CN113952964A - Preparation method and application of molybdenum disulfide/indium oxide nanocomposite material with 2D/3D structure - Google Patents
Preparation method and application of molybdenum disulfide/indium oxide nanocomposite material with 2D/3D structure Download PDFInfo
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- CN113952964A CN113952964A CN202111221907.7A CN202111221907A CN113952964A CN 113952964 A CN113952964 A CN 113952964A CN 202111221907 A CN202111221907 A CN 202111221907A CN 113952964 A CN113952964 A CN 113952964A
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 62
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 230000001699 photocatalysis Effects 0.000 claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 21
- 239000004202 carbamide Substances 0.000 claims description 21
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims description 11
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 4
- 229910052961 molybdenite Inorganic materials 0.000 abstract description 36
- 239000002135 nanosheet Substances 0.000 abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000008878 coupling Effects 0.000 abstract description 6
- 238000010168 coupling process Methods 0.000 abstract description 6
- 238000005859 coupling reaction Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 239000003403 water pollutant Substances 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/10—Photocatalysts
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Abstract
The invention relates to a preparation method and application of a molybdenum disulfide/indium oxide nano composite material with a 2D/3D structure2O3Nanocubes, followed by simple hydrothermal method of 2D structured MoS2Nanosheet loading In2O3Nano cubic surface, low cost and high catalytic activityActive 2D/3D structure MoS2/In2O3A nanocomposite material. By using In2O3Characteristics of material energy band structure and MoS2The material can accelerate the advantage of photoproduction electron-hole separation/migration rate, and the constructed MoS2/In2O3The nano composite material can be used for the reaction of coupling photocatalytic degradation of rhodamine B for efficiently decomposing water by photocatalysis to prepare hydrogen. The raw materials of the invention have the advantages of low price, simple preparation and the like, reduce energy consumption and reaction cost, are convenient for batch production, are nontoxic and harmless, and meet the requirements of energy conservation, environmental protection and sustainable development.
Description
Technical Field
The invention belongs to the technical field of nano material synthesis, and provides a method for synthesizing molybdenum disulfide (MoS) with a 2D/3D structure by using a simple hydrothermal method2) Indium oxide (In)2O3) The nano composite material can be used for coupling photocatalytic degradation of rhodamine B by efficiently decomposing water to produce hydrogen by photocatalysis.
Background
The global energy crisis and environmental pollution are two major problems facing the world today. At present, the photocatalysis technology has the advantages of energy conservation, cleanness, no pollution and the like, and is widely concerned about solving the energy and environmental problems. In the process of preparing hydrogen by decomposing water through photocatalysis, sacrificial agents such as methanol, triethanolamine, lactic acid and the like are added to accelerate the consumption of photoproduction holes, so that photoproduction electrons efficiently participate in hydrogen preparation reaction. However, these non-renewable sacrificial agents are important chemical raw materials, and the photocatalytic hydrogen production reaction using them as sacrificial agents does not meet the requirement of sustainable development. On the other hand, organic dye wastewater represented by rhodamine B poses serious hazards to ecosystem and human health. Therefore, if photocatalytic hydrogen production and photocatalytic degradation of rhodamine B can be carried out in one photocatalytic system, the energy and environmental problems caused by social development are probably solved.
Indium oxide (In)2O3) The material is a typical n-type semiconductor material, has the band gap energy of about 2.8eV, and has the advantages of excellent photochemical stability, proper light absorption, no toxicity, no harm and the like, so the material is widely applied to reactions such as photocatalytic water splitting hydrogen production, photocatalytic organic pollutant degradation, photocatalytic carbon dioxide reduction and the like. However, due to the slow separation and migration rate of photo-generated electrons-holes, single In2O3Materials typically exhibit low photocatalytic activity in photocatalytic reactions. Molybdenum disulfide (MoS)2) The transition metal dihalide compound with a two-dimensional structure similar to graphene is a cocatalyst capable of replacing noble metal and has attracted great attention in photocatalytic reaction. For example: MoS2With TiO2The photocatalytic hydrogen production performance can be remarkably improved by constructing the composite material; MoS2And Cu2The O-structured composite material can obviously accelerate the performance of photocatalytic degradation of dye. However, currently 2D/3D structured MoS2/In2O3The construction of the nano composite material and related research on the photocatalytic degradation of rhodamine B by coupling photocatalytic decomposition of water for hydrogen production have not been reported.
Disclosure of Invention
The invention aims to provide a MoS with a 2D/3D structure2/In2O3Preparation method of nano composite material and 2D/3D structure MoS2/In2O3The nano composite material is used for photocatalytic decomposition of water to prepare hydrogen and coupling photocatalytic degradation of rhodamine B reaction. The MoS2/In2O3The nano composite material has high catalytic activity, and can realize the purpose of removing water pollutants while preparing hydrogen.
Technical scheme of the invention
2D/3D structure MoS2/In2O3The preparation method of the nano composite material comprises the following steps:
step 1: weighing a certain amount of indium acetate and urea, respectively placing the indium acetate and the urea in 15mL and 20mL of distilled water, stirring at room temperature to completely dissolve the indium acetate and the urea, and dropwise adding the urea solution into the indium acetate solution by using a suction tube to form uniform mixed solution.
The molar weight ratio of the indium acetate to the urea is 1: 12.8.
Step 2: transferring the mixed solution into a high-pressure autoclave with a certain volume and a polytetrafluoroethylene lining, heating for a certain time at a certain temperature, carrying out hydrothermal reaction, cooling the high-pressure autoclave to room temperature, centrifuging to collect a white product, washing for 3 times by using distilled water and ethanol respectively, and drying in an oven at 80 ℃ to obtain a precursor.
The volume of the autoclave is 50 mL; the hydrothermal reaction temperature is 130 ℃ and the time is 12 h.
And step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling a certain heating rate to carry out heating reaction, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
The heating rate is 2 ℃/min; the heating reaction temperature is 600 ℃, and the time is 2 h.
And 4, step 4: weighing a certain amount of In2O3Ultrasonically dispersing the mixture in distilled water of certain volume, adding certain amount of sodium molybdate and thioacetamide, ultrasonically stirring until the materials are completely dispersed to form uniform suspension.
Said In2O3The mass is 300 mg; the molar ratio of sodium molybdate to thioacetamide was 1: 5.
And 5: completely transferring the suspension into a polytetrafluoroethylene-lined high-pressure autoclave with a certain volume, heating for a certain time at a certain temperature, carrying out hydrothermal reaction, cooling the high-pressure autoclave to room temperature, centrifugally collecting a sample, washing with distilled water and ethanol for 3 times, drying in an oven at 80 ℃, and finally obtaining MoS with a 2D/3D structure2/In2O3A nanocomposite material.
The volume of the autoclave is 50 mL; the hydrothermal reaction temperature is 210 ℃ and the time is 24 h.
The invention has the advantages of
1. The present invention utilizes the MoS of a 2D layered structure2The nanosheet material can effectively accelerate the advantage of photoproduction electron-hole separation/migration rate to replace the traditional noble metal Pt-based cocatalyst, so that the cheap and high-catalytic-activity 2D/3D structure MoS is successfully constructed2/In2O3A nanocomposite material.
2. The present invention utilizes In2O3The material has the characteristics of an energy band structure (electrons generated by a conduction band can reduce water to prepare hydrogen and holes generated by a valence band can oxidize pollutants), and the photocatalytic water decomposition hydrogen preparation reaction and the photocatalytic rhodamine B degradation reaction are cooperatively coupled, so that the aim of removing water pollutants while preparing hydrogen is fulfilled.
3. The raw materials of the invention have the advantages of low price, simple preparation and the like, reduce energy consumption and reaction cost, are convenient for batch production, are nontoxic and harmless, and meet the requirements of energy conservation, environmental protection and sustainable development.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
FIG. 1A shows In prepared In example 1 of the present invention2O3X-ray diffraction pattern (XRD) of the nanocubes.
FIG. 1B is a MoS prepared according to example 2 of the present invention2XRD pattern of nanoplatelets.
FIG. 1C is a representation of the MoS prepared in examples 3-6 of the present invention2/In2O3XRD pattern of the nanocomposite.
FIG. 2A shows In prepared In example 1 of the present invention2O3Scanning Electron Microscope (SEM) images of nanocubes.
FIG. 2B is a MoS prepared according to example 2 of the present invention2Transmission Electron Microscope (TEM) images of the nanoplatelets.
FIGS. 2C and 2D are 10% MoS prepared according to example 5 of the present invention2/In2O3TEM images of the nanocomposites.
FIG. 3A shows In prepared In examples 1 and 5 of the present invention2O3Nanocubes and 10% MoS2/In2O3Photo-amperometric pattern of the nanocomposite.
FIG. 3B shows In prepared In examples 1 and 5 of the present invention2O3Nanocubes and 10% MoS2/In2O3Electrochemical impedance plot of the nanocomposite.
FIG. 4A shows In prepared In examples 1 and 3 to 6 of the present invention2O3Nanocubes and MoS2/In2O3The hydrogen rate histogram of the photocatalytic decomposition water of the nanocomposite.
FIG. 4B shows In prepared In examples 1 and 3 to 6 of the present invention2O3Nanocubes and MoS2/In2O3A histogram of the total organic carbon removal rate of the photocatalytic degradation rhodamine B of the nanocomposite.
With the above figures, certain embodiments of the invention have been illustrated and described in more detail below. The drawings and the description are not intended to limit the scope of the inventive concept in any way, but rather to illustrate it by those skilled in the art with reference to specific embodiments.
Detailed Description
The invention aims to provide a MoS with a 2D/3D structure2/In2O3The method for preparing the nano composite material uses the synthesized nano composite material as a catalyst for the reaction of coupling photocatalytic degradation of rhodamine B for hydrogen production by high-efficiency photocatalytic decomposition of water. The method uses indium acetate, urea, thioacetamide and sodium molybdate as raw materials to prepare In with a 3D structure by a hydrothermal-calcination method2O3Nanocubes, followed by simple hydrothermal method of 2D structured MoS2Nanosheet loading In2O3Constructing MoS with 2D/3D structure on surface of nano cube2/In2O3A nanocomposite material.
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1: preparation of In2O3Nano cube
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, the solution is stirred for 15min at room temperature to be completely dissolved, and then the urea solution is dropwise added into the indium acetate solution by a suction tube to form uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 130 ℃, cooling the autoclave to room temperature, centrifuging to collect a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
And step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling the heating rate to be 2 ℃/min, heating and reacting at 600 ℃ for 2h, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
Example 2: preparation of MoS2Nano-sheet
Step 1: 0.3088g of sodium molybdate and 0.5635g of thioacetamide are weighed and placed in 35mL of distilled water, and the sodium molybdate and the thioacetamide are completely dispersed by ultrasonic and stirring for 30min at room temperature to form a uniform suspension.
Step 2: transferring the suspension into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 210 ℃ for 24h, cooling the autoclave to room temperature, centrifuging to collect a black product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain MoS with a 2D structure2Nanosheets.
Example 3: preparation of 5% MoS2/In2O3Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, the solution is stirred for 15min at room temperature to be completely dissolved, and then the urea solution is dropwise added into the indium acetate solution by a suction tube to form uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 130 ℃, cooling the autoclave to room temperature, centrifuging to collect a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
And step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling the heating rate to be 2 ℃/min, heating and reacting at 600 ℃ for 2h, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
And 4, step 4: weighing 300mg of In2O3Ultrasonically dispersing the mixture in 35mL of distilled water, then adding 0.0193g of sodium molybdate and 0.0352g of thioacetamide, and ultrasonically stirring the mixture until the materials are completely dispersed to form uniform suspension.
Step (ii) of5: completely transferring the suspension into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 210 ℃ for 24h, cooling the autoclave to room temperature, centrifuging to collect the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 5% MoS2/In2O3A nanocomposite material.
Example 4: preparation of 7.5% MoS2/In2O3Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, the solution is stirred for 15min at room temperature to be completely dissolved, and then the urea solution is dropwise added into the indium acetate solution by a suction tube to form uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 130 ℃, cooling the autoclave to room temperature, centrifuging to collect a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
And step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling the heating rate to be 2 ℃/min, heating and reacting at 600 ℃ for 2h, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
And 4, step 4: weighing 300mg of In2O3Ultrasonic dispersion in 35mL distilled water, then adding 0.0289g sodium molybdate and 0.0528g thioacetamide, ultrasonic stirring until the material is completely dispersed, forming a uniform suspension.
And 5: completely transferring the suspension into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 210 ℃ for 24h, cooling the autoclave to room temperature, centrifuging to collect the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 7.5% MoS2/In2O3A nanocomposite material.
Example 5: preparation of 10% MoS2/In2O3Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, the solution is stirred for 15min at room temperature to be completely dissolved, and then the urea solution is dropwise added into the indium acetate solution by a suction tube to form uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 130 ℃, cooling the autoclave to room temperature, centrifuging to collect a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
And step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling the heating rate to be 2 ℃/min, heating and reacting at 600 ℃ for 2h, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
And 4, step 4: weighing 300mg of In2O3Ultrasonically dispersing the mixture in 35mL of distilled water, then adding 0.0386g of sodium molybdate and 0.0704g of thioacetamide, and ultrasonically stirring the mixture until the materials are completely dispersed to form a uniform suspension.
And 5: completely transferring the suspension into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 210 ℃ for 24h, cooling the autoclave to room temperature, centrifuging to collect the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 10% MoS2/In2O3A nanocomposite material.
Example 6: preparation of 12.5% MoS2/In2O3Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, the solution is stirred for 15min at room temperature to be completely dissolved, and then the urea solution is dropwise added into the indium acetate solution by a suction tube to form uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 130 ℃, cooling the autoclave to room temperature, centrifuging to collect a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
And step 3: placing the precursor in a muffle furnace at room temperature, and adjustingControlling the heating rate to be 2 ℃/min, heating and reacting for 2h at 600 ℃, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube.
And 4, step 4: weighing 300mg of In2O3Ultrasonically dispersing the mixture in 35mL of distilled water, then adding 0.0483g of sodium molybdate and 0.0880g of thioacetamide, and ultrasonically stirring the mixture until the materials are completely dispersed to form a uniform suspension.
And 5: completely transferring the suspension into a 50mL autoclave with a polytetrafluoroethylene lining, carrying out hydrothermal reaction at 210 ℃ for 24h, cooling the autoclave to room temperature, centrifuging to collect the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 12.5% MoS2/In2O3A nanocomposite material.
The crystal phase structure of the catalyst in the present invention was determined by X-ray diffraction (XRD). The XRD patterns of fig. 1A, 1B and 1C can be seen: in2O3Nanocubes and MoS2The characteristic diffraction peaks of the nanosheet material are consistent with the JCPDS No.71-2194 and JCPDS No.37-1492 of the standard card, indicating that the pure phase In2O3And MoS2Have all been successfully prepared; in MoS2/In2O3In the nano composite material, since MoS2The loading content is relatively low, and all nanocomposites exhibit In2O3Characteristic XRD diffraction peak of (1), MoS is not observed2Characteristic peak of (2).
The surface morphology and microstructure of the catalyst in the present invention were determined by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The SEM image of fig. 2A can see that: prepared pure phase In2O3The material has a distinct 3D cubic structure; the TEM image of fig. 2B can be seen: prepared pure phase MoS2The material has an obvious 2D nanosheet structure; the TEM images of fig. 2C and 2D can be seen: MoS when the mass ratio is 10%2Loaded In2O3After surfacing, 10% MoS prepared2/In2O3The nanocomposite still showed In phase with pure In2O3Similar nanocube structure, butMoS with two-dimensional layered structure uniformly distributed on surface2Nanosheets. This result indicates a unique 2D/3D structure of MoS2/In2O3Nanocomposites have been successfully synthesized.
The photo-generated electron-hole separation/transfer rate of the catalyst of the present invention is determined by the photocurrent response and the electrochemical impedance. The photocurrent response graph of fig. 3A can be seen: with pure phase In2O3Material comparison, 10% MoS prepared2/In2O3The nano composite material has obviously improved photocurrent density; the electrochemical impedance plot of fig. 3B can be seen: with pure phase In2O3Material comparison, 10% MoS prepared2/In2O3The nanocomposite material has a significantly reduced impedance semicircle. This result indicates MoS2In can be greatly increased as a cocatalyst2O3The photogenerated electron-hole separation/transport rate of the material.
The photocatalytic performance of the catalyst is determined by photocatalytic decomposition of water to produce hydrogen and coupling photocatalytic rhodamine B reduction. The hydrogen production rate histogram of fig. 4A can be seen: pure phase In2O3The material shows very low photocatalytic hydrogen production activity, and the prepared MoS2/In2O3The nano composite material can obviously improve the activity of photocatalytic hydrogen production. Wherein, 10% MoS2/In2O3The nanocomposite exhibited the highest hydrogen production activity (15.5. mu. mol/g/h) In comparison to the pure phase2O3The material is 77.5 times higher. The rhodamine B total organic carbon removal rate histogram of fig. 4B can be seen: pure phase In2O3The material has the lowest total organic carbon removal rate, and the synthesized MoS2/In2O3The total organic carbon removal rate of the nano composite material is greatly improved. Wherein, 10% MoS2/In2O3The nanocomposite had the highest total organic carbon removal (63.1%) and was about pure phase In2O312 times the material. In addition, as can be seen from fig. 4A and 4B, the hydrogen production rate of the catalyst is in direct proportion to the total organic carbon removal rate of rhodamine B. This result indicates thatPrepared MoS2/In2O3The nano composite material can obviously improve the reaction of photocatalytic water splitting for hydrogen production and also can obviously accelerate the degradation and mineralization processes of rhodamine B molecules.
Claims (7)
1. A preparation method of a 2D/3D structure molybdenum disulfide/indium oxide nano composite material is characterized by comprising the following steps: the method comprises the following steps:
step 1: weighing a certain amount of indium acetate and urea, respectively placing the indium acetate and the urea in 15mL and 20mL of distilled water, stirring at room temperature to completely dissolve the indium acetate and the urea, and dropwise adding the urea solution into the indium acetate solution by using a suction tube to form uniform mixed solution;
step 2: transferring the mixed solution into a high-pressure autoclave with a certain volume and a polytetrafluoroethylene lining, heating for a certain time at a certain temperature, carrying out hydrothermal reaction, cooling the high-pressure autoclave to room temperature, centrifuging to collect a white product, washing for 3 times by using distilled water and ethanol respectively, and drying in an oven at 80 ℃ to obtain a precursor;
and step 3: placing the precursor In a muffle furnace at room temperature, regulating and controlling a certain heating rate to carry out heating reaction, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature2O3A nanocube;
and 4, step 4: weighing a certain amount of In2O3Ultrasonically dispersing the mixture in distilled water with a certain volume, adding a certain amount of sodium molybdate and thioacetamide, and ultrasonically stirring the mixture until the materials are completely dispersed to form uniform suspension;
and 5: completely transferring the suspension into a polytetrafluoroethylene-lined high-pressure autoclave with a certain volume, heating for a certain time at a certain temperature, carrying out hydrothermal reaction, cooling the high-pressure autoclave to room temperature, centrifugally collecting a sample, washing with distilled water and ethanol for 3 times, drying in an oven at 80 ℃, and finally obtaining MoS with a 2D/3D structure2/In2O3A nanocomposite material.
2. The method for preparing the molybdenum disulfide/indium oxide nanocomposite material with the 2D/3D structure according to claim 1, wherein the method comprises the following steps: the molar weight ratio of the indium acetate to the urea in the step 1 is 1: 12.8.
3. The method for preparing the molybdenum disulfide/indium oxide nanocomposite material with the 2D/3D structure according to claim 1, wherein the method comprises the following steps: the volume of the autoclave in the step 2 is 50 mL; the hydrothermal reaction temperature is 130 ℃ and the time is 12 h.
4. The method for preparing the molybdenum disulfide/indium oxide nanocomposite material with the 2D/3D structure according to claim 1, wherein the method comprises the following steps: the heating rate in the step 3 is 2 ℃/min; the heating reaction temperature is 600 ℃, and the time is 2 h.
5. The method for preparing the molybdenum disulfide/indium oxide nanocomposite material with the 2D/3D structure according to claim 1, wherein the method comprises the following steps: in said step 42O3The mass is 300 mg; the molar ratio of sodium molybdate to thioacetamide was 1: 5.
6. The method for preparing the molybdenum disulfide/indium oxide nanocomposite material with the 2D/3D structure according to claim 1, wherein the method comprises the following steps: the volume of the autoclave in the step 5 is 50 mL; the hydrothermal reaction temperature is 210 ℃ and the time is 24 h.
7. The preparation method of any one of the molybdenum disulfide/indium oxide nanocomposite materials with a 2D/3D structure as claimed in claims 1-6, which is used as a catalyst for efficient photocatalytic decomposition of water for hydrogen production coupled with rhodamine B degradation reaction.
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