CN114950487B - Oryza Glutinosa strip-shaped CdS/Ni-CdV2O6Composite photocatalyst, preparation method and application thereof - Google Patents
Oryza Glutinosa strip-shaped CdS/Ni-CdV2O6Composite photocatalyst, preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 240000007594 Oryza sativa Species 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 239000000203 mixture Substances 0.000 claims abstract description 48
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 46
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 46
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 235000009566 rice Nutrition 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000007789 sealing Methods 0.000 claims abstract description 15
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 3
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 238000001291 vacuum drying Methods 0.000 claims description 19
- 241000209094 Oryza Species 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 description 12
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 10
- 238000000967 suction filtration Methods 0.000 description 10
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000010335 hydrothermal treatment Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229910021550 Vanadium Chloride Inorganic materials 0.000 description 5
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 5
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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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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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst, and a preparation method and application thereof, wherein the preparation method comprises the following steps: 1. according to the mol ratio of (0.5-0.8): (0.6-1.2): (0.1-0.3): (0.2-0.4) mixing C 4H6CdO4·2H2O、CH3CSNH2、VCl3 and Ni (NO 3)2·6H2 O) to obtain A, 2 adding the A into deionized water and stirring to uniformly mix the A to obtain B, 3 pouring the B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining, fixing the polytetrafluoroethylene lining in a reaction kettle, placing the polytetrafluoroethylene lining in a homogeneous reaction instrument, reacting the polytetrafluoroethylene lining for 12-16 hours at 120-160 ℃,4 cooling the polytetrafluoroethylene lining to room temperature after the hydrothermal reaction is finished, pouring out the solution, washing and suction filtering the solution, collecting the product, drying and grinding the product to obtain a precursor, 5 adding CdS and the precursor into distilled water according to the molar ratio (1-4) (0.03-0.06) to obtain a solution D, 6 firstly moving the solution D to the reaction kettle to react for 0.5-2 hours at 100-160 ℃, cooling the reaction kettle to room temperature, and 7 washing the reaction kettle with water, drying and grinding the reaction kettle to obtain the CdS/Ni-CdV 2O6 composite photocatalyst.
Description
Technical Field
The invention relates to a photocatalyst material, in particular to a glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst, a preparation method and application thereof.
Background
In recent years, with the increasing severity of global environmental pollution and the emergence of energy crisis, the environment and energy have become topics of great concern. Photocatalysis is one of the effective means for treating the environment and solving the energy, and development of a novel photocatalyst which is pollution-free, efficient and sustainable is becoming a problem to be solved. Therefore, in order to make more effective use of sunlight, it is very interesting to study a catalyst having high photocatalytic activity under visible light.
The forbidden bandwidth of CdS is 2.42eV, the conduction band potential is slightly negative than the hydrogen electrode potential, the valence band potential is slightly positive than the oxygen electrode potential, and the CdS can be excited by visible light to decompose water or organic pollutants in water body by photocatalysis, has high visible light activity, and has the advantages of low preparation cost, simple process and easy formation of size-adjustable nanocrystals, and can be widely applied to the field of photocatalysis. But also limits its practical application due to the presence of some drawbacks: (1) The stability is poor, and the anodic decomposition potential in the photocatalytic reaction is only 0.32eV, so that the photocatalytic reaction is easy to generate a photo-corrosion phenomenon, and the photocatalytic efficiency is reduced; (2) The exposed nano particles have large surface area and high surface free energy, and single nano particles are easy to agglomerate in the photocatalysis process.
In the field of photocatalysis, researchers have modified CdS catalytic materials by a variety of means, including noble metal modification, metal oxide loading, semiconductor recombination, transition metal ion doping, dye sensitization, and the like.
Disclosure of Invention
The invention aims to provide a polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst, a preparation method and application thereof, and the prepared CdS/Ni-CdV 2O6 composite photocatalyst has good hydrogen production activity and stability.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
A preparation method of a Oryza Glutinosa strip CdS/Ni-CdV 2O6 composite photocatalyst comprises the following steps:
Step 1, a molar ratio (0.5-0.8): (0.6-1.2): (0.1-0.3): (0.2-0.4) mixing C 4H6CdO4·2H2O、CH3CSNH2、VCl3 and Ni (NO 3)2·6H2 O to obtain a mixture A;
step 2, according to the proportion (1.4-2.7 g): (40-60 ml) adding the mixture A into deionized water, and fully stirring to uniformly mix the mixture A to obtain a solution B;
Step 3, pouring the solution B into a polytetrafluoroethylene lining and sealing, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, and placing the reaction kettle in a homogeneous phase reactor for reaction for 12-16 h at the temperature of 120-160 ℃;
Step 4, after the hydrothermal reaction of the step 3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, alternately washing with water and filtering until the water is completely washed, collecting a product, then drying the product in vacuum, and finally fully grinding the product to obtain a precursor;
step 5, firstly, according to the mole ratio (1-4): (0.03-0.06) mixing CdS and precursor to obtain a mixture C, and then proportioning (1.03-4.06 g): (30-45 ml) adding the mixture C into distilled water, and then dispersing by using ultrasonic vibration to obtain a solution D;
Step 6, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 0.5-2 h at the temperature of 100-160 ℃, and then naturally cooling to room temperature;
And 7, taking out a sample from the microwave reaction kettle, washing with water and alcohol, and then drying in vacuum and grinding to obtain the CdS/Ni-CdV 2O6 composite photocatalyst.
Further, the stirring in the step 2 adopts a magnetic stirrer to stir for 40-60 min at room temperature.
Further, the filling ratio of the solution B in the polytetrafluoroethylene lining in the step 3 is 40-60%.
Further, the vacuum drying in the step 4 and the step 7 is carried out at the temperature of 60-80 ℃ for 6-8 hours.
Further, the power of the ultrasonic wave in the step 5 is 100w-150w, and the vibration dispersing time is 10-20 min.
Further, the preparation method of CdS in the step 5 comprises the following steps:
Step 5.1, the molar ratio (0.5-0.9): (0.6-1.0) weighing C 4H6CdO4·2H2 O and CH 3CSNH2 and mixing to obtain a mixture E;
step 5.2, firstly, according to the volume ratio (1-5): 1 mixing ethylenediamine and ethylene glycol to obtain solution F, and then mixing according to the proportion (1.1-2.0 g): (30-60 ml) adding the mixture E into the solution F and stirring thoroughly until a transparent solution G is obtained;
Step 5.3, pouring the solution G into a polytetrafluoroethylene lining and sealing, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 5-8 hours at 160-180 ℃;
And 5.4, after the hydrothermal reaction of the step 5.3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, alternately washing with water and filtering until the water is completely washed, collecting a product, vacuum drying the product, and finally grinding the product into fine powder to obtain the CdS material.
Further, the stirring in the step 5.2 adopts a magnetic stirrer with the rotating speed of 500-800 r/min, and the stirring time is 0.5-2 h.
Further, the vacuum drying in the step 5.4 is performed at the temperature of 60-80 ℃ for 6-8 hours.
A CdS/Ni-CdV 2O6 composite photocatalyst is in the shape of Oryza Glutinosa strip.
The invention also protects the application of the CdS/Ni-CdV 2O6 composite photocatalyst as a photolytic water hydrogen production catalyst.
The invention has the following beneficial effects:
The preparation method disclosed by the invention adopts a hydrothermal method to synthesize the CdS/Ni-CdV 2O6 composite photocatalyst, has the advantages of simple reaction process, no need of large-scale equipment and harsh reaction conditions, short time consumption, low-cost and easily available raw materials, low cost and high yield, and is environment-friendly, and compared with a solid-phase sintering method, the preparation method disclosed by the invention does not generate pollution gas. The prepared CdS/Ni-CdV 2O6 composite photocatalyst has single chemical component, high purity and uniform morphology, and the polished glutinous rice strip structure has good photochemical performance, and can at least maintain the stability of 53h under the irradiation of an argon lamp. Meanwhile, the hydrogen production activity is very high.
The invention utilizes self-made CdS, which has better crystallinity and higher purity than commercial CdS, and prepares the CdS with excellent performance by changing the addition amount in the preparation process, thereby having positive significance for the subsequent preparation of the high-purity CdS/Ni-CdV 2O6 composite photocatalyst.
Drawings
Fig. 1: an X-ray diffraction analysis chart of the CdS/Ni-CdV 2O6 composite photocatalyst prepared in the embodiment 1 of the invention;
Fig. 2: SEM (scanning electron microscope) picture of CdS/Ni-CdV 2O6 composite photocatalyst prepared in example 1 of the invention;
Fig. 3: the hydrogen production diagram of the CdS/Ni-CdV 2O6 composite photocatalyst prepared in the embodiment 1 of the invention;
Fig. 4: the hydrogen production cycle chart of the CdS/Ni-CdV 2O6 composite photocatalyst prepared in the embodiment 1 of the invention;
Detailed Description
The following examples are given to illustrate the present invention in further detail, but are not to be construed as limiting the invention thereto.
Example 1
Step 1, according to the mole ratio of 0.5:0.6, weighing cadmium acetate C 4H6CdO4·2H2 O and thioacetamide CH 3CSNH2, and mixing to obtain a mixture E;
step 2, firstly, according to the volume ratio of 1:1, mixing ethylenediamine and ethylene glycol to obtain a solution F, adding 1.1G of the mixture E into 30ml of the solution F, and stirring for 0.5h by using a magnetic stirrer at a rotating speed of 500r/min to obtain a transparent solution G;
Step 3, pouring the solution G into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 60%, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 5 hours at 160 ℃;
step 4, after the hydrothermal reaction of the step 3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and 3 times of alternate suction filtration, vacuum drying the product for 6 hours at 60 ℃, and finally grinding the product into fine powder to obtain a CdS material;
step 5, according to the mole ratio of 0.5:0.6:0.1:0.2 cadmium acetate C 4H6CdO4·2H2 O, thioacetamide CH 3CSNH2, vanadium chloride VCl 3 and nickel nitrate hexahydrate Ni (NO 3)2·6H2 O) were mixed to obtain mixture A;
step 6, adding 1.4g of the mixture A into 40ml of deionized water, and stirring for 40min at room temperature by adopting a magnetic device to obtain a solution B;
Step 7, pouring the solution B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 40%, fixing the polytetrafluoroethylene lining filled with the solution B into a reaction kettle, placing the reaction kettle into a homogeneous phase reactor, and reacting for 12 hours at 120 ℃;
step 8, after the hydrothermal reaction of the step 7 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and alternate suction filtration, vacuum drying the product at 60 ℃ for 6 hours, and fully grinding the product to obtain a precursor;
Step 9, firstly, according to the mole ratio of 1:0.03 mixing CdS and a precursor to obtain a mixture C, adding 1.03g of the mixture C into 30ml of distilled water, and vibrating and mixing for 10min under the condition that the ultrasonic power is 100w to obtain a solution D;
Step 10, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 0.5h at 100 ℃, and then naturally cooling to room temperature;
And 11, taking out a sample from the reaction kettle, washing with distilled water and ethanol, vacuum drying at 60 ℃ for 6 hours, and grinding the dried sample to obtain the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst.
From FIG. 1, it can be seen that CdS corresponds to the card PDF#77-2306, ni-CdV 2O6 corresponds to the card PDF#27-1052 and no other impurity peaks appear, which indicates that the crystallinity of the CdS/Ni-CdV 2O6 composite photocatalyst is good.
As can be seen from FIG. 2, the CdS/Ni-CdV 2O6 composite photocatalyst prepared in example 1 is in the shape of a polished glutinous rice strip with uniform morphology, and the structure not only reduces the possibility of nanoparticle aggregation in CdS, but also has good stability; and the charge transfer rate of CdS is improved, so that the photo-corrosion phenomenon of CdS is inhibited, and the photo-catalytic hydrogen production performance of the CdS/Ni-CdV 2O6 composite photocatalyst material is improved.
As can be seen from FIG. 3, the hydrogen yield of the CdS/Ni-CdV 2O6 composite photocatalyst was 4372. Mu. Mol g -1h-1, whereas the hydrogen yield of CdS as photocatalyst was only 49.3. Mu. Mol g -1h-1.
From FIG. 4, it can be seen that CdS/Ni-CdV 2O6 is capable of maintaining 53h stability without much change in hydrogen production performance.
Example 2
Step 1, according to the mole ratio of 0.6:0.7, weighing cadmium acetate C 4H6CdO4·2H2 O and thioacetamide CH 3CSNH2, and mixing to obtain a mixture E;
Step 2, firstly, according to the volume ratio of 2:1, mixing ethylenediamine and ethylene glycol to obtain a solution F, adding 2.0G of the mixture E into 60ml of the solution F, and stirring for 1h by using a magnetic stirrer at a rotating speed of 600r/min to obtain a transparent solution G;
Step 3, pouring the solution G into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 40%, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 6 hours at 170 ℃;
step 4, after the hydrothermal reaction of the step3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and 3 times of alternate suction filtration, vacuum drying the product at 70 ℃ for 7 hours, and finally grinding the product into fine powder to obtain a CdS material;
Step 5, according to the mole ratio of 0.6:0.8:0.2:0.3 mixing cadmium acetate C 4H6CdO4·2H2 O, thioacetamide CH 3CSNH2, vanadium chloride VCl 3 and nickel nitrate hexahydrate Ni (NO 3)2·6H2 O to obtain mixture A;
Step 6, adding 1.8g of the mixture A into 45ml of deionized water, and stirring for 50min at room temperature by adopting a magnetic device to obtain a solution B;
step 7, pouring the solution B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 45%, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 13h at 140 ℃;
step 8, after the hydrothermal reaction of the step 7 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and alternate suction filtration, then drying the product in vacuum at 70 ℃ for 7 hours, and finally fully grinding the product to obtain a precursor;
Step 9, firstly, according to the mole ratio of 2:0.04 mixing CdS and a precursor to obtain a mixture C, adding 1.73g of the mixture C into 35ml of distilled water, and vibrating and mixing for 15min under the condition that ultrasonic power is 120w to obtain a solution D;
Step 10, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 1h at 120 ℃, and then naturally cooling to room temperature;
and 11, taking out a sample from the reaction kettle, washing with distilled water and ethanol, vacuum drying at 70 ℃ for 7 hours, and grinding the dried sample to obtain the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst.
Example 3
Step 1, according to the mole ratio of 0.7:0.8, weighing cadmium acetate C 4H6CdO4·2H2 O and thioacetamide CH 3CSNH2, and mixing to obtain a mixture E;
Step 2, firstly, according to the volume ratio of 3:1, mixing ethylenediamine and ethylene glycol to obtain a solution F, adding 1.5G of the mixture E into 40ml of the solution F, and stirring for 1.5h by using a magnetic stirrer at a rotating speed of 700r/min to obtain a transparent solution G;
step 3, pouring the solution G into a polytetrafluoroethylene lining and sealing the polytetrafluoroethylene lining, wherein the filling ratio is 50%, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 7 hours at 180 ℃;
Step 4, after the hydrothermal reaction of the step 3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and 3 times of alternate suction filtration, vacuum drying the product for 8 hours at 80 ℃, and finally grinding the product into fine powder to obtain a CdS material;
Step 5, according to the mole ratio of 0.7:1:0.3:0.4 cadmium acetate C 4H6CdO4·2H2 O, thioacetamide CH 3CSNH2, vanadium chloride VCl 3 and nickel nitrate hexahydrate Ni (NO 3)2·6H2 O) were mixed to give mixture A;
step 6, adding 2.2g of the mixture A into 50ml of deionized water, and stirring for 60min at room temperature by adopting a magnetic device to obtain a solution B;
step 7, pouring the solution B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 50%, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 14h at 150 ℃;
Step 8, after the hydrothermal reaction of the step 7 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and alternate suction filtration, vacuum drying the product for 8 hours at 80 ℃, and fully grinding the product to obtain a precursor;
Step 9, firstly, according to the mole ratio of 3: mixing CdS and a precursor to obtain a mixture C at 0.05, adding 2.5g of the mixture C into 40ml of distilled water, and vibrating and mixing for 20min under the condition that the ultrasonic power is 140w to obtain a solution D;
Step 10, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 1.5 hours at 140 ℃, and then naturally cooling to room temperature;
and 11, taking out a sample from the reaction kettle, washing with distilled water and ethanol, vacuum drying at 80 ℃ for 8 hours, and grinding the dried sample to obtain the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst.
Example 4
Step 1, according to the mole ratio of 0.9:1, weighing cadmium acetate C 4H6CdO4·2H2 O and thioacetamide CH 3CSNH2, and mixing to obtain a mixture E;
Step 2, firstly, according to the volume ratio of 5:1, mixing ethylenediamine and ethylene glycol to obtain a solution F, adding 1.8g of the mixture E into 50ml of the solution E, and stirring for 2 hours at a speed of 800r/min by using a magnetic stirrer to obtain a transparent solution F;
Step 3, pouring the solution G into a polytetrafluoroethylene lining and sealing the polytetrafluoroethylene lining, wherein the filling ratio is 60%, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 5 hours at 180 ℃;
Step 4, after the hydrothermal reaction of the step3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and 3 times of alternate suction filtration, vacuum drying the product for 6 hours at 80 ℃, and finally grinding the product into fine powder to obtain a CdS material;
Step 5, according to the mole ratio of 0.8:1.2:0.3:0.4 cadmium acetate C 4H6CdO4·2H2 O, thioacetamide CH 3CSNH2, vanadium chloride VCl 3 and nickel nitrate hexahydrate Ni (NO 3)2·6H2 O) were mixed to give mixture A;
step 6, adding 2.7g of the mixture A into 60ml of deionized water, and stirring for 40min at room temperature by adopting a magnetic device to obtain a solution B;
step 7, pouring the solution B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 60%, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 16 hours at 160 ℃;
step 8, after the hydrothermal reaction of the step 7 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and alternate suction filtration, then drying the product in vacuum for 8 hours at 70 ℃, and finally fully grinding the product to obtain a precursor;
Step 9, firstly, according to the mole ratio of 4:0.06 mixing CdS and a precursor to obtain a mixture C, adding 4.06g of the mixture C into 45ml of distilled water, and vibrating and mixing for 10min under the condition that ultrasonic power is 150w to obtain a solution;
Step 10, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 2 hours at 160 ℃, and then naturally cooling to room temperature;
And 11, taking out a sample from the reaction kettle, washing with distilled water and ethanol, vacuum drying at 80 ℃ for 6 hours, and grinding the dried sample to obtain the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst.
Example 5
Step 1, according to the mole ratio of 0.8:9, weighing cadmium acetate C 4H6CdO4·2H2 O and thioacetamide CH 3CSNH2, and mixing to obtain a mixture E;
Step 2, firstly, according to the volume ratio of 4:1, mixing ethylenediamine and ethylene glycol to obtain a solution F, adding 1.3g of the mixture E into 45ml of the solution E, and stirring for 0.5h by using a magnetic stirrer at a rotating speed of 700r/min to obtain a transparent solution F;
step 3, pouring the solution G into a polytetrafluoroethylene lining and sealing the polytetrafluoroethylene lining, wherein the filling ratio is 40%, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 8 hours at 160 ℃;
Step 4, after the hydrothermal reaction of the step3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and 3 times of alternate suction filtration, vacuum drying the product at 60 ℃ for 7 hours, and finally grinding the product into fine powder to obtain a CdS material;
Step 5, according to the mole ratio of 0.8:0.9:0.2:0.3 mixing cadmium acetate C 4H6CdO4·2H2 O, thioacetamide CH 3CSNH2, vanadium chloride VCl 3 and nickel nitrate hexahydrate Ni (NO 3)2·6H2 O to obtain mixture A;
Step 6, adding 2.0g of the mixture A into 55ml of deionized water, and stirring for 50min at room temperature by adopting a magnetic device to obtain a solution B;
Step 7, pouring the solution B into a polytetrafluoroethylene lining, sealing the polytetrafluoroethylene lining with the filling ratio of 50%, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, placing the reaction kettle in a homogeneous phase reactor, and reacting for 0.5h at 150 ℃;
Step 8, after the hydrothermal reaction of the step 7 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, collecting a product after 3 times of water washing and alternate suction filtration, vacuum drying the product at 60 ℃ for 7 hours, and fully grinding the product to obtain a precursor;
Step 9, firstly, according to the mole ratio of 4: mixing CdS and a precursor to obtain a mixture C at 0.05, adding 3.23g of the mixture C into 45ml of distilled water, and vibrating and mixing for 20min under the condition that the ultrasonic power is 110w to obtain a solution D;
Step 10, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal treatment for 2 hours at 160 ℃, and then naturally cooling to room temperature;
and 11, taking out a sample from the reaction kettle, washing with distilled water and ethanol, vacuum drying at 60 ℃ for 7 hours, and grinding the dried sample to obtain the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst.
Claims (9)
1. The preparation method of the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst is characterized by comprising the following steps of:
step 1, a molar ratio (0.5-0.8): (0.6-1.2): (0.1 to 0.3): (0.2-0.4) mixing C 4H6CdO4·2H2O、CH3CSNH2、VCl3 and Ni (NO 3)2·6H2 O to obtain a mixture A;
Step 2, according to the proportion (1.4-2.7 g): (40-60 ml) adding the mixture A into deionized water, and fully stirring to uniformly mix the mixture A to obtain a solution B;
Pouring the solution B into a polytetrafluoroethylene lining, sealing, fixing the polytetrafluoroethylene lining filled with the solution B in a reaction kettle, and placing the reaction kettle in a homogeneous phase reactor for reaction for 12-16 hours at the temperature of 120-160 ℃;
Step 4, after the hydrothermal reaction of the step 3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, alternately washing with water and filtering until the water is completely washed, collecting a product, then drying the product in vacuum, and finally fully grinding the product to obtain a precursor;
Step 5, firstly, according to the mole ratio (1-4): (0.03-0.06) mixing CdS and a precursor to obtain a mixture C, and then mixing the mixture C with the precursor according to the proportion (1.03-4.06 g): (30-45 ml) adding the mixture C into distilled water, and dispersing by using ultrasonic vibration to obtain a solution D, wherein the preparation method of CdS comprises the following steps:
Step 5.1, a molar ratio (0.5-0.9): (0.6-1.0) weighing C 4H6CdO4·2H2 O and CH 3CSNH2, and mixing to obtain a mixture E;
Step 5.2, firstly, according to the volume ratio (1-5): 1, mixing ethylenediamine and ethylene glycol to obtain a solution F, and then mixing the solution F with the solution F according to the ratio (1.1-2.0 g): (30-60 ml) adding the mixture E into the solution F and fully stirring until a transparent solution G is obtained;
step 5.3, pouring the solution G into a polytetrafluoroethylene lining and sealing, fixing the polytetrafluoroethylene lining filled with the solution G in a reaction kettle, and placing the reaction kettle in a homogeneous phase reactor for reacting for 5-8 hours at 160-180 ℃;
Step 5.4, after the hydrothermal reaction of step 5.3 is finished, naturally cooling the reaction kettle to room temperature, pouring out the solution in the reaction kettle, alternately washing with water and suction filtering until the water is completely washed, collecting a product, vacuum drying the product, and finally grinding the product into fine powder to obtain the CdS material;
Step 6, firstly transferring the solution D into a microwave reaction kettle, performing microwave hydrothermal reaction for 0.5-2 h at the temperature of 100-160 ℃, and then naturally cooling to room temperature;
And 7, taking out a sample from the microwave reaction kettle, washing with water and alcohol, and then drying in vacuum and grinding to obtain the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst.
2. The preparation method of the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the stirring in the step 2 is performed by a magnetic stirrer at room temperature for 40-60 min.
3. The preparation method of the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the filling ratio of the solution B in the polytetrafluoroethylene lining in the step 3 is 40% -60%.
4. The method for preparing the polished glutinous rice strip-shaped CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the vacuum drying in the step 4 and the step 7 is carried out at the temperature of 60-80 ℃ for 6-8 hours.
5. The method for preparing the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the power of ultrasonic waves in the step 5 is 100w-150w, and the vibration dispersion time is 10-20 min.
6. The method for preparing the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the stirring in the step 5.2 is performed by a magnetic stirrer with the rotating speed of 500-800 r/min, and the stirring time is 0.5-2 h.
7. The method for preparing the polished glutinous rice strip CdS/Ni-CdV 2O6 composite photocatalyst according to claim 1, wherein the vacuum drying in the step 5.4 is performed at 60-80 ℃ for 6-8 hours.
8. A CdS/Ni-CdV 2O6 composite photocatalyst prepared by the preparation method according to any one of claims 1 to 7.
9. The use of the CdS/Ni-CdV 2O6 composite photocatalyst according to claim 8 as a photolytic water production hydrogen catalyst.
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