CN110975889A - Tungsten trioxide-molybdenum disulfide type composite photocatalyst and preparation method and application thereof - Google Patents
Tungsten trioxide-molybdenum disulfide type composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 73
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- -1 Tungsten trioxide-molybdenum disulfide Chemical compound 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 129
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 229910052961 molybdenite Inorganic materials 0.000 claims description 122
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 40
- 239000002096 quantum dot Substances 0.000 claims description 22
- 150000003657 tungsten Chemical class 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 19
- 239000002135 nanosheet Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000012266 salt solution Substances 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical group Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical class O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 abstract description 24
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 15
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 24
- 238000003756 stirring Methods 0.000 description 17
- 239000000243 solution Substances 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 229910016043 LixMoS2 Inorganic materials 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000009830 intercalation Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- ANUZKYYBDVLEEI-UHFFFAOYSA-N butane;hexane;lithium Chemical compound [Li]CCCC.CCCCCC ANUZKYYBDVLEEI-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229940087646 methanolamine Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
-
- 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
Abstract
The invention relates to the technical field of photocatalytic materials, in particular to a tungsten trioxide-molybdenum disulfide type composite photocatalyst and a preparation method and application thereof. The tungsten trioxide-molybdenum disulfide type composite photocatalyst provided by the invention comprises a molybdenum disulfide matrix and tungsten trioxide quantum dots loaded on the surface of the molybdenum disulfide matrix. In the invention, molybdenum disulfide and tungsten trioxide are both narrow-bandgap semiconductors, so that the photocatalyst can generate photo-generated electron-hole pairs under the excitation of visible light; the tungsten trioxide quantum dots can absorb visible light and generate photo-generated electrons, and the photo-generated electrons are loaded on the surface of the molybdenum disulfide matrix to form a heterostructure with molybdenum disulfide, so that the separation efficiency of current carriers is improved, the service life of the photo-generated electrons on a molybdenum disulfide valence band is prolonged, and the hydrogen production rate of water under visible light is further improved.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a tungsten trioxide-molybdenum disulfide type composite photocatalyst and a preparation method and application thereof.
Background
The photocatalytic water splitting to generate hydrogen is an ideal hydrogen production method, and the semiconductor absorbs light energy to generate electrons and holes so as to excite water splitting reaction, so that not only can hydrogen be obtained, but also no pollution gas is generated in the reaction process, and solar energy can be converted into chemical energy. The traditional semiconductor photocatalyst has the defects of poor photoresponse, poor stability, high recombination rate of photon-generated carriers and the like, so that the application of the traditional semiconductor photocatalyst in the field of photocatalysis is limited.
Disclosure of Invention
The invention aims to provide a tungsten trioxide-molybdenum disulfide type composite photocatalyst as well as a preparation method and application thereof. WO provided by the present invention3-MoS2The composite photocatalyst has good catalytic activity and stability under visible light, can greatly improve the utilization rate of the photocatalyst to solar energy and improve the efficiency of decomposing hydrogen in water, and the WO provided by the invention3-MoS2The preparation process of the composite photocatalyst is nontoxic, pollution-free and environment-friendly.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a tungsten trioxide-molybdenum disulfide type composite photocatalyst, which comprises MoS2A substrate and a carrier supported on the MoS2WO of the surface of a substrate3And (4) quantum dots.
Preferably, the MoS2The substrate is an ultrathin nanosheet with the thickness of 1-3 nm.
Preferably, said WO3The loading capacity of the quantum dots is 5-35%; said WO3The size of the quantum dots is 1-3 nm.
The invention provides a preparation method of the tungsten trioxide-molybdenum disulfide type composite photocatalyst, which comprises the following steps:
mixing sheet-like MoS2Dispersing in alcohol solvent to obtain MoS2A dispersion liquid;
dissolving a tungsten salt in a solvent to obtain a tungsten salt solution;
the MoS is treated2And mixing the dispersion liquid with the tungsten salt solution to perform oxidation reaction to obtain the tungsten trioxide-molybdenum disulfide type composite photocatalyst.
Preferably, the lamellar MoS2Composed of block-shaped MoS2Stripping to obtain; the tungsten salt is tungsten chloride, metal tungstate or ammonium metatungstate.
Preferably, the lamellar MoS2The molar ratio of the tungsten to tungsten in the tungsten salt is (3.5-24.5): 100. .
Preferably, the alcoholic solvent comprises ethylene glycol, ethanol or glycerol; the solvent is ethylene glycol or water.
Preferably, the temperature of the oxidation reaction is 120-160 ℃, and the time is 40-120 min.
Preferably, the oxidation reaction is carried out under the microwave-assisted condition, and the power of the microwave is 150-600W.
The invention also provides the application of the tungsten trioxide-molybdenum disulfide type composite photocatalyst prepared by the technical scheme or the tungsten trioxide-molybdenum disulfide type composite photocatalyst prepared by the preparation method of the technical scheme in hydrogen production through photocatalytic decomposition of water.
The invention provides tungsten trioxide-molybdenum disulfide (WO)3-MoS2) A composite photocatalyst comprising MoS2A substrate and a carrier supported on the MoS2WO of the surface of a substrate3And (4) quantum dots. In the present invention, MoS2And WO3The tungsten trioxide-molybdenum disulfide type composite photocatalyst is a narrow-bandgap semiconductor, so that a photo-generated electron-hole pair can be generated under the excitation of visible light; WO3Quantum dots are capable of absorbing visible light and producing photo-generated electrons,by loading it to the MoS2Surface of substrate with MoS2The heterostructure is formed, the separation efficiency of the current carrier is improved, and the MoS is prolonged2The life of photogenerated electrons on the valence band, and further the hydrogen rate of decomposing water under visible light is improved. WO provided by the present invention3-MoS2The composite photocatalyst has excellent light absorption capacity, better catalytic activity and stability under visible light, high-efficiency and stable activity of decomposing water to produce hydrogen, and can greatly improve the utilization rate of the photocatalyst to solar energy.
WO3-MoS provided by the invention2The preparation method of the composite photocatalyst has the advantages of simple process, easily obtained raw materials, mild operation conditions and lower production cost; and the preparation process is nontoxic, pollution-free and environment-friendly.
Drawings
FIG. 1 is a pure MoS2Nanosheet and WO provided by the invention3-MoS2A transmission electron microscope characterization comparison graph of the type composite photocatalyst;
FIG. 2 is a pure MoS2Nanosheet, blocky MoS2And WO provided by the present invention3-MoS2A powder X-ray diffraction representation diagram of the type composite photocatalyst;
FIG. 3 shows WO provided by the present invention3-MoS2A ultraviolet-visible absorption spectrum characterization diagram of the type composite photocatalyst;
FIG. 4 shows WO provided by the present invention3-MoS2The photolysis water hydrogen production activity diagram and the stability diagram of the composite photocatalyst.
Detailed Description
The invention provides a WO3-MoS2A composite photocatalyst comprising MoS2A substrate and a carrier supported on the MoS2WO of the surface of a substrate3And (4) quantum dots.
WO provided by the present invention3-MoS2The composite photocatalyst comprises MoS2A substrate. In the present invention, the MoS2The substrate is preferably an ultrathin nanosheet, and the thickness is preferably 1-3 nm. The invention adopts ultra-thin MoS2The nano sheet can improve MoS2Can uniformly disperse WO3Quantum dots, greatly improve WO3The utilization rate of the quantum dots; and the thickness of the atomic layer can reduce the transmission distance of the photo-generated electrons, so that the utilization rate of the photo-generated electrons is improved.
WO provided by the present invention3-MoS2The composite photocatalyst comprises the MoS supported on the surface of the substrate2WO of the surface of a substrate3And (4) quantum dots. In the present invention, the WO3The size of the quantum dots is preferably 1 to 3nm, and more preferably 1 to 2 nm. In the present invention, the WO3The loading amount of the quantum dots is preferably 5-35%, and more preferably 10%.
In the present invention, the WO3-MoS2The composite photocatalyst is MoS2Substrate and WO3Heterostructure formed by quantum dots and having chemical formula of MoS2WO3The expression is WO3-MoS2. In the present invention, the MoS2Substrate and WO3The quantum dots are narrow-band-gap semiconductors, stable in physical and chemical properties and MoS2Substrate and WO3The heterojunction is formed between the quantum dots, so that the separation efficiency of the photo-generated electron hole pair is improved, the service life of the photo-generated electron is prolonged, and the catalyst can have higher activity and stability for decomposing water to produce hydrogen under visible light.
The invention also provides the WO of the technical scheme3-MoS2The preparation method of the composite photocatalyst comprises the following steps:
mixing sheet-like MoS2Dispersing in alcohol solvent to obtain MoS2A dispersion liquid;
dissolving a tungsten salt in a solvent to obtain a tungsten salt solution;
the MoS is treated2And mixing the dispersion liquid with the tungsten salt solution to perform oxidation reaction to obtain the tungsten trioxide-molybdenum disulfide type composite photocatalyst.
The preparation method provided by the invention has the characteristics of simple process, low cost, no pollution and the like, and can be used for preparing the WO with controllable component content, high utilization rate of visible light, high efficiency and stability for photocatalytic water decomposition to produce hydrogen3-MoS2The composite photocatalyst is formed.
The invention relates to a sheet-like MoS2Dispersing in alcohol solvent to obtain MoS2And (3) dispersing the mixture.
In the present invention, the lamellar MoS2Preferably from bulk MoS2Exfoliation to obtain, more preferably, a bulk MoS by lithium intercalation2Peeled into flakes of MoS2The method comprises the following specific steps: mixing the block MoS2Mixing with n-butyl lithium hexane solution for intercalation reaction to obtain LixMoS2(ii) a The obtained LixMoS2Dispersing in water, and performing ultrasonic treatment to obtain lamellar MoS2。
In the present invention, the MoS2The amount ratio of n-butyllithium to n-butyllithium is preferably 0.5g:0.032mol to 4g:0.024mol, more preferably 2 g:0.032 mol; the concentration of the n-butyllithium hexane solution is preferably 0.6 to 3.6mol/L, and more preferably 1.6 mol/L. In the present invention, the mixing is preferably carried out under protective atmosphere conditions, more preferably an argon atmosphere; the mixing is preferably carried out under stirring, preferably at a speed of 600 r/min. In the present invention, the time for the intercalation reaction is preferably 48 hours. The invention can weaken the block MoS through the lithium ion intercalation2The interlaminar forces of (1). In the invention, after the intercalation reaction is finished, the obtained system is preferably centrifuged and washed by hexane to obtain LixMoS2. In the present invention, the LixMoS2X in (3) is preferably 2.2.
To obtain LixMoS2Thereafter, the present invention preferably uses the obtained LixMoS2Dispersing in water, and performing ultrasonic treatment to obtain lamellar MoS2. In the present invention, the power of the ultrasound is preferably 400W, and the time of ultrasound is preferably 12 h. The invention leads Li to be dispersed by ultrasonicxMoS2Decomposition to MoS2. After the ultrasonic dispersion is finished, the obtained system is preferably centrifuged at 2000r/min to remove un-peeled solid at the lower layer, then high-speed centrifugation is continuously carried out at 10000r/min, the obtained solid matter is washed to be neutral by water, and freeze drying is carried out to obtain flaky MoS2. In the present inventionSaid lamellar MoS2The thickness of (A) is preferably 1 to 3 nm.
The invention preferably treats the flake-like MoS under ultrasonic conditions2Dispersed in an alcoholic solvent, which in the present invention preferably comprises ethylene glycol, ethanol or glycerol, more preferably ethylene glycol; the MoS2The concentration of the dispersion is preferably 0.02g/50 mL-0.5 g/50mL, more preferably 0.1g/50 mL.
The invention dissolves tungsten salt in solvent to obtain tungsten salt solution. In the present invention, the tungsten salt is preferably tungsten chloride, metal tungstate or ammonium metatungstate; the metal tungstate is preferably M2WO4·2H2O, wherein M is preferably Na or K; the ammonium metatungstate is preferably (NH)4)6W7O24·6H2And O. The invention can realize the WO control by adjusting the types and the adding proportion of the tungsten salt3And regulating and controlling the content of the quantum dots. In the invention, the solvent is preferably ethylene glycol or water, and the concentration of the tungsten salt solution is preferably 0.5-5 g/L, and more preferably 1.2 g/L.
Obtaining MoS2After dispersing the solution and the tungsten salt solution, the invention mixes the MoS2Mixing the dispersion with the tungsten salt solution to perform oxidation reaction to obtain WO3-MoS2The composite photocatalyst is formed.
In the present invention, the lamellar MoS2The molar ratio of the tungsten to tungsten in the tungsten salt is preferably (3.5-24.5): 100, and more preferably 6.8: 100.
In the invention, the mixing is preferably carried out under stirring conditions, and the stirring speed is preferably 200-1200 r/min, and more preferably 600 r/min. The stirring time is not particularly limited in the present invention, and the stirring is carried out in the form of a flake MoS2And tungsten salt are mixed evenly.
In the invention, the temperature of the oxidation reaction is preferably 120-160 ℃, and more preferably 140-150 ℃; the time is preferably 40-120 min, and more preferably 80 min. In the oxidation reaction process, the tungsten salt is oxidized into the tungsten trioxide, and the tungsten trioxide fully grows on the molybdenum disulfide substrate to obtain the WO3-MoS2Composite photocatalystAn oxidizing agent.
In the invention, the oxidation reaction is preferably carried out under the microwave-assisted condition, and the power of the microwave is preferably 150-600W, and more preferably 300W. The invention adopts microwave to assist the oxidation reaction, can realize bulk heating, has more uniform heat transfer and reduces heat conduction.
In the invention, after the oxidation reaction is finished, the obtained system is preferably subjected to centrifugation, washing and drying in sequence to obtain WO3-MoS2The composite photocatalyst is formed. In the present invention, the washing detergent is preferably deionized water, and the number of washing is preferably 3. In the invention, the drying is preferably carried out under a vacuum condition, the drying temperature is preferably 70-85 ℃, and the drying time is preferably 2.5-4.5 h.
The invention also provides the WO of the technical scheme3-MoS2The composite photocatalyst or WO prepared by the preparation method of the technical scheme3-MoS2The application of the composite photocatalyst in photocatalytic water decomposition for hydrogen production. In the present invention, the WO is utilized3-MoS2The method for preparing the hydrogen by the composite photocatalyst is preferably as follows: mixing WO3-MoS2Dispersing the type composite photocatalyst in a mixed solution of water and a sacrificial agent, and then irradiating under a 300W xenon lamp with a 420nm optical filter (lambda is more than or equal to 420 nm); wherein, the sacrificial agent is preferably methanol or triethanolamine; the volume ratio of the sacrificial agent to water is preferably 1 (4-9); said WO3-MoS2The dosage ratio of the mixed liquid of the type composite photocatalyst, water and the sacrificial agent is preferably 1 mg: (10-20) mL; the irradiation time is preferably 3 h.
WO provided by the present invention3-MoS2The composite photocatalyst synthesizes MoS2And WO3The photocatalyst has the characteristics of strong photoresponse capability and stable physicochemical properties, and the combination of the two enables the photocatalyst to have a proper energy band structure and to carry out a photolysis hydrogen production reaction under the drive of visible light; meanwhile, the two are compounded to form a heterostructure, so that the separation of a photon-generated carrier is promoted, the service life of photon-generated electrons is prolonged, and the hydrogen production rate of photolysis is improved.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) 2g of block MoS is taken2Placing in a sealed flat-bottom flask protected by argon, slowly adding 20mL of n-butyllithium hexane solution with the concentration of 1.6mol/L by using a syringe, stirring for 48h, centrifuging, and washing with hexane to obtain Li2.2MoS2(ii) a Subjecting the Li to2.2MoS2Ultrasonically dispersing in water, ultrasonically treating for 12h under 260W ultrasonic power, centrifuging at 2000r/min until the lower layer is not stripped of solid, centrifuging at 10000r/min, removing the lower layer of solid, washing with water to neutrality, and freeze drying to obtain 1-3 nm thick sheet MoS2；
(2) 0.15g of the flaky MoS obtained in step (1) was taken2Ultrasonically dispersing into 50mL of ethylene glycol, dissolving 32.60mg of tungsten chloride into 20mL of ethylene glycol, fully stirring, and then carrying out MoS2Mixing the dispersion with tungsten chloride glycol solution, stirring, transferring into a bottle shaped like a eggplant, reacting at 160 deg.C for 40min under the assistance of 300W microwave to obtain black solid, centrifuging, washing with water for 3 times, and vacuum drying at 40 deg.C to obtain WO3-MoS2The composite photocatalyst is formed.
Weighing 1mg of the obtained WO3-MoS2Ultrasonically dispersing the composite photocatalyst into a quartz tube filled with 10mL of methanol water solution, wherein the volume ratio of methanol to water is 1: 4; introducing argon into the quartz tube under the stirring condition so as to achieve the aim of exhausting air; irradiating with a 300W xenon lamp with a 420nm filter (λ ≥ 420nm) for 3 hr, and measuring H by gas chromatography2And calculating to obtain the hydrogen production rate of the photocatalyst to be 380 mu mol/h/g.
Example 2
(1) Get2g of MoS Block2Placing in a sealed flat-bottom flask protected by argon, slowly adding 20mL of n-butyllithium hexane solution with the concentration of 1.6mol/L by using a syringe, stirring for 48h, centrifuging, and washing with hexane to obtain Li2.2MoS2(ii) a Subjecting the Li to2.2MoS2Ultrasonically dispersing in water, ultrasonically treating for 12h under 260W ultrasonic power, centrifuging at 2000r/min to remove upper layer solid, centrifuging at 10000r/min to remove lower layer solid, washing with water to neutrality, and freeze drying to obtain 1-3 nm thick sheet MoS2；
(2) 0.4g of the flaky MoS obtained in step (1) was taken2Ultrasonically dispersing into 50mL of ethylene glycol, dissolving 10.8mg of ammonium metatungstate in 20mL of water, and fully stirring to obtain the MoS2Mixing the dispersion with ammonium metatungstate water solution, stirring, transferring into eggplant-shaped bottle, reacting at 120 deg.C for 80min under the assistance of 300W microwave to obtain black solid, centrifuging, washing with water for 3 times, and vacuum drying at 40 deg.C to obtain WO3-MoS2Forming a composite photocatalyst;
(3) weighing 1mg of the obtained WO3-MoS2Ultrasonically dispersing the composite photocatalyst into a quartz tube filled with 10mL of triethanolamine aqueous solution, wherein the volume ratio of triethanolamine to water is 1: 4; introducing argon into the quartz tube under the stirring condition so as to achieve the aim of exhausting air; irradiating with a 300W xenon lamp with a 420nm filter (λ ≥ 420nm) for 3 hr, and measuring H by gas chromatography2Calculating the hydrogen production rate of the photocatalyst; and repeatedly measuring the hydrogen production rate of the photocatalyst, comparing whether the rate changes or not, and further evaluating the stability of the photocatalyst.
Example 3
(1) 2g of block MoS is taken2Placing in a sealed flat-bottom flask protected by argon, slowly adding 20mL of n-butyllithium hexane solution with the concentration of 1.6mol/L by using a syringe, stirring for 48h, centrifuging, and washing with hexane to obtain Li2.2MoS2(ii) a Subjecting the Li to2.2MoS2Ultrasonically dispersing in water, ultrasonically treating at 260W ultrasonic power for 12 hr, centrifuging at 2000r/min to remove upper solid layerCentrifuging at 10000r/min, removing lower layer solid, washing with water to neutrality, and freeze drying to obtain 1-3 nm thick sheet MoS2；
(2) 0.15g of the flaky MoS obtained in step (1) was taken2Ultrasonically dispersing into 50mL of ethylene glycol, dissolving 41mg of sodium tungstate into 20mL of ethylene glycol, fully stirring, and then carrying out MoS2Mixing the dispersion with sodium tungstate glycol solution, stirring, transferring into a eggplant-shaped bottle, reacting at 120 deg.C for 120min under the assistance of 300W microwave to obtain black solid, centrifuging, washing with water for 3 times, and vacuum drying at 40 deg.C to obtain WO3-MoS2Forming a composite photocatalyst;
(3) weighing 1mg of the obtained WO3-MoS2Ultrasonically dispersing the composite photocatalyst into a quartz tube filled with 20mL of methanol water solution, wherein the volume ratio of methanol to water is 1: 9; introducing argon into the quartz tube under the stirring condition so as to achieve the aim of exhausting air; irradiating with a 300W xenon lamp with a 420nm filter (λ ≥ 420nm) for 3 hr, and measuring H by gas chromatography2The hydrogen production rate of the photocatalyst is calculated to be 280 mu mol/h/g.
Characterization and Performance test results
FIG. 1 pure MoS2Nanosheet and WO obtained in examples 1 and 23-MoS2Transmission Electron Micrograph (TEM) of composite photocatalyst of type (I), wherein A in FIG. 1 is pure MoS2Transmission electron microscope image of nano-sheet, the inset in A is pure MoS2Atomic Force Microscopy (AFM) of the nanoplatelets; b in FIG. 1 is pure MoS2Transmission electron microscopy images of the nanosheets; from A and B in FIG. 1, pure MoS can be seen2The nano sheet is of a two-dimensional layered structure, the surface of the nano sheet is smooth, the size of the nano sheet is 0.2 multiplied by 0.2 mu m, and the thickness of the nano sheet is 1 nm; in FIG. 1, C is WO obtained in example 13-MoS2A transmission electron microscope image of the type composite photocatalyst; d in FIG. 1 is WO obtained in example 23-MoS2A transmission electron microscope image of the type composite photocatalyst; WO can be seen from C and D in FIG. 13The quantum dots are uniformly distributed on the MoS2And a good heterostructure is formed on the surface.
FIG. 2 shows WO obtained in example 23-MoS2A powder X-ray diffraction (PXRD) pattern of the type composite photocatalyst; wherein bulk-MoS2Representing a Block MoS2；WO3-MoS2WO prepared in example 2 is shown3-MoS2Forming a composite photocatalyst; MoS2NSs represents pure MoS2Nanosheets. As can be seen in FIG. 2, the massive MoS2After stripping, only 5 diffraction peaks are left, particularly the intensity of the (002) crystal face diffraction peak is greatly reduced, which indicates that the massive MoS is2Successful exfoliation, WO3-MoS2PXRD of type composite photocatalyst does not see WO3Diffraction peaks of quantum dots due to WO3The quantum dot size is too small.
FIG. 3 shows WO obtained in example 23-MoS2The ultraviolet visible absorption spectrogram of the composite photocatalyst can be seen from the figure, and the prepared WO can be seen from the figure3-MoS2The composite photocatalyst has good absorptivity in a visible light region, is mainly concentrated at 500-700 nm, has a maximum absorption peak at about 600nm, and can generate a photon-generated carrier under visible light.
FIG. 4 shows WO prepared in example 23-MoS2The water decomposition hydrogen production activity diagram and the stability test diagram of the composite photocatalyst are shown; wherein A in FIG. 4 is pure MoS2Nanosheets and WO3-MoS2Comparing the hydrogen production activity of the obtained product; b in FIG. 4 is WO3-MoS2The hydrogen production activity diagram of the composite photocatalyst is obtained by 4 times of circulation; from the figure, pure MoS can be seen2The nano-sheet has no H under the irradiation of visible light2Is generated due to pure MoS2The recombination rate of photogenerated carriers of the nanosheets is high; relative to pure MoS2Nanosheets, WO3-MoS2The rate of hydrogen generation by photocatalytic decomposition of the compound photocatalyst is greatly improved, the stability is good, and the rate is almost unchanged after 4 cycles.
The invention leads the block MoS to be2Exfoliated into flake-like MoS of only 2 atomic layers thick2And applying the thin-sheet MoS by microwave method2Thereon grow WO3The quantum dots form a heterostructure.The photocatalyst prepared by the method has the advantages that the thickness is thin, the transmission of a photon-generated carrier can be promoted, the separation efficiency of photon-generated electron holes is improved by the heterostructure, the photocatalytic activity is improved, the heterostructure synthesized by the method has mild operation conditions, the raw materials are easy to obtain, the process is simple, the reaction process is clean and pollution-free, and the like.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The tungsten trioxide-molybdenum disulfide type composite photocatalyst is characterized by comprising MoS2A substrate and a carrier supported on the MoS2WO of the surface of a substrate3And (4) quantum dots.
2. The tungsten trioxide-molybdenum disulfide type composite photocatalyst according to claim 1, wherein said MoS is2The substrate is an ultrathin nanosheet with the thickness of 1-3 nm.
3. The tungsten trioxide-molybdenum disulfide type composite photocatalyst as claimed in claim 1, wherein said WO is3The loading capacity of the quantum dots is 5-35%; said WO3The size of the quantum dots is 1-3 nm.
4. The method for preparing the tungsten trioxide-molybdenum disulfide type composite photocatalyst as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
mixing sheet-like MoS2Dispersing in alcohol solvent to obtain MoS2A dispersion liquid;
dissolving a tungsten salt in a solvent to obtain a tungsten salt solution;
the MoS is treated2And mixing the dispersion liquid with the tungsten salt solution to perform oxidation reaction to obtain the tungsten trioxide-molybdenum disulfide type composite photocatalyst.
5. The method for preparing according to claim 4, wherein the flaky MoS2Composed of block-shaped MoS2Stripping to obtain; the tungsten salt is tungsten chloride, metal tungstate or ammonium metatungstate.
6. The method for preparing according to claim 4 or 5, wherein the flaky MoS2The molar ratio of the tungsten to tungsten in the tungsten salt is (3.5-24.5): 100.
7. The method of claim 4, wherein the alcoholic solvent comprises ethylene glycol, ethanol or glycerol; the solvent is ethylene glycol or water.
8. The method according to claim 4, wherein the temperature of the oxidation reaction is 120 to 160 ℃ and the time is 40 to 120 min.
9. The preparation method according to claim 4 or 8, wherein the oxidation reaction is carried out under the microwave-assisted condition, and the power of the microwave is 150-600W.
10. The application of the tungsten trioxide-molybdenum disulfide type composite photocatalyst as set forth in any one of claims 1 to 3 or the tungsten trioxide-molybdenum disulfide type composite photocatalyst prepared by the preparation method as set forth in any one of claims 4 to 9 in hydrogen production through photocatalytic decomposition of water.
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