CN110560093A - Two-dimensional MoS2Preparation method of Cu-loaded photocatalyst - Google Patents
Two-dimensional MoS2Preparation method of Cu-loaded photocatalyst Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 14
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 70
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 63
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 29
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 30
- 239000001257 hydrogen Substances 0.000 abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 30
- 230000001699 photocatalysis Effects 0.000 abstract description 30
- 238000004519 manufacturing process Methods 0.000 abstract description 22
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 5
- 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 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000004729 solvothermal method Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
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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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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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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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- C—CHEMISTRY; METALLURGY
- 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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- 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
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- 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
- C01B2203/1076—Copper or zinc-based catalysts
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- 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
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Abstract
The invention relates to a two-dimensional MoS2Method for preparing Cu-loaded photocatalyst by two-dimensional MoS2The Cu is loaded, so that the nano material with high catalytic performance is prepared, the photocatalytic hydrogen production performance and activity are high, the nano material has good environmental protection performance, and the environment is not polluted and the user is not hurt in the synthesis and photocatalytic processes.
Description
Technical Field
The invention relates to a two-dimensional MoS2A preparation method of a Cu-loaded photocatalyst belongs to the technical field of photocatalytic materials.
Background
MoS2As a typical layered transition metal sulfurThe compound has been widely applied in the fields of light conversion, photocatalysis and the like, and has great prospect for degrading organic pollutants and preparing energy hydrogen. MoS2The structure of the edge of (1) is relatively complex, sulfur has high unsaturation, and the activity of the reaction is extremely high, so that the attention and the research on the sulfur are widely drawn.
At present, most of catalysts widely used for degrading environmental pollutants in the field of photocatalysis are N-type semiconductor materials of metal oxides, particularly titanium dioxide, although titanium dioxide is cheap and nontoxic, the titanium dioxide can only absorb ultraviolet range of sunlight due to the forbidden band width of more than 3eV, the absorptivity of the titanium dioxide to the sunlight is 3% -5%, and the utilization rate of the titanium dioxide to the sunlight is seriously influenced. The band gap width of the molybdenum disulfide is about 1.29eV, the molybdenum disulfide can well absorb visible light of sunlight, the chemical property of the molybdenum disulfide is stable, and the molybdenum disulfide is not easy to react with other substances at normal temperature, so that the molybdenum disulfide has great research significance and application potential in the field of photocatalysis. Molybdenum disulfide has a huge specific surface area, is porous, is unsaturated, and is easy to combine with other atoms, so that the molybdenum disulfide is a hot spot for researching photocatalytic semiconductors.
Disclosure of Invention
The invention aims to load Cu into two-dimensional MoS through glycol solution2the prepared nano material with high catalytic performance has high activity of photocatalytic hydrogen production performance, has good environmental protection performance, and can not cause environmental pollution and harm to users in the synthesis and photocatalytic processes.
the technical scheme adopted by the invention is as follows:
Two-dimensional MoS2The preparation method of the supported Cu photocatalyst is prepared by a solvothermal method and comprises the following steps:
(1) Two-dimensional MoS2The preparation of (1):
20mg of ammonium tetrathiomolybdate ((NH) were weighed out4)2MoS4) 20ml of N, N-Dimethylformamide (DMF) are added, ultrasound is carried out for 45min, and the yellow solution is poured into 50mlThe polytetrafluoroethylene reaction kettle is put into an electric heating forced air drying oven for reaction for 10 hours, the reaction temperature is 200 ℃, after the reaction is finished, the reaction kettle is naturally cooled to room temperature, centrifuged, separated, precipitated and respectively washed by deionized water and absolute ethyl alcohol for 3 times, and finally freeze-dried for 12 hours to obtain two-dimensional MoS2Marked N-MoS2；
(2) Two-dimensional MoS2Preparation of loaded Cu:
0.5g of the N-MoS prepared in the preceding step was weighed2Added to 28.51477ml Cu (NO)3)2In a glycol solution of (2), wherein CCu0.0002630215g/ml, performing ultrasonic treatment for 30min to obtain black suspension, adjusting the pH of the suspension to 8-9 with 0.2M NaOH solution under the condition of continuous stirring, performing cooling reflux under a 75 ℃ oil bath kettle and a magnetic stirrer, reacting for 5h, naturally cooling the suspension to room temperature, washing with deionized water and absolute ethanol for 3 times respectively, vacuum drying the product in a vacuum drying box at 80 ℃ for 48h, calcining the dried product at 400 ℃ under the protection of inert gas, calcining in a tubular furnace at the temperature rise rate of 1 ℃/min for 2h to obtain the two-dimensional MoS2Cu-supported catalyst, labeled E-Cu-N-MoS2。
The volume fraction of the ethylene glycol solution was 80%.
the invention prepares two-dimensional MoS2The Cu-loaded photocatalyst has stronger photocatalytic hydrogen evolution performance. The two-dimensional MoS is prepared by a solvothermal method and a calcination method2Supported Cu photocatalysts, i.e. Cu-N-MoS2The compound expands the absorption range of ultraviolet and visible light, enhances the absorption of light, inhibits the recombination of photo-generated electron-hole pairs and improves the photocatalytic hydrogen evolution performance of the product in the photocatalytic process; Cu-N-MoS2The compound can be recycled for multiple times in a photocatalytic hydrogen evolution circulation experiment, so that good stability is maintained; Cu-N-MoS2The compound has adsorbability and good application prospect in adsorbing pollutants.
The invention has the advantages that:
1. Two-dimensional MoS2The Cu-supported catalyst hasThe photocatalyst has strong photocatalytic hydrogen evolution performance, has good environmental protection performance, and does not cause pollution to the environment and harm to users in the synthesis and photocatalytic processes.
2、N-MoS2The photocatalytic hydrogen production speed is 1.059 mmoleg-1h-1，Cu-N-MoS2The photocatalytic hydrogen production rate is 1.283mmolg-1h-1E-Cu-N-MoS prepared from eighty percent by volume of ethylene glycol solution2The speed of the photocatalytic hydrogen production is 1.596 mmoleg-1h-1By the pair N-MoS2Literature and Cu-N-MoS2Comparison of photocatalytic hydrogen production shows that two-dimensional MoS loaded with Cu in ethylene glycol solution2The photocatalytic hydrogen evolution efficiency is obviously much higher; the literature reports that the hydrogen production rate of the photocatalyst is 0.24mmolg-1h-1and the actual hydrogen production rate is 1.596 mmoleg-1h-1Compared with the hydrogen production rate reported in the literature, the hydrogen production rate of the product prepared by the method is dozens of times higher. By the pair N-MoS2And Cu-N-MoS2Comparing the adsorption quantity of rhodamine to obtain the Cu-loaded two-dimensional MoS2The adsorption capacity of rhodamine can be improved.
3. The prepared E-Cu-N-MoS2The composite has small particle size and large surface area, and can provide more active sites for photocatalytic hydrogen evolution.
4. The two-dimensional MoS2No one has prepared the Cu-supported catalyst product before its production.
5. The invention adopts glycol solution as synthetic E-Cu-N-MoS2The solvent of the complex is favorable for the transmission of ions in the solution and is favorable for Cu in N-MoS2Loading, thereby effectively improving Cu-N-MoS2The photocatalytic performance of the compound enhances the hydrogen production efficiency, and the subsequent hydrogen production performance experiment proves.
drawings
FIG. 1 is a two-dimensional MoS of the present invention2a Cu-loaded catalyst hydrogen evolution performance diagram (A) and a rhodamine adsorption diagram (B).
FIG. 2 is a catalyst transmission diagram of the product of the present invention, and A is N-MoS2Drawing (1) ofB is Cu-N-MoS2FIG. C is E-Cu-N-MoS2。
Detailed Description
Example 1: two-dimensional MoS2The preparation method of the supported Cu photocatalyst is prepared by a solvothermal method and comprises the following steps:
(1) Two-dimensional MoS2The preparation of (1):
20mg of ammonium tetrathiomolybdate ((NH) were weighed out4)2MoS4) Adding 20ml of N, N-Dimethylformamide (DMF), carrying out ultrasonic treatment for 45min, pouring the yellow solution into a 50ml polytetrafluoroethylene reaction kettle, reacting for 10h in a forced air drying oven at 200 ℃, naturally cooling to room temperature after the reaction is finished, centrifuging, separating, washing precipitates respectively with deionized water and absolute ethyl alcohol for 3 times, and finally carrying out freeze drying for 12h to obtain the two-dimensional MoS2marked N-MoS2；
(2) Two-dimensional MoS2Preparation of loaded Cu:
0.5g of the N-MoS prepared in the preceding step was weighed2Added to 28.51477ml Cu (NO)3)2In a glycol solution of (2), wherein CCu0.0002630215g/ml, performing ultrasonic treatment for 30min to obtain black suspension, adjusting the pH of the suspension to 8-9 with 0.2M NaOH solution under the condition of continuous stirring, performing cooling reflux under 75 ℃ oil bath and magnetic stirrer for 5h, respectively washing the suspension for 3 times with deionized water and absolute ethyl alcohol after the suspension is naturally cooled to room temperature, performing vacuum drying on the product in a vacuum drying box at 80 ℃ for 48h, and finally calcining the dried product in a tubular furnace at the calcining temperature rising rate of 1 ℃/min for 2h under the conditions of nitrogen protection and 400 ℃ to obtain the two-dimensional MoS2Cu-supported catalyst, labeled E-Cu-N-MoS2。
The volume fraction of the ethylene glycol solution was 80%.
Comparative example 1: two-dimensional MoS2The preparation method of the supported Cu photocatalyst comprises the following preparation steps:
(1) two-dimensional MoS2The preparation of (1):
Weighing 20mg of tetrathionAmmonium molybdate ((NH)4)2MoS4) Adding 20ml of N, N-Dimethylformamide (DMF), carrying out ultrasonic treatment for 45min, pouring the yellow solution into a 50ml polytetrafluoroethylene reaction kettle, reacting for 10h in a forced air drying oven at 200 ℃, naturally cooling to room temperature after the reaction is finished, centrifuging, separating, washing precipitates respectively with deionized water and absolute ethyl alcohol for 3 times, and finally carrying out freeze drying for 12h to obtain the two-dimensional MoS2Marked N-MoS2；
(2) Two-dimensional MoS2Preparation of loaded Cu:
0.5g of the N-MoS prepared in the preceding step was weighed2Added to 28.51477ml Cu (NO)3)2in an aqueous solution, wherein CCu0.0002630215g/ml, performing ultrasonic treatment for 30min to obtain black suspension, adjusting the pH of the suspension to 8-9 with 0.2M NaOH solution under the condition of continuous stirring, performing cooling reflux under 75 ℃ oil bath and magnetic stirrer for 5h, respectively washing the suspension for 3 times with deionized water and absolute ethyl alcohol after the suspension is naturally cooled to room temperature, performing vacuum drying on the product in a vacuum drying box at 80 ℃ for 48h, and finally calcining the dried product in a tubular furnace at the calcining temperature rising rate of 1 ℃/min for 2h under the conditions of nitrogen protection and 400 ℃ to obtain the two-dimensional MoS2Cu-supported catalyst, designated Cu-N-MoS2。
N-MoS2The photocatalytic hydrogen production speed is 1.059 mmoleg-1h-1，Cu-N-MoS2The photocatalytic hydrogen production rate is 1.283mmolg-1h-1E-Cu-N-MoS prepared from eighty percent by volume of ethylene glycol solution2the speed of the photocatalytic hydrogen production is 1.596 mmoleg-1h-1By the pair N-MoS2The literature (Shaohong Zang, Guigan Zhang, Zhi-An Lan, Dandan Zheng, Xinchen Wang. enhancement of photocatalytic H)2 evolution on pyrene-based polymer promoted by MoS2 and visible light.Applied Catalysis B:Environmental[J]2019(251),102-111.) and Cu-N-MoS2Comparison of photocatalytic hydrogen production shows that two-dimensional MoS loaded with Cu in ethylene glycol solution2The photocatalytic hydrogen evolution efficiency is obviously much higher; the literature reports that the hydrogen production rate of the photocatalyst is 0.24mmolg-1h-1And the actual hydrogen production rate is 1.596 mmoleg-1h-1Compared with the hydrogen production rate reported in the literature, the hydrogen production rate of the product prepared by the method is dozens of times higher. By the pair N-MoS2and Cu-N-MoS2Comparing the adsorption quantity of rhodamine to obtain the Cu-loaded two-dimensional MoS2The adsorption capacity of rhodamine can be improved.
The invention relates to a two-dimensional MoS2Method for preparing Cu-loaded photocatalyst by two-dimensional MoS2The Cu is loaded, so that the nano material with high catalytic performance is prepared, the photocatalytic hydrogen production performance and activity are high, the nano material has good environmental protection performance, and the environment is not polluted and the user is not hurt in the synthesis and photocatalytic processes.
Claims (1)
1. Two-dimensional MoS2A method for preparing a Cu-loaded photocatalyst is characterized in that: the method comprises the following steps:
(1) Two-dimensional MoS2The preparation of (1):
20mg of ammonium tetrathiomolybdate ((NH) were weighed out4)2MoS4) Adding 20ml of N, N-Dimethylformamide (DMF), carrying out ultrasonic treatment for 45min, pouring the yellow solution into a 50ml polytetrafluoroethylene reaction kettle, reacting for 10h in a forced air drying oven at 200 ℃, naturally cooling to room temperature after the reaction is finished, centrifuging, separating, washing precipitates respectively with deionized water and absolute ethyl alcohol for 3 times, and finally carrying out freeze drying for 12h to obtain the two-dimensional MoS2Marked N-MoS2；
(2) Two-dimensional MoS2Preparation of loaded Cu:
0.5g of the N-MoS prepared in the preceding step was weighed2added to 28.51477ml Cu (NO)3)2Eighty percent by volume of ethylene glycol solution, wherein CCuSubjecting to ultrasonic treatment at 0.0002630215g/ml for 30min to obtain black suspension, adjusting pH to 8-9 with 0.2M NaOH solution under stirring, and subjecting to oil bath at 75 deg.C and magnetic stirringCooling and refluxing the suspension in a stirrer for 5h, respectively washing the suspension with deionized water and absolute ethyl alcohol for 3 times after the suspension is naturally cooled to room temperature, then carrying out vacuum drying on the product in a vacuum drying box at the temperature of 80 ℃ for 48h, and finally calcining the dried product in a tubular furnace at the calcining heating rate of 1 ℃/min for 2h under the conditions of nitrogen protection and the temperature of 400 ℃ to prepare the two-dimensional MoS2Cu-supported catalyst, labeled E-Cu-N-MoS2。
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