CN113019365B - Z type WO3:Yb3+,Er3+/Ag/Ag3VO4Preparation method and application of/Ag photocatalyst - Google Patents
Z type WO3:Yb3+,Er3+/Ag/Ag3VO4Preparation method and application of/Ag photocatalyst Download PDFInfo
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- CN113019365B CN113019365B CN202110275747.8A CN202110275747A CN113019365B CN 113019365 B CN113019365 B CN 113019365B CN 202110275747 A CN202110275747 A CN 202110275747A CN 113019365 B CN113019365 B CN 113019365B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- GSDSWSVVBLHKDQ-JTQLQIEISA-N Levofloxacin Chemical compound C([C@@H](N1C2=C(C(C(C(O)=O)=C1)=O)C=C1F)C)OC2=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-JTQLQIEISA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229960003376 levofloxacin Drugs 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052691 Erbium Inorganic materials 0.000 claims description 5
- 239000003242 anti bacterial agent Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 238000004020 luminiscence type Methods 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 229940088710 antibiotic agent Drugs 0.000 claims description 3
- 230000003115 biocidal effect Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 230000000593 degrading effect Effects 0.000 claims description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 2
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 17
- 239000004065 semiconductor Substances 0.000 abstract description 8
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 5
- 238000007540 photo-reduction reaction Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 3
- 230000027756 respiratory electron transport chain Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002803 fossil fuel Substances 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 239000000891 luminescent agent Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 239000002784 hot electron Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
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- 238000005067 remediation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
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Abstract
The invention discloses Z type WO3:Yb3+,Er3+/Ag/Ag3VO4A preparation method and application of an Ag photocatalyst. Firstly adopts a hydrothermal method to prepare WO3:Yb3+,Er3+And Ag3VO4Secondly, silver nano particles are loaded on Ag by adopting a photo-reduction method3VO4Forming Ag/Ag on the surface of3VO4and/Ag, and finally preparing the target product by a high-temperature calcination method. In the present invention, WO3Can be used as a substrate of an up-conversion light-emitting agent and also can be used as a high-efficiency semiconductor catalyst, so that the photocatalytic activity is greatly improved. In addition, the silver nanoparticles having the plasma effect can serve as a conductive channel and a promoter to promote electron transfer and increase the yield of hydrogen. Therefore, the photoresponse range is remarkably widened, and the separation efficiency of electron-hole pairs is greatly improved. The synthesized photocatalyst is used for photocatalytic degradation of levofloxacin, and generates clean energy, namely hydrogen.
Description
Technical Field
The invention belongs to the field of photocatalysis, and particularly relates to synthesis ofZ-shaped WO simultaneously having up-conversion luminescent agent and plasma effect3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst and application thereof in degrading antibiotic pollutants under sunlight and photolyzing water to produce hydrogen.
Background
Currently, global energy demand is primarily dependent on fossil fuels. However, as a non-renewable energy source, fossil fuels will be rapidly depleted in the near future. With the globalization of economy and the increase of population, the demand for energy will become larger and larger in the future. To address the problem of energy demand, it is important to develop clean and renewable energy sources. Fortunately, hydrogen, as a zero-emission fuel and a renewable energy source, is a promising substitute for traditional fossil fuels. Traditionally, water-gas separation reactions and natural gas-steam reactions are common hydrogen production strategies in the industry. However, these processes release large amounts of carbon dioxide, which causes greenhouse effects and climate change. Photocatalytic technology combined with solar energy can produce clean hydrogen energy by decomposing water. Meanwhile, some substances with strong reducibility are added into the wastewater as sacrificial agents, such as antibiotics, so that not only can high-efficiency hydrogen production be realized, but also the wastewater can be used for purifying the water environment. In recent years, people do a lot of work on the aspect of photocatalytic hydrogen production, but still have some problems, such as low sunlight utilization rate, high raw material cost, easy recombination of electron-hole pairs and the like. Therefore, in order to realize the practical application of the photocatalytic technology using the pollutants as the sacrificial agent in hydrogen production, the development of a novel photocatalyst with high performance is urgent.
Most wide bandgap semiconductor photocatalysts have high catalytic activity. However, they can only absorb ultraviolet light for photocatalytic reaction. However, the proportion of ultraviolet light in sunlight is very small (about 4%), resulting in low sunlight utilization. The up-conversion luminescent agents used in recent years can convert light of low energy into light of high energy, thereby improving the utilization rate of sunlight. However, the upconversion light-emitting agent particles are mostly used in a form directly bonded to or coated with a semiconductor, which is disadvantageous for light transmission, absorption and conversion. The above problems can be effectively solved if the semiconductor particles are prepared to have both photocatalytic and photoconversion properties. Furthermore, in recent years, the study of the surface plasmon resonance effect can raise new expectations for the field of photocatalysis. The metal with plasma resonance effect can generate high-energy 'hot electron', and can play a role in promoting electron transfer in a Z-type photocatalytic system. Based on the above, it is necessary to develop a highly efficient photocatalyst and to construct a novel photocatalytic system.
Disclosure of Invention
The invention aims to provide a novel Z-shaped WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, obviously enhances the photocatalytic activity of the semiconductor photocatalyst. By means of the excellent light conversion performance and catalytic performance of the up-conversion light-emitting agent, excitation of a self wide band gap semiconductor and a plasma effect is enhanced, the response range of light is greatly widened, and the separation efficiency of electron hole pairs is also obviously improved.
The technical scheme adopted by the invention is as follows: z type WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, firstly adopts a hydrothermal method to prepare WO3:Yb3+,Er3+And Ag3VO4Secondly, silver nano particles are loaded on Ag by adopting a photo-reduction method3VO4Forming Ag/Ag on the surface of3VO4Ag, finally preparing the Z-type WO by a high-temperature calcination method3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst. The preparation method comprises the following steps:
1)WO3:Yb3+,Er3+the preparation of (1): mixing Na2WO4·2H2O、Yb2O3And Er2O3Dissolving in hot nitric acid, adding ethanol into the mixed solution, stirring for dissolving, transferring into high-pressure kettle, performing hydrothermal reaction for 24 hr, cleaning, centrifuging, drying, and annealing to obtain WO3:Yb3+,Er3+；
2)Ag3VO4The preparation of (1): AgNO is added3Dissolving in a mixed solution of concentrated nitric acid and deionized water to obtain a solution A; reacting NH4VO3Ultrasonically dissolving the mixture in a mixed solution of NaOH and deionized water to obtain a solution B; mixing solution A and solution B, stirring for 30-40min, adjusting pH of the mixed solution to 10, stirring at 80 deg.C for 12 hr, centrifuging, washing, and drying to obtain Ag3VO4A powder;
3)Ag/Ag3VO4preparation of Ag powder: mixing Ag3VO4Dissolving the powder in ethanol, ultrasonically dispersing for 10min, irradiating the obtained suspension with 300W xenon lamp, heating at 50 deg.C for 1.0h, and mixing with Ag+Reducing to Ag, centrifuging, washing, drying to obtain Ag/Ag3VO4Ag powder;
4)WO3:Yb3+,Er3+/Ag/Ag3VO4preparation of Ag photocatalyst: mixing WO3:Yb3+,Er3+And Ag/Ag3VO4Adding Ag powder into deionized water, stirring and dispersing for 30-40min to obtain suspension; heating the obtained suspension to boiling point by magnetic stirring, keeping for 30min, centrifuging, collecting solid powder, washing with deionized water and ethanol, drying at 60 deg.C for 12 hr, and calcining in muffle furnace to obtain WO3:Yb3+,Er3+/Ag/Ag3VO4Ag powder.
Further, the above-mentioned Z-type WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, in the step 1), the temperature of hydrothermal reaction is 180 ℃; the annealing treatment is to anneal for 2.0h at 300 ℃ in an air atmosphere.
Further, the above-mentioned Z-type WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, step 1) the up-conversion luminescence agent WO3:Yb3+,Er3+In mole percent, 1 mol% of Yb3+And 1 mol% Er3+。
Further, the above-mentioned Z-form WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, step 2) In the method, concentrated nitric acid and deionized water are mixed according to the volume ratio of 1: 5; and (4) according to the solid-liquid ratio, NaOH and deionized water are 4: 25.
Further, the above-mentioned Z-type WO3:Yb3+,Er3+/Ag/Ag3VO4The Ag photocatalyst is calcined in a muffle furnace in the step 4), wherein the calcination temperature is 300 ℃, and the calcination time is 2.0 h.
Further, said WO3:Yb3+,Er3+/Ag/Ag3VO4In the Ag photocatalyst, 1 mol% of Yb is contained3+And 1 mol% Er3+。
Z-shaped WO provided by the invention3:Yb3+,Er3+/Ag/Ag3VO4The application of the/Ag photocatalyst in degrading antibiotics under sunlight.
Further, the method comprises the following steps: adding WO Z into solution containing antibiotics3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, irradiated under sunlight.
Further, the antibiotic is levofloxacin.
Z-shaped WO provided by the invention3:Yb3+,Er3+/Ag/Ag3VO4The application of the/Ag photocatalyst in photocatalytic hydrogen production.
The invention has the beneficial effects that:
in the present invention, Z-form WO3:Yb3+,Er3+/Ag/Ag3VO4the/Ag photocatalyst is prepared by a hydrothermal method and a high-temperature calcination method, and has high catalyst yield, high catalyst activity and obvious effect. To date, a large number of semiconductor photocatalysts responsive to visible light have been studied and applied for environmental remediation. However, near infrared light (NIR), which accounts for about 44% of sunlight, has been rarely studied in the field of photocatalysis. In the present invention, the upconversion light-emitting agent WO3:Yb3+,Er3+Can absorb 980nm near infrared light, and convert the light into ultraviolet light for exciting WO3The light response range is widened, and the emitted visible light is used for exciting silver nano particlesPlasma effect. Meanwhile, WO3:Yb3+,Er3+Can degrade organic pollutants in the wastewater by photocatalysis. The silver nano-particles with the plasma effect can be used as a conductive channel and a promoter to accelerate the electron transfer and improve the hydrogen yield. Z-form WO prepared by the invention3:Yb3+,Er3+/Ag/Ag3VO4the/Ag photocatalyst can provide new insight for designing and constructing a high-performance and high-efficiency photocatalytic system.
Drawings
FIG. 1a is WO3:Yb3+,Er3+X-ray powder diffraction (XRD) pattern of (a).
FIG. 1b is Ag3VO4X-ray powder diffraction (XRD) pattern of (a).
FIG. 1c is Ag/Ag3VO4X-ray powder diffraction (XRD) pattern of/Ag.
FIG. 1d is WO3:Yb3+,Er3+/Ag3VO4X-ray powder diffraction (XRD) pattern of (a).
FIG. 1e is WO3:Yb3+,Er3+/Ag/Ag3VO4X-ray powder diffraction (XRD) pattern of/Ag.
FIG. 2 is WO3:Yb3+,Er3+/Ag/Ag3VO4Scanning Electron Microscope (SEM) picture of/Ag.
FIG. 3 is WO3:Yb3+,Er3+/Ag/Ag3VO4Transmission Electron Microscope (TEM) image (a) and high magnification transmission electron microscope (HRTEM) image (b) of/Ag.
FIG. 4 is WO3:Yb3+,Er3+/Ag/Ag3VO4X-ray energy dispersive spectroscopy (EDX) diagram of/Ag.
FIG. 5 is WO3:Yb3+,Er3+/Ag/Ag3VO4X-ray photoelectron spectroscopy (XPS) of all elements in/Ag.
FIG. 6a is Ag3VO4、WO3、WO3:Yb3+,Er3+、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4Solid ultraviolet diagram of/Ag.
FIG. 6b-1 is WO3:Yb3+,Er3+The measured ultraviolet pattern of the solid.
FIG. 6b-2 is Ag3VO4The measured ultraviolet pattern of the solid.
FIG. 7 is WO3:Yb3+,Er3+、Ag3VO4、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4Ag degradation effect graph.
FIG. 8 is Ag3VO4、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4The hydrogen production effect of Ag.
FIG. 9 shows a Z-shaped WO3:Yb3+,Er3+/Ag/Ag3VO4A mechanism diagram of the Ag photocatalyst photocatalytic degradation of levofloxacin and hydrogen production.
Detailed Description
Example 1WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst
(I) preparation method
(1) Up-conversion luminescence agent WO3:Yb3+,Er3+Preparation of
According to the stoichiometric ratio, 3.00g of Na is taken2WO4·2H2O、0.0719g Yb2O3And 0.0698g Er2O3Dissolved in 5mL of 60 ℃ hot nitric acid, and then 30mL of ethanol was added to the resulting mixed solution, and dissolved with stirring to give a yellow solution, which was then transferred to an autoclave. Keeping the autoclave at 180 ℃ and carrying out hydrothermal reaction for 24 h. The resulting product was thoroughly washed with distilled water and centrifuged 6 times. Drying at 80 deg.C, and annealing at 300 deg.C for 2.0h in air atmosphere to obtain WO3:Yb3+,Er3+In mol% of 1 mol% of Yb3+And 1 mol% Er3+。
(2)Ag3VO4Preparation of (2)
Weighing 7.6g AgNO3Dissolving the solid in a solution of 6mL of concentrated nitric acid and 30mL of deionized water to obtain a clear and transparent solution A; weighing 1.76NH4VO3The solid was dissolved in a solution of 4.8g NaOH and 30mL deionized water and sonicated to completely dissolve, yielding clear and transparent solution B. And mixing the solution A and the solution B, stirring for 30min, and adjusting the pH of the mixed solution to 10 by using a 4mol/L NaOH solution. Transferring the obtained mixed solution into a 250mL three-neck flask, stirring at 80 ℃ for 12h, centrifuging, washing and drying to obtain orange-yellow Ag3VO4And (3) powder.
(3)Ag/Ag3VO4Preparation of/Ag
1.50g of Ag3VO4The powder was dissolved in 20mL of ethanol and dispersed thoroughly with ultrasound for 10 min. Irradiating the obtained suspension with 300W xenon lamp, heating at 50 deg.C for 1.0h, and collecting Ag+Reducing the Ag into Ag. Repeatedly centrifuging, washing with deionized water, and oven drying at 70 deg.C for 12 hr to obtain Ag/Ag3VO4Ag powder.
(4)WO3:Yb3+,Er3+/Ag/Ag3VO4Preparation of/Ag
1.52g of WO3:Yb3+,Er3+And 0.89g Ag/Ag3VO4the/Ag powder was added to a 100mL beaker with 50mL deionized water and the resulting mixture was thoroughly dispersed for 30min to give a homogeneous suspension. The suspension was heated to boiling point with magnetic stirring, held for 30min, centrifuged to collect solid powder, washed several times with deionized water and ethanol. Drying in a drying oven at 60 ℃ for 12h, calcining in a muffle furnace at 300 ℃ for 2.0h to obtain WO3:Yb3+,Er3+/Ag/Ag3VO4Ag powder.
(II) detection
1. FIGS. 1a to 1e are WO3:Yb3+,Er3+，Ag3VO4，Ag/Ag3VO4/Ag，WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4X-ray powder diffraction (XRD) pattern of/Ag.
WO prepared as shown in FIG. 1a3:Yb3+,Er3+Has a main diffraction peak in WO3The (002) (020), (200), (112), (022), (202) and (222) crystal planes of (JCPDS #72-1465) correspond to 2 θ ═ 23.15 °, 23.61 °, 24.37 °, 28.96 °, 33.30 °, 34.19 ° and 41.92 °, respectively. As can be seen from fig. 1b, diffraction peaks were found at 19.20 °, 30.86 °, 32.33 °, 35.07 °, 35.94 ° and 38.92 ° with monoclinic α -Ag3VO4(JCPDS #43-0542) has (011), (-121), (301), (202), and (022) matches. As shown in FIG. 1c, except for Ag3VO4Besides the diffraction peaks, there are 3 distinct diffraction peaks at the 2 theta values of 38.12 degrees, 44.28 degrees and 64.43 degrees, which indicates that Ag nanoparticles are successfully loaded by the photoreduction method. As shown in FIG. 1d, WO can be seen3:Yb3+,Er3+And Ag3VO4Characteristic diffraction peaks of (a) indicating the formation of binary WO3:Yb3+,Er3+/Ag3VO4And (c) a complex. In FIG. 1e, WO can be observed simultaneously3:Yb3+,Er3+、Ag3VO4And diffraction peaks of Ag. The above results show that WO was successfully prepared3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst.
2. FIG. 2 is WO3:Yb3+,Er3+/Ag/Ag3VO4Scanning Electron Microscope (SEM) picture of/Ag.
As can be seen from FIG. 2, WO3:Yb3+,Er3+The nano-particles present the geometrical characteristics of a cuboid with the length of 80-100nm, the width of 70-80nm and the thickness of 20-30 nm. Pure Ag3VO4The length of the nano particles is 100-120nm, the width is 80-100nm, the thickness is 30-50 nm, and the nano particles are also cuboid particles with a certain nano scale, but the nano particles are more than WO3:Yb3+,Er3+Slightly larger. As shown in FIG. 2, two kinds of rectangular parallelepiped particles are combined to form WO3:Yb3+,Er3+/Ag3VO4A photocatalytic system. From the appearance, the closely connected nano cuboid particles make the electrons easier to transfer. Meanwhile, the combination of the two nano cuboid morphology characteristics particles can provide abundant redox reaction sites for organic molecule degradation, thereby improving the photocatalytic performance. At the same time, in Ag3VO4Some small spherical nanoparticles with a diameter of 10-20nm were observed on both sides, indicating that Ag nanoparticles have been successfully deposited on Ag by photo-reduction3VO4Of the surface of (a). In conclusion, we have successfully prepared WO3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst.
3. FIG. 3 is WO3:Yb3+,Er3+/Ag/Ag3VO4Transmission Electron Microscope (TEM) image (a) and high magnification transmission electron microscope (HRTEM) image (b) of/Ag.
In FIG. 3 a shows WO3:Yb3+,Er3+/Ag/Ag3VO4The structure composition and position relation of the/Ag photocatalyst. In combination with the SEM image of FIG. 2, it can be determined that the left black bulk particles are Ag3VO4The smaller black particles on the right are WO3:Yb3+,Er3+. It was also observed that Ag nanoparticles having an average particle diameter of about 10nm were entrapped in WO3:Yb3+,Er3+And Ag3VO4In between, other Ag nanoparticles are located in Ag3VO4To the other side of the same. Furthermore, in fig. 3 b, the HRTEM image shows the lattice fringes of the specific substance. 0.363nm lattice fringes and WO3:Yb3+,Er3+The (200) crystal planes of (A) and (B) are identical. In addition, the lattice fringes are 0.238nm with Ag3VO4The (121) crystal plane of (A) is identical. In WO3:Yb3+,Er3+And Ag3VO4In between and in Ag3VO4The other side of the silver nano-particles is provided with two 0.236nm lattice stripes which belong to Ag nano-particles. Based on the above calculation and analysis, WO was successfully prepared3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst.
4. FIG. 4 is WO3:Yb3+,Er3+/Ag/Ag3VO4X-ray energy dispersive spectroscopy (EDX) diagram of/Ag.
The characteristic peaks of all elements in the prepared sample can be clearly seen from fig. 4, which demonstrates that the photocatalyst consists of these elements, without other impurities. The characteristic peaks of W, Yb, Er and O elements are found, and WO is determined3:Yb3+,Er3+Is present. In addition, characteristic peaks of V, Ag and O were also detected, demonstrating that Ag3VO4And the presence of Ag in3VO4And SPR effects in Ag nanoparticles. These results are substantially consistent with those of XRD, SEM and TEM. It was demonstrated that the Z-type photocatalyst has been successfully prepared.
5. FIG. 5 is WO3:Yb3+,Er3+/Ag/Ag3VO4XPS spectra of all elements in/Ag.
Using X-ray photoelectron spectroscopy (XPS) on WO3:Yb3+,Er3+/Ag/Ag3VO4The elemental composition and valence structure of/Ag were characterized and the results are shown in FIG. 5. As can be seen from FIG. 5, WO3:Yb3+,Er3+/Ag/Ag3VO4The Ag/W sample contains 6 elements of W, Yb, Er, V, Ag and O, and each peak in the sample is clear. The results show that WO3:Yb3+,Er3+/Ag/Ag3VO4the/Ag composite material is successfully prepared as a Z-type photocatalyst.
6. FIG. 6a, FIG. 6b-1 and FIG. 6b-2 are Ag3VO4、WO3，WO3:Yb3+,Er3+、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4Solid UV-map of/Ag and estimated WO3:Yb3+,Er3+And Ag3VO4The bandwidth of (c).
As can be seen from FIG. 6a, WO3The particles have an absorption edge around 430nm, which indicates WO3Absorption in the near ultraviolet region. In thatDoped Yb3+And Er3+Ions to form WO3:Yb3+,Er3+And then, the absorption strength is obviously enhanced, and the absorption range is obviously widened. Ag3VO4There is an absorption edge around 635nm, which proves that Ag3VO4Can absorb both ultraviolet light and visible light. Notably, WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4Ag has stronger light absorption than that of a single photocatalyst. However, in combination with WO3:Yb3+,Er3+/Ag3VO4In contrast, WO3:Yb3+,Er3+/Ag/Ag3VO4The light absorption range of/Ag is wider, and even the light absorption range extends to a near infrared region. This is mainly due to WO3:Yb3+,Er3+The fluorescent material can be used as an up-conversion light-emitting agent to convert long-wave light into short-wave light. In addition, through the construction of the Z-type photocatalytic system, the response range of light is widened. Using Kubelka-Munk function,. alpha.hv ═ A (h v-E)bg)1/2The band gap of the semiconductor can be calculated, wherein alpha, h, v and EbgAnd a represents an absorption coefficient, planck constant, light frequency, band gap, and constant, respectively. As can be seen from FIGS. 6b-1 and 6b-2, WO was prepared3:Yb3+,Er3+And Ag3VO4The band gaps of (A) are 2.88eV and 1.94eV, respectively, which are substantially consistent with values reported in the literature.
Example 2WO3:Yb3+,Er3+/Ag/Ag3VO4Application of Ag photocatalyst in photocatalytic degradation of Levofloxacin (LEV) and hydrogen production
(I) WO3:Yb3+,Er3+、Ag3VO4、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4Ag degradation effect.
The experimental method comprises the following steps: mixing WO 0.1g Z3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalystThe mixture was placed in 100mL of 10mg/L levofloxacin solution. Irradiating with visible light at 25-28 deg.C for 180min, and sampling every 30 min. The results are shown in FIG. 7.
As can be seen from FIG. 7, each suspension was left in the dark for 30min before exposure to sunlight to reach absorption/desorption equilibrium. From the dark experiment, it can be seen that the LEV concentration in the presence of the photocatalyst is slightly reduced within 30min, indicating that the prepared photocatalysts have slight absorption effect on LEV. The blank shows that the non-catalytic photocatalytic degradation capability of LEV is weak in the absence of photocatalyst, confirming that LEV is photostable. When the suspension is irradiated with sunlight, the degradation rate of the LEV increases gradually with the increase of the irradiation time. Among them, WO3:Yb3+,Er3+/Ag/Ag3VO4the/Ag photocatalyst showed the highest degradation rate in these four samples, indicating that it had the highest photocatalytic performance. WO3:Yb3+,Er3+/Ag/Ag3VO4The degradation rate of the Ag photocatalyst to LEV reaches 90.44% after the irradiation of sunlight for 180 min. Under the same conditions, Ag3VO4、WO3:Yb3+,Er3+And WO3:Yb3+,Er3+/Ag/Ag3VO4The photocatalytic degradation activity is low, and the LEV degradation rates are respectively 33.67%, 56.84% and 63.80%.
(II) Ag3VO4、WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4The hydrogen production effect of Ag.
The photocatalytic performance of the photocatalyst can be evaluated by the hydrogen production amount of the prepared sample. FIG. 8 shows Ag3VO4、 WO3:Yb3+,Er3+/Ag3VO4And WO3:Yb3+,Er3+/Ag/Ag3VO4The change trend of the accumulated hydrogen production of Ag within 180 min. It can be seen that the hydrogen production of all three systems increases with longer irradiation time. Introduction of WO3:Yb3+,Er3+Form Z-type WO3:Yb3+,Er3+/Ag3VO4After the photocatalysis system, the hydrogen yield is obviously increased and can reach 345.22 mu mol/g under the same condition. The results show that WO3:Yb3+,Er3+/Ag/Ag3VO4The hydrogen yield of the Ag photocatalyst is the highest among three samples, and can reach 489.02 mu mol/g. Improvement of photocatalytic performance with WO3:Yb3+,Er3+/Ag/Ag3VO4The successful construction of the/Ag photocatalysis system is closely related, and the system can keep stronger positive valence band potential and negative conduction band potential. Secondly, WO3:Yb3+,Er3+Has excellent light conversion and photocatalysis performance, and obviously widens the light response range. Finally, Ag nano particles with SPR effect are used as a conductive channel and a cocatalyst, and the transfer of photo-generated electrons is greatly accelerated.
Claims (9)
- Z type WO 13:Yb3+,Er3+/Ag/Ag3VO4The Ag photocatalyst is characterized in that the preparation method comprises the following steps:1) up-conversion luminescence agent WO3:Yb3+,Er3+The preparation of (1): mixing Na2WO4·2H2O、Yb2O3And Er2O3Dissolving in hot nitric acid, adding ethanol into the mixed solution, stirring for dissolving, transferring into high-pressure kettle, performing hydrothermal reaction for 24 hr, cleaning, centrifuging, drying, and annealing at 300 deg.C for 2.0 hr in air atmosphere to obtain WO3:Yb3+,Er3+；2）Ag3VO4The preparation of (1): mixing AgNO3Dissolving in a mixed solution of concentrated nitric acid and deionized water to obtain a solution A; reacting NH4VO3Ultrasonically dissolving the mixture in a mixed solution of NaOH and deionized water to obtain a solution B; mixing the solution A and the solution B, stirring for 30-40min, adjusting pH of the mixed solution to 10, stirring at 80 deg.C for 12h, centrifuging, washing, and drying to obtain Ag3VO4Powder;3）Ag/Ag3VO4preparation of Ag powder: mixing Ag3VO4Dissolving the powder in ethanol, ultrasonically dispersing for 10min, irradiating the obtained suspension with 300W xenon lamp, heating at 50 deg.C for 1.0h, and mixing with Ag+Reducing to Ag, centrifuging, washing, drying to obtain Ag/Ag3VO4Ag powder;4）WO3:Yb3+,Er3+/Ag/Ag3VO4preparation of Ag powder: mixing WO3:Yb3+,Er3+And Ag/Ag3VO4Adding Ag powder into deionized water, stirring and dispersing for 30-40min to obtain suspension; heating the obtained suspension to boiling point by magnetic stirring, keeping for 30min, centrifuging, collecting solid powder, washing with deionized water and ethanol, drying at 60 deg.C for 12 hr, and calcining in muffle furnace to obtain WO3:Yb3+,Er3+/Ag/Ag3VO4Ag powder.
- 2. Z-shaped WO as claimed in claim 13:Yb3+,Er3+/Ag/Ag3VO4The Ag photocatalyst is characterized in that in the step 1), the temperature of the hydrothermal reaction is 180 ℃.
- 3. Z-form WO of claim 13:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, characterized in that, in the step 1), the up-conversion luminescence agent WO3:Yb3+,Er3+In mole percent, 1 mol% of Yb3+And 1 mol% Er3+。
- 4. Z-form WO of claim 13:Yb3+,Er3+/Ag/Ag3VO4the/Ag photocatalyst is characterized in that in the solution A in the step 2), concentrated nitric acid and deionized water are in a ratio of 1:5 by volume; in the solution B, NaOH/deionized water =4.8g:30mL in a solid-to-liquid ratio.
- 5. Z-form WO of claim 13:Yb3+,Er3+/Ag/Ag3VO4the/Ag photocatalyst is characterized in that in the step 4), the material is calcined in a muffle furnace, the calcination temperature is 300 ℃, and the calcination time is 2.0 h.
- 6. WO type Z according to claim 13:Yb3+,Er3+/Ag/Ag3VO4The application of the/Ag photocatalyst in degrading antibiotics under sunlight.
- 7. Use according to claim 6, characterized in that: the method comprises the following steps: adding the Z-form WO of claim 1 to a solution containing an antibiotic3:Yb3+,Er3+/Ag/Ag3VO4Ag photocatalyst, irradiated under sunlight.
- 8. Use according to claim 6 or 7, wherein the antibiotic is levofloxacin.
- 9. WO type Z according to claim 13:Yb3+,Er3+/Ag/Ag3VO4The application of the/Ag photocatalyst in photocatalytic hydrogen production.
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