CN110368956B - Nanometer flower-shaped VS2Preparation method of composite micro-particle CdS photocatalyst - Google Patents
Nanometer flower-shaped VS2Preparation method of composite micro-particle CdS photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000011859 microparticle Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 15
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- 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 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000005547 deoxyribonucleotide Substances 0.000 claims abstract description 7
- 125000002637 deoxyribonucleotide group Chemical group 0.000 claims abstract description 7
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- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
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- 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
- 235000011178 triphosphate Nutrition 0.000 claims abstract description 7
- 239000001226 triphosphate Substances 0.000 claims abstract description 7
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 claims abstract description 7
- JCIBFWRKAKESTL-UHFFFAOYSA-N 2-(16-bromohexadecyl)pyridine Chemical compound BrCCCCCCCCCCCCCCCCC1=CC=CC=N1 JCIBFWRKAKESTL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
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- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
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- 239000002057 nanoflower Substances 0.000 claims 7
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- 238000006303 photolysis reaction Methods 0.000 abstract description 2
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- 238000011160 research Methods 0.000 description 2
- QAQSNXHKHKONNS-UHFFFAOYSA-N 1-ethyl-2-hydroxy-4-methyl-6-oxopyridine-3-carboxamide Chemical compound CCN1C(O)=C(C(N)=O)C(C)=CC1=O QAQSNXHKHKONNS-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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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
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- 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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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
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Abstract
The invention discloses a nanometer flower-shaped VS2The preparation method of the composite micro-particle CdS photocatalyst comprises the following steps of 1: mixing 0.5-2 mol of cadmium nitrate, 2-4 mol of sodium metavanadate, 0.01-0.05 mol of bromohexadecyl pyridine and 0.001-0.005 mol of deoxyribonucleotide triphosphate to form a mixture; step 2: adding 40-60 ml of ethanol into the mixture, stirring and dissolving for the first time, adding 0.15-0.3 g of thioacetamide, stirring and dissolving for the second time to obtain a solution A; and step 3: putting the solution A into a reaction kettle for hydrothermal reaction at 160-180 ℃, and cooling to room temperature; and 4, step 4: taking out the solution B, filtering, drying the filtrate and grinding into powder to obtain the nano flower-like VS2Composite micro-particle CdS photocatalyst. The nano flower-like VS prepared by the method2The composite micro-particle CdS photocatalyst can effectively improve the water photolysis performance of CdS.
Description
Technical Field
The invention belongs to the technical field of photocatalysts, and relates to a photocatalystPopcorn like VS2A preparation method of a composite micro-particle CdS photocatalyst.
Background
Exhaustion of energy resources and destruction of ecological environment pollution are two of the most urgent problems facing modern society. Thus, photocatalysis can provide a new solution to the problem of producing renewable fuels (such as hydrogen, methanol and methane) by photocatalysis, and to alleviate both problems by degrading and mineralizing toxic pollutants. Semiconductor photocatalytic technology has attracted extensive attention due to its potential applications in environmental remediation, particularly in air and wastewater purification processes. Semiconductor nanomaterials have been 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 (2.4ev) accords with most of the solar visible light spectrum intensity, so that the pure-phase CdS energy band gap can be used as a visible light sensitive photocatalyst to degrade organic pollutants or produce clean energy H2. But the currently used CdS has low photocatalytic efficiency.
Disclosure of Invention
The invention aims to provide a nano flower-shaped VS2Preparation method of composite micro-particle CdS photocatalyst and nanoflower-shaped VS prepared by same2The composite micro-particle CdS photocatalyst can effectively improve the water photolysis performance of CdS.
The invention is realized by the following technical scheme:
nanometer flower-shaped VS2The preparation method of the composite particulate CdS photocatalyst comprises the following steps:
step 1: mixing 0.5-2 mol of cadmium nitrate, 2-4 mol of sodium metavanadate, 0.01-0.05 mol of bromohexadecyl pyridine and 0.001-0.005 mol of deoxyribonucleotide triphosphate to form a mixture;
step 2: adding 40-60 ml of ethanol into the mixture, stirring and dissolving for the first time, adding 0.15-0.3 g of thioacetamide, stirring and dissolving for the second time to obtain a solution A;
and 3, step 3: placing the solution A in a reaction kettle for hydrothermal reaction at 160-180 ℃, 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 the nano flower-shaped VS2Composite micro-particle CdS 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, sealed and then placed in a reaction kettle and subjected to hydrothermal reaction in a homogeneous phase reactor.
Furthermore, the hydrothermal reaction time in the step 3 is 20-24 h.
Further, the lining in the step 3 is a polytetrafluoroethylene lining, and the filling ratio is 40-60%.
Further, the step 4 of suction filtration is to adopt ultrapure water and ethanol for suction filtration.
Further, the drying in the step 4 is vacuum drying for 6-8 hours at the temperature of 60-80 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a nano flower-shaped VS2Method for preparing composite micro-particle CdS photocatalyst, which adopts one-step hydrothermal method to prepare final product, has simple preparation method, and prepares flower-like VS2The CdS nano-particles are compounded with the micro-particle CdS to form a regular nano-sheet and micro-particle structure, and the structure is beneficial to full contact of a sample in photocatalytic hydrogen production; 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 occurrence of photo-corrosivity of the CdS is inhibited, 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 prepared in example 1;
FIG. 2 is a scanning analysis chart of the photocatalyst prepared in example 1;
FIG. 3 is a graph showing the hydrogen production performance of the photocatalyst prepared in example 1.
Detailed Description
Specific examples are given below.
Example 1
Nanometer flower-shaped VS2The preparation method of the composite particulate CdS photocatalyst comprises the following steps:
step 1: 0.5mol of cadmium nitrate, 2mol of sodium metavanadate, 0.01mol of bromohexadecyl pyridine and 0.001mol of deoxyribonucleotide triphosphate are mixed to form a mixture;
and 2, step: adding 40ml of ethanol into the mixture, magnetically stirring for 15min at the rotating speed of 500r/min and dissolving, adding 0.15g of thioacetamide, magnetically stirring for 0.5h at the rotating speed of 500r/min and dissolving to obtain a solution A;
and step 3: putting the solution A into a polytetrafluoroethylene lining, sealing, putting into a reaction kettle, carrying out hydrothermal reaction for 20 hours at 160 ℃ in a homogeneous phase reactor, 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 60 deg.C for 6 hr, and grinding into powder to obtain nanometer flower-like VS2Composite micro CdS photocatalyst.
Taking nano flower-like VS2Composite particulate CdS photocatalyst samples, as shown in FIG. 1, VS was prepared in this example2CdS/CdS complex with CdS numbered 80-0006 and VS numbered 36-1139 of PDF standard card2Correspondingly, the VS was successfully prepared2A CdS complex; as shown in FIG. 2, particulate CdS are attached to flower-like VS, which is composed of sheet layers2On the nanostructure; as shown in FIG. 3, the flower-like VS prepared for this example2The performance diagram of the granular CdS nano composite photocatalyst for preparing hydrogen by decomposing water shows that the performance after compounding is improved by 15.5 times compared with that of pure-phase CdS.
Example 2
Nano flower-shaped VS2Composite particlesThe preparation method of the CdS photocatalyst comprises the following steps:
step 1: mixing 1mol of cadmium nitrate, 2mol of sodium metavanadate, 0.02mol of bromohexadecyl pyridine and 0.002mol of deoxyribonucleotide triphosphate to form a mixture;
step 2: adding 50ml of ethanol into the mixture, magnetically stirring for 15min at the rotating speed of 600r/min and dissolving, adding 0.2g of thioacetamide, magnetically stirring for 1h at the rotating speed of 600r/min and dissolving to obtain a solution A;
and step 3: putting the solution A into a polytetrafluoroethylene lining, sealing, putting into a reaction kettle, carrying out hydrothermal reaction for 22 hours at 160 ℃ in a homogeneous phase reactor, 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 the solution B, alternately filtering with three times of ultrapure water and three times of ethanol, vacuum drying the filtrate at 60 deg.C for 6 hr, and grinding into powder to obtain nanometer flower-like VS2Composite micro CdS photocatalyst.
Example 3
Nanometer flower-shaped VS2The preparation method of the composite micro-particle CdS photocatalyst comprises the following steps:
step 1: mixing 1.5mol of cadmium nitrate, 3mol of sodium metavanadate, 0.03mol of bromohexadecyl pyridine and 0.003mol of deoxyribonucleotide triphosphate to form a mixture;
and 2, step: adding 60ml of ethanol into the mixture, magnetically stirring for 18min at the rotating speed of 700r/min and dissolving, adding 0.15g of thioacetamide, magnetically stirring for 1.5h at the rotating speed of 700r/min and dissolving to obtain a solution A;
and 3, step 3: putting the solution A into a polytetrafluoroethylene lining, sealing, putting into a reaction kettle, carrying out hydrothermal reaction for 24 hours at 180 ℃ in a homogeneous phase reactor, and cooling to room temperature to obtain a solution B; wherein the filling ratio of the lining 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 70 deg.C for 7 hr, and grinding into powder to obtain nanometer flower-like VS2Composite micro CdS photocatalyst.
Example 4
Nanometer flower-shaped VS2The preparation method of the composite micro-particle CdS photocatalyst comprises the following steps:
step 1: mixing 2mol of cadmium nitrate, 4mol of sodium metavanadate, 0.05mol of cetyl pyridinium bromide and 0.005mol of deoxyribonucleotide triphosphate to form a mixture;
and 2, step: adding 60ml of ethanol into the mixture, magnetically stirring for 20min at the rotating speed of 800r/min and dissolving, adding 0.3g of thioacetamide, magnetically stirring for 2h at the rotating speed of 800r/min and dissolving to obtain a solution A;
and step 3: putting the solution A into a polytetrafluoroethylene lining, sealing, putting into a reaction kettle, carrying out hydrothermal reaction for 24 hours at 180 ℃ in a homogeneous reactor, 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 8 hr, and grinding into powder to obtain nanometer flower-like VS2Composite micro CdS photocatalyst.
The invention adopts a simpler one-step hydrothermal synthesis process to generate a final product, has simple preparation process, short period, no need of large-scale equipment and harsh reaction conditions, cheap and easily-obtained raw materials, low cost, high yield and environmental friendliness. Prepared CdS composite VS2Regular nanosheet and microparticle structures are formed. The structure is beneficial to the full contact of samples in photocatalysis, and the photochemical performance of the structure can be greatly enhanced. The prepared product has the advantages of uniform chemical composition, high purity and uniform appearance.
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 (8)
1. Nanometer flower-shaped VS2The preparation method of the composite particulate CdS photocatalyst is characterized by comprising the following steps of:
step 1: mixing 0.5-2 mol of cadmium nitrate, 2-4 mol of sodium metavanadate, 0.01-0.05 mol of bromohexadecyl pyridine and 0.001-0.005 mol of deoxyribonucleotide triphosphate to form a mixture;
step 2: adding 40-60 ml of ethanol into the mixture, stirring and dissolving for the first time, adding 0.15-0.3 g of thioacetamide, stirring and dissolving for the second time to obtain a solution A;
and step 3: placing the solution A in a reaction kettle for hydrothermal reaction at 160-180 ℃, 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 the nano flower-shaped VS2Composite micro-particle CdS photocatalyst.
2. A nanoflower VS according to claim 12The preparation method of the composite micro-particle CdS photocatalyst is characterized in that in the step 2, the primary stirring is magnetic stirring for 15-20 min at the rotating speed of 500-800 r/min.
3. A nanoflower VS according to claim 12The preparation method of the composite micro-particle CdS photocatalyst is characterized in that in the step 2, the secondary stirring is magnetic stirring for 0.5-2 hours at the rotating speed of 500-800 r/min.
4. A nanoflower VS according to claim 12The preparation method of the composite particulate CdS photocatalyst is characterized in that in the step 3, the solution A is placed in a lining and sealed, then placed in a reaction kettle and subjected to hydrothermal reaction in a homogeneous phase reactor.
5. A nanoflower VS according to claim 42The preparation method of the composite micro-particle CdS photocatalyst is characterized in that the hydrothermal reaction time in the step 3 is 20-24 hours.
6. A nanoflower VS according to claim 42The preparation method of the composite particle CdS photocatalyst is characterized in that the lining in the step 3 is a polytetrafluoroethylene lining and the filling ratio is 40 to E60％。
7. A nanoflower VS according to claim 12The preparation method of the composite micro-particle CdS photocatalyst is characterized in that the suction filtration in the step 4 is performed by adopting ultrapure water and ethanol.
8. A nanoflower VS according to claim 12The preparation method of the composite micro-particle CdS photocatalyst is characterized in that the drying in the step 4 is vacuum drying for 6-8 hours at the temperature of 60-80 ℃.
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