CN110368955B - VS (virtual switch)2Preparation method of CdS composite photocatalyst - Google Patents
VS (virtual switch)2Preparation method of CdS composite photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 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
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 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
- 238000001035 drying Methods 0.000 claims abstract description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 39
- 229910052717 sulfur Inorganic materials 0.000 description 12
- 239000011593 sulfur Substances 0.000 description 12
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 8
- NGTSQWJVGHUNSS-UHFFFAOYSA-N bis(sulfanylidene)vanadium Chemical compound S=[V]=S NGTSQWJVGHUNSS-UHFFFAOYSA-N 0.000 description 8
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 229910001456 vanadium ion Inorganic materials 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000926 separation method 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
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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 discloses a VS2The preparation method of the CdS composite photocatalyst comprises the steps of mixing 0.5-2 mol of cadmium acetate, 2-4 mol of ammonium metavanadate and 8-10 mol of thioacetamide to obtain a mixture; adding 40-60 ml of deionized water into the mixture, stirring for the first time, adding 8-10 ml of ammonia water, stirring for the second time, and dissolving to obtain a solution A; placing the solution A in a reaction kettle for primary hydrothermal reaction at 140-160 ℃, cooling to room temperature, performing secondary hydrothermal reaction at 160-180 ℃, and cooling to room temperature to obtain a solution B; taking out the solution B, filtering, drying the filtrate and grinding into powder to obtain VS2A CdS composite photocatalyst; the method has the advantages of simple operation, short time consumption, low preparation cost, high product purity and excellent performance of the prepared photocatalyst.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and relates to VS2A preparation method of a CdS composite photocatalyst.
Background
With the rapid development of industry and the mass combustion of fossil fuels, the problems of environmental pollution and energy shortage faced by human beings are increasingly highlighted. The direct discharge of various pollutants into the agricultural environment not only affects the agricultural production, but also affects the health of human beings. Meanwhile, the large consumption of fossil fuels also brings about an increasingly severe energy crisis, and the search for new clean energy has become a target for human pursuit. Solar energy is an effective way for obtaining renewable resources, photoelectric conversion, photothermal conversion, photochemical conversion and other methods can achieve the purpose of storing and using the solar energy, and the semiconductor material-based photocatalytic technology is a method for converting the light energy into chemical energy, so that the solar energy can be directly converted into hydrogen energy or used for catalyzing and degrading pollutants.
Semiconductor photocatalysts such as ZnO and TiO2 cannot fully utilize sunlight because of their wide band gaps. Scientists have therefore developed a variety of visible light responsive semiconductor photocatalysts, wherein CdS has a better visible light response, mainly because CdS has a suitable position of the conduction band edge, a good visible light absorption range, and excellent electron mobility. [ Zhangjing ] research on the activity of hydrogen production by photolysis and the characteristics of photo-generated charge of a CdS-based semiconductor photocatalyst [ Ph scientific thesis ]. Changchun: jilin university, 2015 however, the high electron-hole recombination rate limits its hydrogen production rate. Therefore, there is an urgent need to find a method for reducing electron-hole recombination.
At present, some researchers compound precious metals such as gold, silver and platinum with a semiconductor to effectively reduce the electron-hole recombination rate, but the precious metals are expensive and are not beneficial to large-area popularization, and promoters such as the precious metals are not uniformly distributed on the surface of the semiconductor photocatalyst.
Disclosure of Invention
The invention solves the technical problem of providing VS with simple method operation, short time consumption and high product purity2The preparation method of the CdS composite photocatalyst has low preparation cost and excellent performance of the prepared photocatalyst.
The invention is realized by the following technical scheme:
VS (virtual switch)2The preparation method of the/CdS composite photocatalyst comprises the following steps:
step 1: taking 0.5-2 mol of cadmium acetate, 2-4 mol of ammonium metavanadate and 8-10 mol of thioacetamide, and mixing to obtain a mixture;
step 2: adding 40-60 ml of deionized water into the mixture, stirring for the first time, adding 8-10 ml of ammonia water, and stirring for the second time to obtain a solution A;
and step 3: placing the solution A in a reaction kettle for primary hydrothermal reaction at 140-160 ℃, cooling to room temperature, performing secondary hydrothermal reaction at 170-180 ℃, and cooling to room temperature to obtain a solution B;
and 4, step 4: taking out the solution B, filtering, drying the filtrate and grinding into powder to obtain VS2A CdS composite photocatalyst.
Further, in the step 2, the primary stirring is magnetic stirring for 15-20 min at the rotating speed of 500-800 r/min.
Further, in the step 2, the secondary stirring is magnetic stirring for 0.5-2 hours at the rotating speed of 500-800 r/min.
Further, in the step 3, the solution A is placed in a liner and sealed, and is placed in a reaction kettle to carry out primary hydrothermal reaction and secondary hydrothermal reaction in a homogeneous phase reactor.
Further, the lining in the step 3 is a polytetrafluoroethylene lining, and the filling ratio is 40-60%.
Furthermore, the time of the first hydrothermal reaction in the step 3 is 18-20 hours.
Further, the time of the secondary hydrothermal reaction in the step 3 is 5-8 hours.
Further, in the step 4, ultra-pure water and ethanol are adopted for suction filtration.
Further, the drying in the step 4 is vacuum drying for 8-10 hours at 70-80 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a VS2The preparation method of the CdS composite photocatalyst adopts a segmented temperature rise method to synthesize a final product, and has lower synthesis temperature; the method has a simple synthesis path, does not need large-scale equipment and harsh reaction conditions, and has the advantages of cheap and easily-obtained raw materials, low cost, high yield and no need of excessive post-treatment compared with commonly used precious metals such as gold, silver, platinum and the like; it will VS2Complexing with CdS, VS2The introduction of the CdS nano particles improves the separation of photo-generated electron-hole pairs of the CdS nano particles, the specific surface area of the CdS nano particles after the compounding is increased, the migration rate of photo-generated electrons is accelerated, and the photocatalysis performance of the CdS nano particles is further improved.
Drawings
FIG. 1 is an X-ray diffraction analysis chart of the photocatalyst produced in example 1;
FIG. 2 is a scanning analysis chart of the photocatalyst produced in example 1;
FIG. 3 is a graph showing the hydrogen production performance of the photocatalyst produced in example 1.
Detailed Description
Specific examples are given below.
Example 1
VS (virtual switch)2The preparation method of the/CdS composite photocatalyst comprises the following steps of:
step 1: taking and mixing 0.5mol of cadmium acetate, 2mol of ammonium metavanadate and 8mol of thioacetamide to obtain a mixture;
step 2: adding 40ml of deionized water into the mixture, and magnetically stirring for 15min at the rotating speed of 500r/min, wherein the concentration of cadmium ions is 0.0125mol/L, the concentration of vanadium ions is 0.05mol/L, and the concentration of sulfur ions is 0.2 mol/L; then 8ml of ammonia water is added and the mixture is magnetically stirred for 0.5h at the rotating speed of 500r/min, thus obtaining solution A;
and step 3: placing the solution A into a polytetrafluoroethylene lining, sealing, placing the polytetrafluoroethylene lining into a reaction kettle in a homogeneous phase reactor, carrying out a hydrothermal reaction for 18h at 140 ℃, carrying out a combined reaction of vanadium ions and sulfur ions in the process to generate vanadium disulfide, and cooling to room temperature; carrying out secondary hydrothermal reaction for 5h at 170 ℃, carrying out combined reaction on cadmium ions and residual sulfur ions in the process to generate cadmium sulfide, compounding the cadmium sulfide and vanadium disulfide, and cooling to room temperature to obtain a solution B; wherein the fill ratio of the liner is 40%;
and 4, step 4: taking out the solution B, alternately filtering with three times of ultrapure water and three times of ethanol, vacuum drying the filtrate at 70 deg.C for 8 hr, and grinding into powder to obtain VS2A CdS composite photocatalyst.
Get VS2Sample of/CdS composite photocatalyst, as shown in FIG. 1, VS was prepared in this example2CdS/CdS composite with CdS with PDF standard card number of 41-1049 and VS with PDF standard card number of 36-11392Correspondingly, the VS was successfully prepared2A CdS complex; as shown in FIG. 2, CdS is attached to VS2To form the composite photocatalyst; as shown in FIG. 3, VS was prepared for this example2The performance of the/CdS composite photocatalyst for preparing hydrogen by decomposing water is improved by 5.09 times compared with that of pure-phase CdS.
Example 2
VS (right-angle switch)2The preparation method of the/CdS composite photocatalyst comprises the following steps:
step 1: mixing 1mol of cadmium acetate, 3mol of ammonium metavanadate and 9mol of thioacetamide to obtain a mixture;
step 2: adding 45ml of deionized water into the mixture, and magnetically stirring for 15min at the rotating speed of 600r/min, wherein the concentration of cadmium ions is 0.0222mol/L, the concentration of vanadium ions is 0.0667mol/L, and the concentration of sulfur ions is 0.2 mol/L; adding 9ml of ammonia water, and magnetically stirring for 1h at the rotating speed of 600r/min to obtain a solution A;
and step 3: placing the solution A into a polytetrafluoroethylene lining, sealing, placing the polytetrafluoroethylene lining into a reaction kettle in a homogeneous phase reactor, carrying out a hydrothermal reaction for 19 hours at 145 ℃, carrying out a combined reaction of vanadium ions and sulfur ions in the process to generate vanadium disulfide, and cooling to room temperature; carrying out secondary hydrothermal reaction for 6h at 175 ℃, carrying out combined reaction on cadmium ions and residual sulfur ions in the process to generate cadmium sulfide, compounding the cadmium sulfide and vanadium disulfide, and cooling to room temperature to obtain a solution B; wherein the fill ratio of the liner is 50%;
and 4, step 4: taking out solution B, alternately filtering with three times of ultrapure water and three times of ethanol, vacuum drying the filtrate at 70 deg.C for 9 hr, and grinding into powder to obtain VS2A CdS composite photocatalyst.
Example 3
VS (virtual switch)2The preparation method of the/CdS composite photocatalyst comprises the following steps:
step 1: taking 1.5mol of cadmium acetate, 3.5mol of ammonium metavanadate and 9.5mol of thioacetamide, and mixing to obtain a mixture;
step 2: adding 50ml of deionized water into the mixture, and magnetically stirring for 20min at the rotating speed of 700r/min, wherein the concentration of cadmium ions is 0.03mol/L, the concentration of vanadium ions is 0.07mol/L, and the concentration of sulfur ions is 0.19 mol/L; adding 9ml of ammonia water, and magnetically stirring for 1h at the rotating speed of 700r/min to obtain a solution A;
and step 3: placing the solution A into a polytetrafluoroethylene lining, sealing, placing the polytetrafluoroethylene lining into a reaction kettle in a homogeneous phase reactor, carrying out hydrothermal reaction for 20 hours at 150 ℃, carrying out combined reaction on vanadium ions and sulfur ions in the process to generate vanadium disulfide, and cooling to room temperature; carrying out secondary hydrothermal reaction for 7h at 170 ℃, carrying out combined reaction on cadmium ions and residual sulfur ions in the process to generate cadmium sulfide, compounding the cadmium sulfide and vanadium disulfide, and cooling to room temperature to obtain a solution B; wherein the fill ratio of the liner is 55%;
and 4, step 4: taking out solution B, alternately filtering with three times of ultrapure water and three times of ethanol, vacuum drying the filtrate at 80 deg.C for 9 hr, and grinding into powder to obtain VS2A CdS composite photocatalyst.
Example 4
VS (virtual switch)2The preparation method of the/CdS composite photocatalyst comprises the following steps:
step 1: mixing 2mol of cadmium acetate, 4mol of ammonium metavanadate and 10mol of thioacetamide to obtain a mixture;
step 2: adding 60ml of deionized water into the mixture, and magnetically stirring for 20min at the rotating speed of 800r/min, wherein the concentration of cadmium ions is 0.033mol/L, the concentration of vanadium ions is 0.067mol/L, and the concentration of sulfur ions is 0.6 mol/L; then 10ml of ammonia water is added and magnetically stirred for 2 hours at the rotating speed of 800r/min to obtain a solution A;
and 3, step 3: placing the solution A into a polytetrafluoroethylene lining, sealing, placing the polytetrafluoroethylene lining into a reaction kettle in a homogeneous phase reactor, carrying out a hydrothermal reaction for 20 hours at 160 ℃, carrying out a combined reaction of vanadium ions and sulfur ions in the process to generate vanadium disulfide, and cooling to room temperature; carrying out secondary hydrothermal reaction at 180 ℃ for 8h, carrying out combined reaction on cadmium ions and residual sulfur ions in the process to generate cadmium sulfide, compounding the cadmium sulfide and vanadium disulfide, and cooling to room temperature to obtain a solution B; wherein the fill ratio of the liner is 60%;
and 4, step 4: taking out the solution B, alternately filtering with three times of ultrapure water and three times of ethanol, vacuum drying the filtrate at 80 deg.C for 10 hr, and grinding into powder to obtain VS2A CdS composite photocatalyst.
The method adopts a sectional heating method to synthesize the final product, has lower synthesis temperature, simpler synthesis path, no need of large-scale equipment and harsh reaction conditions, cheap and easily obtained raw materials, low cost, high yield, no need of excessive post-treatment, environmental friendliness and suitability for large-scale production; the product prepared by the method has uniform chemical composition, high purity and uniform appearance, and can show good photochemical performance when being used as a material for producing hydrogen by photolysis of water; compared with pure-phase CdS, the product prepared by the method reduces the recombination of photo-generated electrons and holes and improves the migration rate of the photo-generated electrons.
The embodiments given above are preferable examples for implementing the present invention, and the present invention is not limited to the above-described embodiments. Any non-essential addition and replacement made by the technical characteristics of the technical scheme of the invention by a person skilled in the art belong to the protection scope of the invention.
Claims (9)
1. VS (virtual switch)2The preparation method of the/CdS composite photocatalyst is characterized by comprising the following steps of:
step 1: taking 0.5-2 mol of cadmium acetate, 2-4 mol of ammonium metavanadate and 8-10 mol of thioacetamide, and mixing to obtain a mixture;
step 2: adding 40-60 ml of deionized water into the mixture, stirring for the first time, adding 8-10 ml of ammonia water, and stirring for the second time to obtain a solution A;
and step 3: placing the solution A in a reaction kettle for primary hydrothermal reaction at 140-160 ℃, cooling to room temperature, performing secondary hydrothermal reaction at 170-180 ℃, and cooling to room temperature to obtain a solution B;
and 4, step 4: taking out the solution B, filtering, drying the filtrate and grinding into powder to obtain VS2A CdS composite photocatalyst.
2. A VS as claimed in claim 12The preparation method of the/CdS composite photocatalyst is characterized in that in the step 2, magnetic stirring is carried out for 15-20 min at the rotating speed of 500-800 r/min.
3. A VS as claimed in claim 12Preparation method of/CdS composite photocatalyst and preparation method thereofCharacterized in that the secondary stirring in the step 2 is magnetic stirring for 0.5-2 hours at the rotating speed of 500-800 r/min.
4. A VS as claimed in claim 12The preparation method of the/CdS composite photocatalyst is characterized in that the solution A in the step 3 is placed in a lining to be sealed and is placed in a reaction kettle to carry out primary hydrothermal reaction and secondary hydrothermal reaction in a homogeneous phase reactor.
5. A VS as defined in claim 42The preparation method of the/CdS composite photocatalyst is characterized in that in the step 3, the inner lining is a polytetrafluoroethylene inner lining, and the filling ratio is 40-60%.
6. A VS as defined in claim 42The preparation method of the/CdS composite photocatalyst is characterized in that the time of one-time hydrothermal reaction in the step 3 is 18-20 hours.
7. A VS as defined in claim 42The preparation method of the/CdS composite photocatalyst is characterized in that the time of the secondary hydrothermal reaction in the step 3 is 5-8 hours.
8. A VS as claimed in claim 12The preparation method of the/CdS composite photocatalyst is characterized in that ultrapure water and ethanol are adopted for suction filtration in the step 4.
9. A VS as claimed in claim 12The preparation method of the/CdS composite photocatalyst is characterized in that the drying in the step 4 is vacuum drying for 8-10 hours at the temperature of 70-80 ℃.
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| CN113193198A (en) * | 2021-04-30 | 2021-07-30 | 陕西科技大学 | Cobalt-doped vanadium disulfide micron sheet and preparation method thereof |
| CN114984945A (en) * | 2022-06-24 | 2022-09-02 | 陕西科技大学 | CdS/V 2 O 5 Composite photocatalyst and preparation method thereof |
| CN114975963A (en) * | 2022-06-28 | 2022-08-30 | 陕西科技大学 | VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof |
| CN115779932B (en) * | 2022-11-01 | 2024-04-02 | 陕西科技大学 | V-CdS/NiS 2 Preparation method of composite photocatalyst |
Citations (5)
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| CN106378160A (en) * | 2016-09-19 | 2017-02-08 | 江苏大学 | Method for preparing CdS/MoS2 composite hollow-block photocatalyst |
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| CN108126712A (en) * | 2017-12-22 | 2018-06-08 | 陕西科技大学 | A kind of VOOH/VS4Micron composite granule and preparation method and application |
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| CN109939699A (en) * | 2019-04-16 | 2019-06-28 | 湘潭大学 | A kind of molybdenum doping vanadium disulfide micron floral material and its preparation method and application |
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| CN106378160A (en) * | 2016-09-19 | 2017-02-08 | 江苏大学 | Method for preparing CdS/MoS2 composite hollow-block photocatalyst |
| CN108046320A (en) * | 2017-12-19 | 2018-05-18 | 重庆大学 | A kind of preparation method of electrode material for super capacitor vanadic sulfide nano flower |
| CN108126712A (en) * | 2017-12-22 | 2018-06-08 | 陕西科技大学 | A kind of VOOH/VS4Micron composite granule and preparation method and application |
| CN109201083A (en) * | 2018-10-29 | 2019-01-15 | 陕西科技大学 | A kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide and preparation method thereof |
| CN109939699A (en) * | 2019-04-16 | 2019-06-28 | 湘潭大学 | A kind of molybdenum doping vanadium disulfide micron floral material and its preparation method and application |
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