CN114984945B - CdS/V2O5Composite photocatalyst and preparation method thereof - Google Patents
CdS/V2O5Composite photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 13
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 abstract description 5
- 238000006303 photolysis reaction Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 20
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005086 pumping Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100001234 toxic pollutant Toxicity 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The application relates to the technical field of photocatalysts, and in particular discloses a CdS/V 2O5 composite photocatalyst, a preparation method and application thereof, and a preparation method of the CdS/V 2O5 composite photocatalyst, which comprises the following steps: adding cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide into deionized water and ammonia water, stirring, adding thioacetamide, and stirring to obtain a dark green solution A; pouring the solution A into polytetrafluoroethylene, and reacting for 20-24 hours at the temperature of 140-160 ℃; cooling to room temperature after the hydrothermal reaction is finished, carrying out suction filtration on the solution to obtain a product, and drying the product to obtain a sample; placing the sample into a porcelain boat and preserving heat for 2-5 hours at 400-600 ℃ to obtain a product; cooling the product to room temperature, taking out and grinding to obtain the CdS/V 2O5 composite photocatalyst. The CdS/V 2O5 composite photocatalyst has the advantage of improving the photodecomposition performance of CdS.
Description
Technical Field
The invention relates to the technical field of photocatalysts, in particular to a CdS/V 2O5 composite photocatalyst and a preparation method thereof.
Background
The exhaustion of energy resources and the destruction of ecological environment are two of the most urgent problems facing modern society. Thus, photocatalysis may provide a new solution to both problems by photocatalytic production of renewable fuels (such as hydrogen, methanol and methane) and by degradation and mineralization of toxic pollutants. Semiconductor photocatalytic technology has attracted considerable attention due to its potential application in environmental remediation, particularly in the purification of air and waste water. Semiconductor nanomaterials have become the main focus of research because of their unique optoelectronic properties.
In semiconductors CdS is a well known material, typically with a cubic or hexagonal crystal structure. A large number of researches show that the pure-phase CdS energy band gap width (2.4 ev) accords with most of solar visible light spectrum intensity, and the pure-phase CdS energy band gap width can be used as a visible light-sensitive photocatalyst to degrade organic pollutants or produce clean energy H 2. However, currently used CdS has low photocatalytic hydrogen production efficiency.
Disclosure of Invention
In order to improve the photodecomposition water performance of CdS, the application provides a CdS/V 2O5 composite photocatalyst, and a preparation method and application thereof.
In a first aspect, the present application provides a method for preparing a CdS/V 2O5 composite photocatalyst, which adopts the following technical scheme:
The preparation method of the CdS/V 2O5 composite photocatalyst comprises the following steps:
Step one: the molar ratio is (1.4-1.7): (3-6): (0.01-0.05) cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide are added into 40-60ml of deionized water and 8-10 ml of ammonia water, and the mixture is stirred uniformly to obtain a mixed solution with the concentration of cadmium nitrate of 0.024-0.029 mol/L; adding (1.27-1.5) g of thioacetamide into the mixed solution, and uniformly stirring to obtain a dark green solution A;
step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, and reacting for 20-24 hours at 140-160 ℃;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the solution, performing suction filtration to obtain a product, and performing vacuum drying on the product to obtain a sample;
step four: putting the sample into a porcelain boat, vacuumizing a tube furnace, slowly introducing argon into the tube furnace until the air in the tube furnace is completely discharged, and heating the tube furnace to 400-600 ℃ from room temperature at a heating rate of 10 ℃/min for 2-5 hours to obtain a product;
step five: and cooling the product to room temperature, taking out and grinding to obtain the CdS/V 2O5 composite photocatalyst.
Further, the mixed solution in the first step is obtained by stirring for 15-20 min at room temperature.
Further, the dark green solution A in the step one is obtained by stirring for 0.5 to 2 hours at the rotating speed of 500 to 800 r/min.
Further, the filling ratio of the second step is 50% -60%.
Further, the third step is to alternately filter the water and the ethanol for three times.
Further, the vacuum drying in the third step is performed at 60-80 ℃ for 6-8 hours.
In a second aspect, the application provides a CdS/V 2O5 composite photocatalyst, which adopts the following technical scheme:
The CdS/V 2O5 composite photocatalyst prepared by the preparation method is characterized in that: the CdS/V 2O5 composite photocatalyst has a regular nano-sheet structure.
Compared with the prior art, the application has the following technical effects:
the CdS/V 2O5 composite photocatalyst has uniform chemical composition, high purity and uniform morphology, and the structure of the catalyst is a regular nano-sheet structure, so that the structure is favorable for full contact of samples in photocatalysis, and the photochemical performance of the catalyst can be greatly enhanced.
In addition, the preparation method of the CdS/V 2O5 composite photocatalyst adopts a simpler hydrothermal and solid-phase sintering method synthesis process to generate a final product, and has the advantages of simple preparation process, short period, no need of large-scale equipment and harsh reaction conditions, low-cost and easily obtained raw materials, low cost, high yield and environmental friendliness.
Drawings
FIG. 1 is an X-ray diffraction analysis chart of CdS/V 2O5 in example 1.
FIG. 2 is a graph of a scanning analysis of CdS/V 2O5 in example 1.
FIG. 3 is a graph showing the analysis of hydrogen production performance of CdS/V 2O5 in example 1.
Detailed Description
The following examples are given to illustrate the invention in further detail, with particular reference to: the following examples, in which no specific conditions are noted, are conducted under conventional conditions or conditions recommended by the manufacturer, and the raw materials used in the following examples are commercially available from ordinary sources except for the specific descriptions.
Example 1
A preparation method of a CdS/V 2O5 composite photocatalyst comprises the following steps:
Step one: the molar ratio is 1.4:3: adding 40ml of deionized water and 8ml of ammonia water into 0.01 cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide, magnetically stirring for 15min at room temperature to obtain a mixed solution with cadmium nitrate concentration of 0.024mol/L, adding 1.27g of thioacetamide into the mixed solution, and stirring at the speed of 500r/min for 0.5h in a magnetic stirrer to obtain a dark green solution A;
Step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, controlling the filling ratio to be 50%, and reacting for 20 hours at 140 ℃;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the cooled solution after the reaction, alternately carrying out suction filtration on the solution by three times of deionized water and three times of ethanol, collecting a product, and drying the product at 60 ℃ for 6 hours under a vacuum condition to obtain a sample;
step four: putting the sample into a porcelain boat, pumping the tube furnace to a vacuum state, slowly introducing argon into the tube furnace, and repeatedly operating for three times until the air in the tube furnace is completely discharged, and heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min for 2 hours to obtain a product;
Step five: and cooling the product to room temperature, taking out and grinding for 15min to obtain the CdS/V 2O5 composite photocatalyst.
As can be seen from FIG. 1, the samples prepared correspond to PDF #65-2887 for CdS, PDF #52-0794 for V 2O5, indicating that CdS/V 2O5 was successfully prepared.
As can be seen from FIG. 2, the morphology of the CdS/V 2O5 sample is flaky, which increases the light absorption area and improves the photocatalytic hydrogen production performance.
As can be seen from fig. 3, V 2O5 shows that V 2O5 has no photocatalytic hydrogen production performance at a hydrogen production rate of 0; the hydrogen yield of CdS was 47.9. Mu. Mol g -1h-1;CdS/V2O5 and 901. Mu. Mol g -1h-1, which is 18 times the hydrogen yield of pure phase CdS.
Example 2
A preparation method of a CdS/V 2O5 composite photocatalyst comprises the following steps:
Step one: the molar ratio is 1.5:4: adding 45ml of deionized water and 9ml of ammonia water into 0.02 of cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide, magnetically stirring for 15min at room temperature to obtain a mixed solution with cadmium nitrate concentration of 0.026mol/L, adding 1.3g of thioacetamide into the mixed solution, and stirring at 600r/min for 1h in a magnetic stirrer to obtain a dark green solution A;
step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, controlling the filling ratio to be 45%, and reacting for 22 hours at 145 ℃;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the cooled solution after the reaction, alternately carrying out suction filtration on the solution by three times of deionized water and three times of ethanol, collecting a product, and drying the product at 60 ℃ for 6 hours under a vacuum condition to obtain a sample;
Step four: putting the sample into a porcelain boat, pumping the tube furnace to a vacuum state, slowly introducing argon into the tube furnace, and repeatedly operating for three times until the air in the tube furnace is completely discharged, and heating from room temperature to 450 ℃ at a heating rate of 10 ℃/min for 3 hours to obtain a product;
Step five: and cooling the product to room temperature, taking out and grinding for 15min to obtain the CdS/V 2O5 composite photocatalyst.
Example 3
A preparation method of a CdS/V 2O5 composite photocatalyst comprises the following steps:
Step one: the molar ratio is 1.6:5: adding 50ml of deionized water and 9ml of ammonia water into 0.04 cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide, magnetically stirring for 20min at room temperature to obtain a mixed solution with cadmium nitrate concentration of 0.029mol/L, adding 1.4g of thioacetamide into the mixed solution, and stirring at the speed of 700r/min for 1.5h in a magnetic stirrer to obtain a dark green solution A;
Step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, controlling the filling ratio to be 50%, and reacting for 24 hours at 150 ℃;
Step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the cooled solution after the reaction, alternately carrying out suction filtration on the solution by three times of deionized water and three times of ethanol, collecting a product, and drying the product at 80 ℃ for 8 hours under a vacuum condition to obtain a sample;
step four: putting the sample into a porcelain boat, pumping the tube furnace to a vacuum state, slowly introducing argon into the tube furnace, and repeatedly operating for three times until the air in the tube furnace is completely discharged, and heating from room temperature to 500 ℃ at a heating rate of 10 ℃/min for 4 hours to obtain a product;
Step five: and cooling the product to room temperature, taking out and grinding for 15min to obtain the CdS/V 2O5 composite photocatalyst.
Example 4
A preparation method of a CdS/V 2O5 composite photocatalyst comprises the following steps:
Step one: the molar ratio is 1.7:6: adding 60ml of deionized water and 10ml of ammonia water into 0.05 cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide, magnetically stirring for 20min at room temperature to obtain a mixed solution with cadmium nitrate concentration of 0.025mol/L, adding 1.5g of thioacetamide into the mixed solution, and stirring at the speed of 800r/min for 2h by a magnetic stirrer to obtain a dark green solution A;
step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, controlling the filling ratio to be 60%, and reacting for 24 hours at 160 ℃;
Step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the cooled solution after the reaction, alternately carrying out suction filtration on the solution by three times of deionized water and three times of ethanol, collecting a product, and drying the product at 80 ℃ for 8 hours under a vacuum condition to obtain a sample;
Step four: putting the sample into a porcelain boat, pumping the tube furnace to a vacuum state, slowly introducing argon into the tube furnace, and repeatedly operating for three times until the air in the tube furnace is completely discharged, and heating from room temperature to 600 ℃ at a heating rate of 10 ℃ per minute for 5 hours to obtain a product;
Step five: and cooling the product to room temperature, taking out and grinding for 15min to obtain the CdS/V 2O5 composite photocatalyst.
Claims (6)
1. The preparation method of the CdS/V 2O5 composite photocatalyst is characterized by comprising the following steps of:
Step one: the molar ratio is (1.4-1.7): (3-6): (0.01-0.05) adding cadmium nitrate, ammonium metavanadate and hexadecyl trimethyl ammonium bromide into 40-60ml of deionized water and 8-10 ml of ammonia water, and uniformly stirring to obtain a mixed solution with the concentration of cadmium nitrate of 0.024-0.029 mol/L; then adding 1.27-1.5 g of thioacetamide into the mixed solution, and uniformly stirring to obtain a dark green solution A;
Step two: pouring the solution A into a reaction kettle filled with polytetrafluoroethylene, placing the reaction kettle into a homogeneous phase reactor, and reacting for 20-24 hours at 140-160 ℃;
step three: naturally cooling the reaction kettle to room temperature after the reaction is finished, pouring out the solution, performing suction filtration to obtain a product, and performing vacuum drying on the product to obtain a sample;
Step four: putting the sample into a porcelain boat, vacuumizing a tube furnace, slowly introducing argon into the tube furnace until the air in the tube furnace is completely discharged, and heating the tube furnace to 400-600 ℃ from room temperature at a heating rate of 10 ℃/min, and preserving heat for 2-5 h ℃ to obtain a product;
Step five: and cooling the product to room temperature, taking out and grinding to obtain the CdS/V 2O5 composite photocatalyst with the regular nano-sheet structure.
2. The method for preparing the CdS/V 2O5 composite photocatalyst according to claim 1, which is characterized in that: the mixed solution obtained in the step one is obtained by stirring for 15-20 min at room temperature.
3. The method for preparing the CdS/V 2O5 composite photocatalyst according to claim 1, which is characterized in that: the dark green solution A in the step one is obtained by stirring for 0.5-2 hours at the rotating speed of 500-800 r/min.
4. The method for preparing the CdS/V 2O5 composite photocatalyst according to claim 1, which is characterized in that: and the filling ratio of the second step is 50% -60%.
5. The method for preparing the CdS/V 2O5 composite photocatalyst according to claim 1, which is characterized in that: and in the third step, the suction filtration is performed by alternately performing suction filtration on the water and the ethanol for three times.
6. The method for preparing the CdS/V 2O5 composite photocatalyst according to claim 1, which is characterized in that: and the third step of vacuum drying is to dry for 6-8 hours at the temperature of 60-80 ℃.
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