CN110665517B - Composite material prepared by carrying bismuth molybdate and cadmium sulfide on phlogopite/ZnO for concerted catalysis and preparation method thereof - Google Patents

Composite material prepared by carrying bismuth molybdate and cadmium sulfide on phlogopite/ZnO for concerted catalysis and preparation method thereof Download PDF

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CN110665517B
CN110665517B CN201910712418.8A CN201910712418A CN110665517B CN 110665517 B CN110665517 B CN 110665517B CN 201910712418 A CN201910712418 A CN 201910712418A CN 110665517 B CN110665517 B CN 110665517B
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刘孝恒
邱波
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Nanjing University of Science and Technology
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Abstract

The invention discloses a phlogopite/ZnO supported bismuth molybdate and cadmium sulfide composite material for concerted catalysis and a preparation method thereof. The composite material is microscopically in a shape of a sphere and a sheet which are connected, wherein spherical particles attached to a phlogopite sheet are connected solid zinc oxide spheres and bismuth molybdate hollow spheres coated by cadmium sulfide. The spherical metal oxide on the phlogopite sheet has the characteristics of good dispersity, large specific surface area and stable structure, and shows good photocatalytic performance; the cycle performance of the material is tested under the same condition, the degradation rate reaches 80% after 3 cycles, and the material has good cycle stability.

Description

Composite material prepared by carrying bismuth molybdate and cadmium sulfide on phlogopite/ZnO for concerted catalysis and preparation method thereof
Technical Field
The invention relates to a phlogopite/ZnO supported bismuth molybdate and cadmium sulfide composite material for concerted catalysis and a preparation method thereof, belonging to the field of nano material preparation.
Background
In recent years, due to water resource shortage caused by climate change and water resource pollution, the recovery and reuse of water resources have been receiving wide attention worldwide, and obtaining clean water is becoming an increasingly serious problem in countries where the economy and population are rapidly expanding. An important solution to the water resource problem is to recover and reuse the wastewater to ensure sustainable use of water resources, however, the wastewater contains persistent pollutants that are difficult to degrade, which cannot be completely eliminated by ordinary wastewater treatment methods, and which may cause serious harm to human beings and wild animals because they are difficult to degrade and have carcinogenicity. To ensure that the water does not contain persistent contaminants, numerous water treatment techniques have been employed, including adsorption, membrane separation and coagulation. However, these processes only concentrate or convert the contaminants from water to a solid state, thereby requiring additional cost to dispose of these secondary contaminants.
At present, photocatalytic degradation of organic pollutants is considered to be a promising treatment method, and semiconductor materials generate electrons and holes through illumination to remove oxidation and decompose pollutants, which is a very environment-friendly treatment mode. After more than forty years of research and development, people have achieved a series of important research results on the development of photocatalytic reaction mechanisms and reaction systems, but there are still many important scientific and technical problems to be solved from practical application, such as: preparing a photocatalyst capable of being excited by long-wavelength light; the photogenerated electron-hole should have suitable redox capability; inhibiting the recombination of photo-generated electrons and holes; has better stability against light corrosion; cheap and easily available materials, simple preparation method and the like.
Phlogopite is a type of 2: clay minerals of nature 1, the silicon atom of the tetrahedral centre usually being replaced by a trivalent cation (Fe) 3+ /Al 3+ ) While the trivalent aluminum ions in the octahedron are substituted by Fe 2+ /Mg 2+ By substitution, the vermiculite is rendered electronegative and hydrated cations (e.g. K) are present between the layers in order to balance the charge + ,Na + ,Li + ,Mg 2+ ,Ca 2+ ). Under the heating condition, the interlayer water is vaporized to leave a space for carrying sulfur. Therefore, the surface of the expanded vermiculite tetrahedron is mainly Mg 2+ And K + Therefore, the ion exchange material has the characteristics of cation exchange and anion adsorption.
Zinc oxide and cadmium sulfide are classical photocatalytic materials, but because the chemical properties of the zinc oxide and the cadmium sulfide are unstable, the zinc oxide and the cadmium sulfide can be dissolved by light during photocatalysis, and dissolved harmful metal ions have certain biological toxicity, so that the zinc oxide and the cadmium sulfide are rarely used as civil photocatalytic materials at present. But the stability can be effectively improved by compounding or doping with other semiconductors. Bismuth molybdate is a visible light catalyst with good performance, and has the characteristics of no toxicity, chemical stability, low price, adjustable electronic structure and the like, which are generally accepted by researchers. Zhan Shu et al prepared a composite of silver and Zinc oxide Nanoparticles using an angstromite as a carrier [ Zhan Shu Yi Zhang1, Qian Yang and Huanging Yang halo Nanotubes Supported Ag and ZnO Nanoparticles with synthetic Enhanced Antibacterial Activity [ J ]. Nanoscale Research Letter,2017,12(1) ], Lan Wang et al successfully synthesized a novel Layered Zinc Silicate nanosheet material using a liquid phase epitaxial growth method [ Lan Wang, Deltlew. Bahnemann, chemistry. two-Dimensional layer silicon with an extended cationic nanoparticle for use in a slurry deposition method [ CdS/ZnO 2 ] composite of silver and Zinc oxide Nanoparticles using an angstromite as a carrier [ CdS Shohan Shu & gt ] CdS/ZnO Nanoparticles are simply deposited by a CdS/CdS ion deposition method [ CdS J ] (CdS/CdS 8108, CdS/ZnO Nanoparticles are deposited into a solution of silver Nanoparticles for use CdS/ZnO heterostructures for soluble hydrocarbon production units [ J ]. International Journal of hydrocarbon Energy,2017,42(16):11356 and 11363 ]. The preparation method is complex and high in cost, and a catalyst with excellent performance, simple preparation and low cost is needed.
Disclosure of Invention
The invention aims to provide a composite material which is prepared by carrying out concerted catalysis on phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows:
the phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide composite material is of a microscopically connected spherical and flaky structure, wherein the spheres are bismuth molybdate hollow spheres and zinc oxide solid spheres, and the sheets are phlogopite sheets.
The preparation method of the phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide composite material comprises the following steps:
firstly, grinding phlogopite into powder by using a ball mill, placing the powder in a hydrochloric acid solution at a certain temperature, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
Fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
and sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a mixture with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethanol solution (1: 100g/ml) in which urea is dissolved with stirring, placing the resulting solution in a polytetrafluoroethylene-lined autoclave, washing the resulting sample, drying it and marking it as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
Compared with the existing catalyst, the catalyst has the advantages that: (1) the method comprises the steps of preparing a phlogopite-loaded zinc oxide nano material by a simple precipitation method, (2) preparing bismuth molybdate nanospheres with hollow sphere structures under a hydrothermal condition, and (3) degrading the dye by irradiating the material for 1 hour under visible light to obtain 95% rhodamine B, wherein the material has good photocatalytic performance. (4) The degradation rate of the material is still as high as 80% after 3 cycles of cycle performance test under the same condition, and the material has good cycle stability.
Drawings
FIG. 1 is a diagram of the synthetic mechanism of the present invention.
FIG. 2 is a graph showing the degradation performance of the bismuth molybdate and cadmium sulfide composite material with phlogopite/ZnO loading on the rhodamine B solution, prepared in example 1 of the present invention.
FIG. 3 is an XRD diffraction pattern of a phlogopite/ZnO supported bismuth molybdate and cadmium sulfide composite material according to example 1 of the present invention.
FIG. 4 is a transmission electron micrograph of a phlogopite/ZnO supported bismuth molybdate and cadmium sulfide composite material prepared in example 1 of the present invention, wherein a is a photograph which shows that bismuth molybdate particles are attached to phlogopite and have a size of about 10 nm; the b picture shows the sheet structure of the phlogopite obviously, and the phlogopite is about 50 nm.
Detailed Description
FIG. 1 is a diagram of the synthetic mechanism of the invention, in hydrogen peroxide, phlogopite is peeled into slices by oxygen released by hydrogen peroxide, then high-temperature calcination is carried out for secondary peeling, ZnO nanoparticles are loaded on the peeled vermiculite slices through a simple precipitation method, bismuth molybdate nanoparticles are loaded through a hydrothermal method, and finally cadmium sulfide is used for modification to prepare the phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide composite material.
The phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide composite material prepared by the invention has excellent electrochemical performance as a photocatalytic material, which is mainly due to the unique nano structure: firstly, zinc oxide and cadmium sulfide can effectively improve the stability of the zinc oxide and the cadmium sulfide by compounding with stable bismuth molybdate, so that the performance of the zinc oxide and the cadmium sulfide is improved; secondly, the heterojunction formed between the zinc oxide, bismuth molybdate and cadmium sulfide can effectively inhibit electron-hole recombination.
The phlogopite/ZnO loaded bismuth molybdate and cadmium sulfide composite material is prepared by the following steps:
firstly, grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
and sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a mixture with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethanol solution (1: 100g/ml) in which urea is dissolved with stirring, placing the resulting solution in a polytetrafluoroethylene-lined autoclave, washing the resulting sample, drying it and marking it as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
Example 1
Firstly, grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
And sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a mixture with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethyl alcohol solution (1: 100g/ml) dissolved with urea under stirring, placing the obtained solution in a polytetrafluoroethylene-lined autoclave, carrying out hydrothermal treatment for 24h, washing, drying and marking the obtained sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
Example 2
Firstly, grinding phlogopite into powder by using a ball mill, stirring the powder in a hydrochloric acid solution for 6 hours, and washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
Fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
and sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a mixture with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethyl alcohol solution (1: 100g/ml) dissolved with urea under stirring, placing the obtained solution in a polytetrafluoroethylene-lined autoclave, carrying out hydrothermal treatment for 18h, washing and drying the obtained sample, and marking the sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
Example 3
Grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
Secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
and sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a mixture with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethyl alcohol solution (1: 100g/ml) dissolved with urea under stirring, placing the obtained solution in a polytetrafluoroethylene-lined autoclave, carrying out hydrothermal treatment for 12h, washing and drying the obtained sample, and marking the sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
Example 4
Firstly, grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain a sodium phlogopite sample;
thirdly, calcining the sodium-modified phlogopite sample obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the sample in 30% hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
and sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in a solution with a molar ratio of 2: 1 of bismuth nitrate and ammonium molybdate for 10min, then adding an absolute ethyl alcohol solution (1: 100g/ml) dissolved with urea under stirring, and mixing Putting the obtained solution into a polytetrafluoroethylene-lined high-pressure kettle, carrying out hydrothermal treatment for 10 hours, washing, drying and marking the obtained sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 dispersing/ZnO/phlogopite in methanol solution of cadmium nitrate (molar ratio of zinc oxide to cadmium nitrate is 25: 1), ultrasonic treating for 10min, oven drying at 100 deg.C for 1h, dispersing the obtained sample in Na 2 Stirring the solution of S (the molar ratio of cadmium nitrate to sodium sulfide is 1: 3) for 30min, and marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.

Claims (7)

1. The composite material is characterized in that the phlogopite/ZnO supported bismuth molybdate and cadmium sulfide composite material is microscopically in a connected spherical and flaky structure, and the sample is formed by attaching bismuth molybdate and cadmium sulfide to phlogopite nanosheets; the bismuth molybdate is of a hollow sphere structure, the size of the bismuth molybdate is 10nm, and the composite material is prepared by the following steps:
firstly, grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain sodium phlogopite;
thirdly, calcining the sodium phlogopite obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the stripped phlogopite in a hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
sixthly, weighing the ZnO/phlogopite obtained in the fifth step, and dispersing the ZnO/phlogopite in bismuth nitrate and molybdenumPerforming ultrasonic treatment for 10min in an ethylene glycol solution of ammonium nitrate, wherein the molar ratio of bismuth nitrate to ammonium molybdate is 2: 1, adding an absolute ethanol solution containing urea under stirring, placing the obtained solution in a polytetrafluoroethylene-lined autoclave, washing the obtained sample, drying and marking the sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 ZnO/phlogopite dispersed in a solution of cadmium nitrate in methanol at a zinc oxide to cadmium nitrate molar ratio of 25: 1, performing ultrasonic treatment for 10min, drying at 100 ℃ for 1h, and dispersing the obtained sample in Na 2 And stirring the solution of S for 30min, wherein the molar ratio of cadmium nitrate to sodium sulfide is 1: 3, marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
2. A preparation method of a composite material with phlogopite/ZnO loaded with bismuth molybdate and cadmium sulfide for concerted catalysis comprises the following steps:
firstly, grinding phlogopite into powder by using a ball mill, placing the powder into a hydrochloric acid solution, stirring for 6 hours, washing, drying and grinding the obtained precipitate to obtain an acidified phlogopite sample;
secondly, mixing the acidified phlogopite obtained in the first step with Na 2 CO 3 Mixing the solutions, stirring for 1.0-2.0 h at room temperature, washing, drying and grinding the obtained precipitate to obtain sodium phlogopite;
thirdly, calcining the sodium phlogopite obtained in the second step for 4 hours to obtain stripped phlogopite, and placing the stripped phlogopite in a hydrogen peroxide solution to stir for 1 hour for secondary stripping;
fourthly, weighing the materials with the mass ratio of 1: 8: 8, dispersing peeled vermiculite, urea and zinc nitrate hexahydrate in deionized water, washing, drying and grinding the obtained light red precipitate;
fifthly, calcining the sample obtained in the fourth step, and marking the obtained sample as ZnO/phlogopite;
sixthly, weighing the ZnO/phlogopite obtained in the fifth step, dispersing the ZnO/phlogopite in ethylene glycol solution of bismuth nitrate and ammonium molybdate, and carrying out ultrasonic treatment for 10min, wherein the molar ratio of bismuth nitrate to ammonium molybdate is 2: 1, then adding anhydrous ethyl alcohol dissolved with urea under stirring Alcohol solution, placing the obtained solution in a polytetrafluoroethylene-lined autoclave, washing the obtained sample, drying and marking the obtained sample as Bi 2 MoO 6 ZnO/phlogopite;
seventh step, weighing the sample Bi obtained in the sixth step 2 MoO 6 ZnO/phlogopite dispersed in a methanol solution of cadmium nitrate, the molar ratio of zinc oxide to cadmium nitrate being 25: 1, performing ultrasonic treatment for 10min, drying at 100 ℃ for 1h, and dispersing the obtained sample in Na 2 And stirring the solution of S for 30min, wherein the molar ratio of cadmium nitrate to sodium sulfide is 1: 3, marking the obtained sample as CdS/Bi 2 MoO 6 ZnO/phlogopite.
3. The method of claim 2, wherein in the first step, p H of the solution is 5.
4. The method of claim 2, wherein in the second step, Na 2 CO 3 The concentration of the solution was 1.5 mol/L.
5. The method according to claim 2, wherein in the third step, the phlogopite is exfoliated by calcining at 500 ℃ and stirring in a water bath at 60 ℃ for 1 hour.
6. The method of claim 2, wherein in the fourth step, the reactants are stirred at 95 ℃ for 3.5 h.
7. The method of claim 2, wherein in the fifth step, the sample is calcined at 400 ℃ for 4 hours.
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