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 PDFInfo
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- 229910052628 phlogopite Inorganic materials 0.000 title claims abstract description 124
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 44
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 26
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 6
- 230000002153 concerted effect Effects 0.000 title claims abstract description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 178
- 239000011787 zinc oxide Substances 0.000 claims abstract description 89
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims description 41
- 238000001035 drying Methods 0.000 claims description 34
- 238000000227 grinding Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 32
- 239000011734 sodium Substances 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 24
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 24
- 239000002244 precipitate Substances 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 229910052902 vermiculite Inorganic materials 0.000 claims description 11
- 239000010455 vermiculite Substances 0.000 claims description 11
- 235000019354 vermiculite Nutrition 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 9
- 239000011609 ammonium molybdate Substances 0.000 claims description 9
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims description 9
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002135 nanosheet Substances 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 6
- 238000009210 therapy by ultrasound Methods 0.000 claims 4
- 235000019441 ethanol Nutrition 0.000 claims 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 239000012798 spherical particle Substances 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 8
- 238000000643 oven drying Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000010335 hydrothermal treatment Methods 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910001923 silver oxide Inorganic materials 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 206010040844 Skin exfoliation Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000004110 Zinc silicate Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
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- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000002077 nanosphere Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100001239 persistent pollutant Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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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
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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