CN112158878B - Preparation method of hexagonal pyramid-like CdS and application of hexagonal pyramid-like CdS in field of photocatalytic hydrogen production - Google Patents
Preparation method of hexagonal pyramid-like CdS and application of hexagonal pyramid-like CdS in field of photocatalytic hydrogen production Download PDFInfo
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000001257 hydrogen Substances 0.000 title claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 24
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 9
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical group [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000003607 modifier Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 230000035484 reaction time Effects 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- -1 spheres Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
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- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a preparation method of hexagonal pyramid-like CdS and application of the hexagonal pyramid-like CdS in the field of photocatalytic hydrogen production, and belongs to the field of inorganic materials. Firstly, mixing a cadmium source solution and a sodium sulfide solution to obtain a precipitate; mixing the precipitate with urea, LiOH & H 2 And (3) reacting the O molten salt system to obtain the hexagonal pyramid-like CdS. The invention does not adopt any organic surfactant or surface modifier, does not need post treatment, has no environmental pollution and is easy for industrialized production. The quasi-hexagonal pyramid CdS prepared by the precipitation-molten salt method has wide application prospect in the aspect of photocatalytic hydrogen production due to the unique three-dimensional structure.
Description
Technical Field
The invention belongs to the field of inorganic materials, and relates to a preparation method of hexagonal pyramid CdS and application of the hexagonal pyramid CdS in the field of photocatalytic hydrogen production.
Background
CdS is used as a common direct band gap semiconductor, the forbidden band width of the CdS is 2.4eV, the direct band gap semiconductor has a high response range to sunlight, and the conduction band potential of the CdS is lower than the hydrogen production reduction potential, so that the CdS is researched as an excellent photocatalytic hydrogen production catalyst. The micro-morphology of CdS can greatly affect the photocatalytic activity of CdS. The photocatalyst with higher catalytic activity can be obtained by regulating and controlling the microscopic morphology of CdS.
The microstructure of CdS reported at present mainly has the shapes of particles, spheres, nano rods, nano wires and the like, but CdS with a hexagonal pyramid-like structure is not reported yet.
Disclosure of Invention
The invention aims to provide a preparation method of hexagonal pyramid-like CdS and application of the hexagonal pyramid-like CdS in the field of photocatalytic hydrogen production.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of quasi-hexagonal pyramid CdS, which uses urea and LiOH H 2 O is molten salt, the cadmium source solution and the sodium sulfide solution are reactants, and the precipitation-low temperature molten salt method is adopted to prepare the hexagonal pyramid-like CdS.
Preferably, the molar ratio of the cadmium source solution to the sodium sulfide solution is 1 (1-3).
Preferably, urea and LiOH H 2 The mass ratio of O is 1 (1-5).
Preferably, the cadmium source is cadmium acetate, cadmium nitrate, or cadmium chloride.
The preparation method of the hexagonal pyramid-like CdS specifically comprises the following steps:
1) mixing and stirring a sodium sulfide solution and a cadmium source solution, and filtering to obtain a precipitate;
2) mixing urea, LiOH & H 2 Mixing the precipitate obtained in the step 1) with O, and adding the mixture into a reaction kettle for reaction;
3) and after the reaction is finished, washing the reaction solution to be neutral, separating to obtain solid powder, and drying the solid powder to obtain the hexagonal pyramid-like CdS.
Preferably, in step 1), the temperature for mixing and stirring is 30 ℃ and the time is 3 h.
Preferably, in the step 2), the reaction temperature is 150-300 ℃, and the reaction time is 8-72 h.
The invention also relates toThe invention discloses the hexagonal pyramid-like CdS prepared by the method, and the 4h photocatalytic hydrogen production performance of the hexagonal pyramid-like CdS is 20.1 mmol/g -1 。
The invention also discloses application of the hexagonal pyramid-like CdS as a photocatalytic hydrogen production catalyst.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of quasi-hexagonal pyramid CdS, which comprises the steps of firstly, generating cadmium sulfide in a cadmium source solution and a sodium sulfide solution, and reacting the cadmium sulfide in urea and LiOH & H 2 In the O molten salt system, urea and LiOH & H are adopted 2 And O is molten salt, the molten salts with different melting points can be obtained by regulating the proportion between the O and the O, and meanwhile, the CdS is easy to grow under the alkaline condition, so that the CdS with better crystallinity can be easily obtained. The invention does not adopt any organic surfactant or surface modifier, does not need post treatment, has no environmental pollution and is easy for industrialized production.
The hexagonally pyramid-like CdS prepared by the precipitation-molten salt method has wide application prospect in the aspect of photocatalytic hydrogen production due to the unique three-dimensional structure.
Drawings
FIG. 1 is an XRD pattern of hexagonal pyramid like CdS as prepared in example 3 of the present invention;
FIG. 2 is an SEM image of hexagonal pyramid like CdS prepared in example 3 of the present invention;
FIG. 3 is a photo-catalytic hydrogen production performance diagram of hexagonal pyramid like CdS prepared in example 3 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that the terms "comprises" and "comprising," and any variations thereof, in the description of the present invention, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the invention discloses a preparation method of quasi-hexagonal pyramid CdS, which comprises the following steps: 0.1 to 0.3mol/L of sodium sulfide is weighed and dissolved in 50mL of water to prepare a sodium sulfate solution, the sodium sulfate solution is slowly dripped into 100mL of 0.1mol/L cadmium acetate solution and stirred for 3h at 50 ℃, and then the obtained precipitate is filtered. Taking 10g of urea and LiOH & H 2 O is mixed uniformly and the mixture and the product obtained before are ground uniformly by a mortar. Adding the mixture into a high-pressure reaction kettle, wherein the reaction temperature is 150 ℃ and 300 ℃, and the reaction time is 8-72 h. And after the reaction is finished, washing the obtained mixture with water until the pH value reaches 7.0-7.2, then carrying out suction filtration on the obtained sample, and drying the sample in a vacuum drying oven at 60 ℃ for 5 hours to obtain the hexagonal pyramid-like CdS sample.
Example 1
1) Weighing 0.1mol of sodium sulfide, dissolving the sodium sulfide in 50mL of water to prepare a sodium sulfide solution, slowly dripping the sodium sulfide solution into 100mL of 0.1mol/L cadmium acetate, stirring for 3h at 50 ℃, and filtering out the obtained precipitate;
2) mixing urea with LiOH & H 2 And mixing the O uniformly according to the mass ratio of 1:1, and grinding the mixture and the obtained precipitate uniformly by using a mortar. Adding the mixture into a high-pressure reaction kettle, wherein the reaction temperature is 150 ℃, and the reaction time is 72 h;
3) and after the reaction is finished, washing the obtained mixture with water until the pH value reaches 7.2, then carrying out suction filtration on the obtained sample, and drying the sample in a vacuum drying oven at 50 ℃ for 3h to obtain the prepared hexagonal pyramid-like CdS sample.
Example 2
1) Weighing 0.2mol of sodium sulfide, dissolving the sodium sulfide in 50mL of water to prepare a sodium sulfide solution, slowly dripping the sodium sulfide solution into 100mL of 0.1mol/L cadmium chloride solution, stirring for 3 hours at 50 ℃, and filtering out the obtained precipitate;
2) mixing urea with LiOH & H 2 And mixing the O uniformly according to the mass ratio of 1:3, and grinding the mixture and the obtained precipitate uniformly by using a mortar. Adding the mixture into a high-pressure reaction kettle, wherein the reaction temperature is 200 ℃, and the reaction time is 24 ℃;
3) and after the reaction is finished, washing the obtained mixture with water until the pH value reaches 7.1, then carrying out suction filtration on the obtained sample, and drying the sample in a vacuum drying oven at 50 ℃ for 3h to obtain the prepared hexagonal pyramid-like CdS sample.
Example 3
1) Weighing 0.2mol of sodium sulfide, dissolving the sodium sulfide in 50mL of water to prepare a sodium sulfide solution, slowly dripping the sodium sulfide solution into 100mL of 0.1mol/L cadmium nitrate solution, stirring for 3 hours at 50 ℃, and filtering out the obtained precipitate;
2) mixing urea with LiOH & H 2 And mixing the O uniformly according to the mass ratio of 1:4, and grinding the mixture and the obtained precipitate uniformly by using a mortar. Adding the mixture into a high-pressure reaction kettle, wherein the reaction temperature is 250 ℃, and the reaction time is 48 hours;
3) and after the reaction is finished, washing the obtained mixture with water until the pH value reaches 7.1, then carrying out suction filtration on the obtained sample, and drying the sample in a vacuum drying oven at 50 ℃ for 3h to obtain the prepared hexagonal pyramid-like CdS sample.
Example 4
1) Weighing 0.3mol of sodium sulfide, dissolving the sodium sulfide in 50mL of water to prepare a sodium sulfide solution, slowly dripping the sodium sulfide solution into 100mL of 0.1mol/L cadmium acetate solution, stirring for 3h at 50 ℃, and filtering out the obtained precipitate;
2) mixing urea with LiOH & H 2 And mixing the O uniformly according to the mass ratio of 1:5, and grinding the mixture and the obtained precipitate uniformly by using a mortar. Adding the mixture into a high-pressure reaction kettle, wherein the reaction temperature is 300 ℃, and the reaction time is 8 hours;
3) and after the reaction is finished, washing the obtained mixture with water until the pH value reaches 7.0, then carrying out suction filtration on the obtained sample, and drying the sample in a vacuum drying oven at 50 ℃ for 3h to obtain the prepared hexagonal pyramid-like CdS sample.
FIG. 1 is an XRD pattern of CdS prepared according to example 3 of the present invention, from which pure phase CdS with better product crystallinity can be seen.
FIG. 2 is an SEM image of a CdS sample prepared according to example 3, wherein the CdS prepared is hexagonal pyramid-like.
The specific test method for photocatalytic hydrogen production in the application adopts a 50W led lamp with the wavelength of 460nm as a light source and 0.35M Na 2 SO 3 And 0.25M NaS is used as a sacrificial agent, 10mg of prepared CdS is dispersed in 100mL of water, electromagnetic stirring is adopted to enable the sample to be in a stirring state, a constant-temperature water bath is adopted to keep the temperature of the reactor at 5 ℃, hydrogen production by water photolysis is carried out in a closed system, and the product is automatically detected once every 1h by adopting gas chromatography. The gas chromatography was carried out by Fuli model 9790 II.
As a result, referring to the hydrogen production performance graph of the hexagonal pyramid-shaped CdS sample prepared in example 3 shown in FIG. 3, it can be seen that the hydrogen production amount is 20.1mmol g after 4h photocatalytic hydrogen production performance test -1 And the hydrogen yield of the granular CdS obtained by dissolving 5mmol of cadmium acetate and 10mmol of thioacetamide in 50ml of deionized water and reacting at 150 ℃ for 24 hours by adopting a hydrothermal method is only 4.03mmol g of hydrogen after the granular CdS is subjected to photocatalytic reaction for 4 hours -1 The result shows that the prepared rhombic CdS has high photocatalytic hydrogen production activity.
TABLE 1 comparison table of photocatalytic hydrogen production performance of CdS prepared by different methods
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. The preparation method of the hexagonal pyramid-like CdS is characterized by comprising the following steps of:
1) mixing and stirring a sodium sulfide solution and a cadmium source solution, and filtering to obtain a precipitate;
2) mixing urea, LiOH & H 2 Mixing the precipitate in the step 1) with O, adding the mixture into a reaction kettle, and reacting for 8-72 h at the reaction temperature of 150-300 ℃;
3) and after the reaction is finished, washing the reaction solution to be neutral, separating to obtain solid powder, and drying the solid powder to obtain the hexagonal pyramid-like CdS.
2. The method for preparing hexagonally pyramidal CdS as claimed in claim 1, wherein the mixing and stirring temperature in step 1) is 30 ℃ and the time is 3 hours.
3. The method for preparing hexagonally pyramidal CdS as claimed in claim 1, wherein the molar ratio of the cadmium source solution to the sodium sulfide solution is 1 (1-3).
4. The method of preparing hexagonally pyramidal CdS as claimed in claim 1, wherein the reaction is carried out in the presence of urea and LiOH-H 2 The mass ratio of O is 1 (1-5).
5. The method of preparing hexagonally pyramidal CdS as claimed in claim 1, wherein the cadmium source is cadmium acetate, cadmium nitrate or cadmium chloride.
6. The hexagonal pyramid-like CdS prepared by the method as claimed in any one of claims 1 to 5, wherein the 4h photocatalytic hydrogen production performance of the hexagonal pyramid-like CdS is 20.1 mmol-g -1 。
7. Use of the hexagonally pyramidal CdS as claimed in claim 6 as a photocatalytic hydrogen production catalyst.
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| CN112158878A (en) | 2021-01-01 |
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