CN115957744A - ZnWO 4 Preparation method and application of photocatalyst - Google Patents
ZnWO 4 Preparation method and application of photocatalyst Download PDFInfo
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- CN115957744A CN115957744A CN202310043350.5A CN202310043350A CN115957744A CN 115957744 A CN115957744 A CN 115957744A CN 202310043350 A CN202310043350 A CN 202310043350A CN 115957744 A CN115957744 A CN 115957744A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 11
- 239000011975 tartaric acid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 230000001007 puffing effect Effects 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 238000004817 gas chromatography Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 3
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 abstract 1
- 239000004246 zinc acetate Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 10
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 7
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- -1 tungstate radicals Chemical class 0.000 description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention relates to ZnWO 4 A preparation method and application of a photocatalyst, belonging to the technical field of photocatalytic materials. The preparation method comprises the following steps: stirring and dissolving ammonium tungstate in a hydrogen peroxide solution, dissolving zinc acetate in deionized water, adding tartaric acid, stirring and dissolving, mixing the two solutions, stirring, placing in an oven, grinding after drying and puffing a sample, placing in a muffle furnace for calcining, washing and drying to obtain ZnWO 4 A photocatalyst. The invention has stronger photocatalytic oxidation reduction capability, increases the visible light catalytic activity, has better photocatalytic hydrogen evolution performance, and has great development and application prospects in the aspect of photocatalytic green clean energy.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to ZnWO 4 A preparation method and application of the photocatalyst.
Background
The photocatalysis technology is a technology for converting solar energy into high value-added chemicals, and has good application potential in the aspects of developing clean energy and relieving increasingly serious energy crisis and environmental problems. Solar photocatalytic hydrogen production by water decomposition for converting and storing solar energy in a clean, efficient, low-cost and large-scale manner has become one of the most important subjects in the field of energy research.
ZnWO 4 Is a common photocatalyst and is applied to the fields of environment and energy due to excellent stability, but ZnWO 4 Has not been reported as a hydrogen evolution photocatalyst, and ZnWO 4 The preparation method of the photocatalyst is less, the preparation material is single, and the recombination of photon-generated carriers is quicker, so that the photocatalytic performance of the photocatalyst is poorer.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides ZnWO 4 A preparation method and application of the photocatalyst.
The technical scheme adopted by the invention is as follows:
ZnWO 4 The preparation method of the photocatalyst comprises the following steps: stirring and dissolving ammonium tungstate in a hydrogen peroxide solution to obtain a solution A; dissolving zinc acetate dihydrate in deionized water, adding tartaric acid, and stirring until the tartaric acid is dissolved to obtain a solution B; mixing the solution A and the solution B, stirring, placing in an oven, drying, puffing, grinding, calcining in a muffle furnace, naturally cooling, washing, centrifuging, and drying at 60 deg.C to obtain ZnWO 4 A photocatalyst.
Further, a ZnWO as mentioned above 4 The preparation method of the photocatalyst comprises the steps of preparing ammonium tungstate hydrate, and preparing the photocatalyst by using ammonium tungstate hydrate and adopting a molecular formula of H 40 N 10 O 41 W 12 ·xH 2 O, molecular weight 3042.58.
Further, a ZnWO as described above 4 The preparation method of the photocatalyst comprises the following steps of adding ammonium tungstate hydrate, zinc acetate dihydrate and tartaric acid in a molar ratio of W: zn: tartaric acid = 1.
Further, a ZnWO as mentioned above 4 Preparation of photocatalystThe concentration of the hydrogen peroxide solution is 30 percent.
Further, a ZnWO as mentioned above 4 The preparation method of the photocatalyst comprises the step of setting the temperature of the oven at 80 ℃.
Further, a ZnWO as mentioned above 4 A method for preparing a photocatalyst, the calcination conditions being: the temperature is raised to 400 ℃ at a speed of 2 ℃/min, then raised to 600 ℃ at a speed of 1 ℃/min, and kept at 600 ℃ for 240min.
ZnWO prepared by the preparation method of any one of the above 4 The application of the photocatalyst in the catalytic hydrogen evolution under the irradiation of visible light.
Further, the application and the method are as follows: under the condition of normal temperature and normal pressure, 20mL of methanol aqueous solution is added into a container, 20 mu L of chloroplatinic acid aqueous solution is added, and then 20mg of ZnWO is added 4 Carrying out ultrasonic treatment on the photocatalyst for 10min to obtain dispersion; introducing argon gas into the container at a rate of 40mL/min for 30min, sealing the container, taking 1000 μ L of gas in the container with a microinjector every 15min under the irradiation of visible light, detecting gas components by adopting a gas chromatography separation technology, and determining the hydrogen evolution concentration.
Further, in the above application, the concentration of the methanol aqueous solution is 1.25mol/L.
Further, in the above-mentioned application, the concentration of the chloroplatinic acid aqueous solution is 1wt%.
The invention has the beneficial effects that:
1. ZnWO of the invention 4 In the preparation process of the photocatalyst, the hydrogen peroxide solution can dissolve a large amount of ammonium tungstate which is hardly dissolved in other solutions, and the peroxygen radical is used as an initiator, so that free radical polymerization can be promoted, and tartrate can better complex zinc ions and tungstate radicals. In addition, the peroxy radical can inhibit the transition from the tungstate radical to the tungsten oxide crystal phase.
2. ZnWO of the invention 4 The photocatalyst has better photocatalytic performance, ammonium tungstate is dissolved in hydrogen peroxide solution, hydrogen peroxide can provide peroxy radicals, and due to the existence of the peroxy radicals, exciton dissociation is induced to generate holes, generation of photon-generated carriers is promoted, and hole electron recombination is inhibitedTime, thereby improving photocatalytic performance and solar energy utilization efficiency.
3. ZnWO of the invention 4 The photocatalyst has better performance of decomposing water and generating hydrogen by photocatalysis, and ZnWO is used for preparing the photocatalyst 4 The method has no report in the field of photocatalytic hydrogen evolution, is simple and convenient to operate, has low cost and mild conditions, and is beneficial to large-scale production.
Drawings
FIG. 1 shows ZnWO prepared in example 1 4 -1 ZnWO prepared in example 2 4 -2 XRD pattern of photocatalyst.
FIG. 2 is ZnWO prepared in example 1 4 -1 ZnWO prepared in example 2 4 -2 comparative hydrogen evolution diagram of photocatalyst.
FIG. 3 shows different H values detected by gas chromatography 2 Plot of volume versus peak area of gas chromatography.
Detailed Description
Example 1
ZnWO 4 The preparation method of the photocatalyst comprises the following steps:
stirring 2.55g of ammonium tungstate hydrate in 20mL of 30% hydrogen peroxide solution until the ammonium tungstate hydrate is dissolved to obtain a solution A; dissolving 2.19g of zinc acetate dihydrate into 10mL of deionized water, adding 4.5g of tartaric acid, and stirring until the mixture is dissolved to obtain a solution B; then mixing and stirring the solution A and the solution B, placing the mixture in an oven at 80 ℃, grinding the mixture after drying and expanding the sample, placing the mixture in a muffle furnace, heating the mixture to 400 ℃ at 2 ℃/min, heating the mixture to 600 ℃ at 1 ℃/min, keeping the temperature at 600 ℃ for 240min, naturally cooling and centrifugally washing the mixture, and placing the mixture in an oven at 60 ℃ to dry the mixture to obtain ZnWO 4 Photocatalyst, noted as ZnWO 4 -1。
Example 2
Control ZnWO 4 The preparation method comprises the following steps:
uniformly stirring 2.55g of ammonium tungstate hydrate in 20mL of deionized water to obtain a solution A; dissolving 2.19g of zinc acetate dihydrate in 10mL of deionized water, adding 4.5g of tartaric acid, and stirring until the mixture is dissolved to obtain a solution B; then mixing the solution A and the solution B, stirring uniformly, and standingDrying and puffing the sample in an oven at 80 ℃, grinding, placing in a muffle furnace, heating to 400 ℃ at 2 ℃/min, heating to 600 ℃ at 1 ℃/min, keeping at 600 ℃ for 240min, naturally cooling, centrifugally washing, and placing in an oven at 60 ℃ for drying to obtain a comparative sample ZnWO 4 Photocatalyst, noted as ZnWO 4 -2。
FIG. 1 is ZnWO prepared in example 1 4 -1 ZnWO prepared in example 2 4 -2 XRD pattern of photocatalyst. As can be seen from FIG. 1, znWO 4 The diffraction peak of the-1 sample is sharp, which indicates that the crystallinity of the product is good, and corresponds to XRD standard card JCPDS15-0774, while ZnWO 4 The-2 sample has obvious diffraction peaks at 22.5 degrees and 33.6 degrees, which correspond to diffraction angles of tungsten oxide, and shows that the peroxy radical can inhibit the growth to the tungsten oxide crystal phase.
Example 3ZnWO 4 Application of photocatalyst in catalytic decomposition of water under irradiation of visible light
1) At normal temperature and pressure, a 2 mL of 1.25mol/L aqueous methanol solution was added to a vessel, 20. Mu.L of 1wt% aqueous chloroplatinic acid was added, and 20mg of the ZnWO prepared in example 1 was added 4 1, performing ultrasonic treatment on the photocatalyst for 10min to obtain a dispersion; introducing argon gas into the container at a rate of 40mL/min for 30min, sealing the container, taking 1000 μ L of gas in the container with a microinjector every 15min under the irradiation of visible light, detecting the gas components of the sample by adopting a gas chromatography separation technology, and determining the hydrogen evolution concentration.
2) Working according to step 1), except for using the ZnWO prepared in example 1 4 -1 replacement of the photocatalyst by ZnWO prepared in example 2 4 -2 photocatalyst, the other conditions are not changed, 1000 mul of gas in a container is taken by a micro injector every 15min, gas components of the sample are detected by adopting a gas chromatography separation technology, and the concentration of hydrogen evolution is measured.
FIG. 3 shows different H values detected by gas chromatographic separation 2 The degree of fit of the graph in fig. 3, which is a standard curve, is 0.9993, indicating that there is a good linear relationship between the two, and the peak area of the gas chromatograph and the substance concentration can be converted by the standard curve.
The peak area of the extracted gas is measured by gas chromatography, and then converted into its hydrogen evolution concentration by a hydrogen peak area standard curve, as shown in fig. 2, one hour later, znWO 4 -1 production of H 2 The amount is 178.56. Mu. Mol/L ZnWO 4 -2 production of H 2 The amount of 43.45. Mu. Mol/L, znWO 4 -1 is obviously better than ZnWO 4 And 2, the sample shows that the photoproduction electron transfer capability is stronger after the hydrogen peroxide is added, and the electron hole pair has stronger oxidation reduction capability.
Claims (10)
1. ZnWO 4 The preparation method of the photocatalyst is characterized by comprising the following steps: stirring and dissolving ammonium tungstate in a hydrogen peroxide solution to obtain a solution A; dissolving zinc acetate dihydrate in deionized water, adding tartaric acid, and stirring until the tartaric acid is dissolved to obtain a solution B; mixing the solution A and the solution B, stirring, placing in an oven, drying, puffing, grinding, calcining in a muffle furnace, naturally cooling, washing, centrifuging, and drying at 60 deg.C to obtain ZnWO 4 A photocatalyst.
2. ZnWO according to claim 1 4 The preparation method of the photocatalyst is characterized in that the ammonium tungstate is ammonium tungstate hydrate, and the molecular formula is H 40 N 10 O 41 W 12 ·xH 2 O, molecular weight 3042.58.
3. ZnWO according to claim 2 4 The preparation method of the photocatalyst is characterized in that the addition amounts of the ammonium tungstate hydrate, the zinc acetate dihydrate and the tartaric acid are as follows, in terms of molar ratio, W: zn: tartaric acid = 1.
4. ZnWO according to claim 1 4 The method for producing a photocatalyst is characterized in that the concentration of the hydrogen peroxide solution is 30%.
5. ZnWO according to claim 1 4 Photo catalysisThe preparation method of the curing agent is characterized in that the temperature set by the oven is 80 ℃.
6. ZnWO according to claim 1 4 The preparation method of the photocatalyst is characterized in that the calcination conditions are as follows: the temperature is raised to 400 ℃ at a speed of 2 ℃/min, then raised to 600 ℃ at a speed of 1 ℃/min, and kept at 600 ℃ for 240min.
7. ZnWO prepared by the preparation method of any one of claims 1 to 6 4 The application of the photocatalyst in the catalytic hydrogen evolution under the irradiation of visible light.
8. Use according to claim 7, characterized in that the method is as follows: under the condition of normal temperature and normal pressure, 20mL of methanol aqueous solution is added into a container, 20 mu L of chloroplatinic acid aqueous solution is added, and then 20mg of ZnWO is added 4 Performing ultrasonic treatment on the photocatalyst for 10min to obtain dispersion; introducing argon gas into the container at a rate of 40mL/min for 30min, sealing the container, taking 1000 μ L of gas in the container with a microinjector every 15min under the irradiation of visible light, detecting gas components by adopting a gas chromatography separation technology, and determining the hydrogen evolution concentration.
9. Use according to claim 8, wherein the concentration of the aqueous methanol solution is 1.25mol/L.
10. Use according to claim 8, wherein the concentration of the aqueous chloroplatinic acid solution is 1wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116809107A (en) * | 2023-06-27 | 2023-09-29 | 辽宁大学 | ZnWO (zinc-oxygen) device 4 /g-C 3 N 4 Heterostructure nanofiber catalyst and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557141A (en) * | 2012-03-02 | 2012-07-11 | 河北联合大学 | Structure-oriented synthetic method of zinc tungstate nanometer sheet |
| CN106140141A (en) * | 2016-06-21 | 2016-11-23 | 常州工程职业技术学院 | A kind of oxygen-containing defected ZnWO4catalysis material and preparation method thereof |
| CN108585111A (en) * | 2018-05-12 | 2018-09-28 | 辽宁大学 | The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam |
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- 2023-01-29 CN CN202310043350.5A patent/CN115957744B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557141A (en) * | 2012-03-02 | 2012-07-11 | 河北联合大学 | Structure-oriented synthetic method of zinc tungstate nanometer sheet |
| CN106140141A (en) * | 2016-06-21 | 2016-11-23 | 常州工程职业技术学院 | A kind of oxygen-containing defected ZnWO4catalysis material and preparation method thereof |
| CN108585111A (en) * | 2018-05-12 | 2018-09-28 | 辽宁大学 | The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam |
Non-Patent Citations (4)
| Title |
|---|
| J. GRABIS ET AL.: ""PHOTOCATALYTIC ACTIVITY OF ZnWO4 NANOPARTICLES PREPARED BY COMBUSTION SYNTHESIS"", 《LATVIAN JOURNAL OF CHEMISTRY》, pages 93 - 98 * |
| MEI‑TING LI ET AL.: ""Effects of tungsten source and tartrate additive on the microstructure and photoluminescence of hydrothermally crystallized ZnWO4"", 《TUNGSTEN》, vol. 1, pages 266 - 275 * |
| WU YAN ET AL.: ""Photocatalytic Activity of Nanosized ZnWO, Prepared by the Sol-gel Method"", 《CHEM. RES. CHINESE U.》, vol. 23, no. 4, pages 465 - 468, XP022856031, DOI: 10.1016/S1005-9040(07)60100-7 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116809107A (en) * | 2023-06-27 | 2023-09-29 | 辽宁大学 | ZnWO (zinc-oxygen) device 4 /g-C 3 N 4 Heterostructure nanofiber catalyst and preparation method and application thereof |
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