
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- CN109201038B CN109201038B CN201811272287.8A CN201811272287A CN109201038B CN 109201038 B CN109201038 B CN 109201038B CN 201811272287 A CN201811272287 A CN 201811272287A CN 109201038 B CN109201038 B CN 109201038B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/22—Vanadium
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- 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
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Abstract
The invention provides a V2O3/VO2A composite electrocatalyst prepared by the method comprising: reacting NH4VO3With an aqueous solution of N-acetyl-L-cysteine (NAC), according to NH4VO3: mixing and uniformly dispersing NAC (1-4) to (3-7), and performing hydrothermal reaction at 170-220 ℃ to obtain V2O3/VO2A composite electrocatalyst. The method adopts one-step hydrothermal reaction to directly synthesize the final product, has low synthesis temperature, simple and easy operation process, cheap and easily-obtained raw materials, low cost, high yield, no need of post-treatment, environmental friendliness and suitability for large-scale production; the product has uniform chemical composition, high purity and uniform appearance, and can be applied to the water splitting hydrogen production electrocatalyst in the field of electrocatalysis.
Description
Technical Field
The invention belongs to the technical field of electrocatalysts for hydrogen production by water cracking, and particularly relates to a V2O3/VO2A composite electrocatalyst and a method for preparing the same.
Background
Vanadium is a typical multi-valence element, and various forms of oxides exist. The vanadium-oxygen system has multiple oxidation states and coordination polyhedral properties, so that the vanadium-oxygen system can be embedded into organic groups or metal ions and has the characteristic of thermotropic phase transition. Common oxides of vanadium, e.g. V2O5，VO2，V2O3Due to special properties and potential application force, the ceramic material has an important position in the fields of industry, ceramics, energy sources and the like.
The powder material is VO2And V2O3The main material of the material can be used for preparing ceramic materials, film materials, polymer composite materials and catalyst materials.
At present, VO is concerned2And V2O3The reports of electrocatalysts are very limited, and the patent directly synthesizes a V by a simple one-step hydrothermal method2O3/VO2A composite electrocatalyst.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned disadvantages of the prior art, and an object of the present invention is to provide a V2O3/VO2The preparation method of the composite electrocatalyst is simple to operate, the reaction conditions are mild, and the prepared V2O3/VO2The appearance is uniform. In order to achieve the above object, the present invention adopts the following technical solutions.
(1) Weighing NH4VO3And N-acetyl-L-cysteine (NAC) with the molar ratio of (1-4) to (3-7), respectively dissolving the NAC in 10-20 ml of deionized water, wherein the concentration of a vanadium source is (0.02-0.04) mol/L and the concentration of the NAC is (0.06-0.7) mol/L, and magnetically stirring at room temperature for 10-30 min to obtain a clear solution;
(2) mixing the two clear solutions in the step (1), and magnetically stirring at room temperature for 40-60 min to obtain a clear mixed solution;
(3) pouring the clear mixed solution in the step (2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 170-220 ℃, and the reaction time is 18-28 h;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 5-10 h at the temperature of 40-70 ℃ to obtain V2O3/VO2And (3) powder.
The invention has the beneficial effects that:
(1) the method adopts one-step hydrothermal reaction to directly synthesize the final product, so that the method has the advantages of low synthesis temperature, simple process, easy operation, cheap and easily-obtained raw materials, low cost, high yield, no need of post-treatment, environmental friendliness and suitability for large-scale production;
(2) the product prepared by the method has uniform chemical composition, high purity and uniform appearance;
(3) v prepared by the method2O3/VO2The powder can be applied to water cracking hydrogen production electro-catalysts in the field of electro-catalysis.
Description of the drawings:
FIG. 1 shows V prepared in example 3 of the present invention2O3/VO2An X-ray diffraction (XRD) pattern of the powder;
FIG. 2 shows V prepared in example 3 of the present invention2O3/VO2Scanning Electron Microscope (SEM) photographs of the powder;
FIG. 3 is a graph of V prepared in example 3 of the present invention2O3/VO2Linear Sweep Voltammetry (LSV) performance test plots of the powders.
The specific implementation mode is as follows:
the invention is explained in more detail below with reference to the drawings and the examples:
example 1:
(1) weighing NH4VO3And N-acetyl-L-cysteine (NAC) with the molar ratio of 1:3, respectively dissolving in 10ml of deionized water, wherein the concentration of a vanadium source is 0.02mol/L and the concentration of the NAC is 0.06mol/L, and magnetically stirring for 10min at room temperature to obtain a clear solution;
(2) mixing the two clear solutions in the step (1), and magnetically stirring at room temperature for 40min to obtain clear mixed solution;
(3) pouring the clear mixed solution in the step (2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 170 ℃ and the reaction time is 28 hours;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 10 hours at 40 ℃ to obtain V2O3/VO2And (3) powder.
Example 2:
(1) weighing NH4VO3And NAC in a 4: 9, respectively dissolving in 15ml of deionized water, wherein the concentration of a vanadium source is 0.267mol/L, the concentration of NAC is 0.06mol/L,magnetically stirring at room temperature for 20min to obtain a clear solution;
(2) mixing the two clear solutions in the step (1), and magnetically stirring for 50min at room temperature to obtain clear mixed solution;
(3) pouring the clear mixed solution in the step (2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 220 ℃ and the reaction time is set to be 20 hours;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 8 hours at the temperature of 60 ℃ to obtain V2O3/VO2And (3) powder.
Example 3:
(1) weighing NH4VO3And NAC in a 3: 5, respectively dissolving the vanadium source and the NAC in 15ml of deionized water, wherein the concentration of the vanadium source is 0.04mol/L and the concentration of the NAC is 0.067mol/L, and magnetically stirring for 20min at room temperature to obtain clear solutions;
(2) mixing the two clear solutions in the step (1), and magnetically stirring for 50min at room temperature to obtain clear mixed solution;
(3) pouring the clear mixed solution in the step (2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 220 ℃ and the reaction time is set to be 20 hours;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 8 hours at the temperature of 60 ℃ to obtain V2O3/VO2And (3) powder.
FIG. 1 shows V prepared in this example2O3/VO2X-ray diffraction (XRD) pattern of the powder. FIG. 1 shows that the XRD characteristic peak of the product prepared by the invention is respectively associated with V2O3And VO2The characteristic peaks are corresponding to each other, which shows that V is prepared by the invention2O3/VO2And (3) mixing the materials.
FIG. 2 shows V prepared in this example2O3/VO2Scanning Electron Microscope (SEM) photographs of the powder. FIG. 2 shows the preparation of V according to the invention2O3/VO2The powder has regular nanometer rod-shaped appearance.
FIG. 3 shows V prepared in this example2O3/VO2Linear Sweep Voltammetry (LSV) performance test plots of the powders. FIG. 3 shows that the sample has a current density of 10mA/cm2When the catalyst is used, the overpotential of the catalyst is 453mV, and the catalyst has good electrocatalytic hydrogen evolution activity.
Example 4:
(1) weighing NH4VO3And N-acetyl-L-cysteine (NAC) in a 4: 7, respectively dissolving the vanadium source and the NAC in 20ml of deionized water, wherein the concentration of the vanadium source is 0.04mol/L and the concentration of the NAC is 0.07mol/L, and magnetically stirring the solution at room temperature for 30min to obtain a clear solution;
(2) mixing the two clear solutions in the step (1), and magnetically stirring at room temperature for 60min to obtain clear mixed solution;
(3) pouring the clear mixed solution in the step (2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 200 ℃ and the reaction time is set to be 20 hours;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 6 hours at the temperature of 60 ℃ to obtain V2O3/VO2And (3) powder.
Claims (2)
1. V-shaped groove2O3/VO2The preparation method of the composite electrocatalyst is characterized by comprising the following steps of:
reacting NH4VO3With an aqueous solution of N-acetyl-L-cysteine NAC, according to NH4VO3: mixing and uniformly dispersing NAC (1-4) and (3-7), and then carrying out hydrothermal reaction at 170-220 ℃ for 18-28 h to obtain V2O3/VO2A composite electrocatalyst.
2. A V according to claim 12O3/VO2The preparation method of the composite electrocatalyst is characterized by comprising the following specific steps of:
1) reacting NH4VO3And respectively dissolving NAC in 10-20 ml of deionized water, and magnetically stirring at room temperature for 10-30 min to obtain NH4VO3Solution and NAC solution;
2) reacting NH in 1)4VO3Mixing the solution and the NAC solution according to the molar ratio of solute (1-4) to solute (3-7), respectively dissolving the mixture in 10-20 ml of deionized water, wherein the concentration of a vanadium source is 0.02-0.04 mol/L, the concentration of NAC is 0.06-0.7 mol/L, and magnetically stirring at room temperature for 40-60 min to obtain a clear mixed solution;
3) pouring the clear mixed solution obtained in the step 2) into a 50ml reaction kettle, sealing, and carrying out hydrothermal reaction in an oven, wherein the reaction temperature is set to be 170-220 ℃, and the reaction time is 18-28 h;
4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out suction filtration on the solution, then respectively cleaning the solution for 3 times by using ethanol and deionized water, and finally carrying out vacuum drying on the obtained black powder for 5-10 h at the temperature of 40-70 ℃ to obtain V2O3/VO2And (3) powder.
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| CN109772366A (en) * | 2019-03-18 | 2019-05-21 | 陕西科技大学 | A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst |
| CN110560078A (en) * | 2019-09-30 | 2019-12-13 | 陕西科技大学 | v-shaped groove2O3Preparation method of @ Ni difunctional composite electrocatalyst |
| CN112811467A (en) * | 2021-01-18 | 2021-05-18 | 陕西科技大学 | V-shaped groove2O3Method for preparing nanoparticles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008011198A2 (en) * | 2006-01-18 | 2008-01-24 | Vanderbilt University | Method of preparing vanadium dioxide nanoparticles |
| CN102910675A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Preparation of VO2 nanosheet material and applications thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008011198A2 (en) * | 2006-01-18 | 2008-01-24 | Vanderbilt University | Method of preparing vanadium dioxide nanoparticles |
| CN102910675A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Preparation of VO2 nanosheet material and applications thereof |
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