CN108940332B - High-activity MoS2/g-C3N4/Bi24O31Cl10Preparation method of composite photocatalyst - Google Patents
High-activity MoS2/g-C3N4/Bi24O31Cl10Preparation method of composite photocatalyst Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 63
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 63
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 11
- 230000000694 effects Effects 0.000 title claims abstract description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 126
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 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 abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 4
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 4
- 238000009841 combustion method Methods 0.000 claims abstract description 4
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 51
- 239000007787 solid Substances 0.000 claims description 44
- 239000011259 mixed solution Substances 0.000 claims description 34
- 238000009210 therapy by ultrasound Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 9
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000006303 photolysis reaction Methods 0.000 abstract description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 11
- 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 11
- 229940043267 rhodamine b Drugs 0.000 description 11
- 239000004098 Tetracycline Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 229960002180 tetracycline Drugs 0.000 description 8
- 229930101283 tetracycline Natural products 0.000 description 8
- 235000019364 tetracycline Nutrition 0.000 description 8
- 150000003522 tetracyclines Chemical class 0.000 description 8
- 238000005215 recombination Methods 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 229960004989 tetracycline hydrochloride Drugs 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 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
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- B01J27/24—Nitrogen compounds
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- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention belongs to the technical field of new materials, new energy utilization and environmental pollution treatment, and relates to high-activity MoS2/g‑C3N4/Bi24O31Cl10A preparation method of a composite photocatalyst. Bi is prepared by taking bismuth nitrate, ammonium chloride and citric acid as raw materials and adopting an improved solution combustion method24O31Cl10(ii) a g-C is prepared from melamine and acetic acid by one-step thermal polymerization method3N4(ii) a Ammonium molybdate and thiourea are used as raw materials, dimethylformamide is used as a solvent, and a hydrothermal method is adopted to prepare MoS2(ii) a Subjecting the Bi subjected to ultrasonic dispersion treatment24O31Cl10And g-C3N4、MoS2And (3) carrying out ultrasonic mixing reaction in a methanol solution, washing, centrifuging and drying to obtain the composite photocatalyst. The method is simple and easy to implement, low in cost and good in repeatability, and has wide application prospects in the fields of photolysis of water, photocatalytic oxidation of environmental pollutants and the like.
Description
Technical Field
The invention belongs to the technical field of new materials, new energy utilization and environmental pollution treatment, and relates to high-activity MoS2/g-C3N4/Bi24O31Cl10A preparation method of a composite photocatalyst.
Background
With the increasing increase of the environmental pollution problem, the photocatalytic technology receives more and more attention in the aspects of hydrogen production by photolysis and organic pollutant degradation. Wherein, TiO2Has the advantages of low cost, good photocatalytic stability, high photocatalytic efficiency and the like, and is a common material in the field of photocatalysis. But TiO 22The photocatalyst can only be excited by ultraviolet light due to the wide forbidden band width of about 3.1eV, and the ultraviolet light only accounts for about 5% of the solar spectrum, so that the photocatalyst has low utilization rate of sunlight and limits the application of the photocatalyst in the aspect of environmental management to a certain extent. Therefore, to make the most of the solar energy, the development and research of new catalysts that can be excited by visible light are the focus and focus of research.
The bismuth-based catalyst is a novel visible light catalyst which is most concerned at present, has become good in the aspect of controlling environmental pollution, and is increasingly popular with researchers at home and abroad. The most outstanding advantage of the method is that the forbidden band width is narrow, and the characteristic is favorable for photocatalytic degradation of organic pollutants in the environment under visible light. Wherein Bi24O31Cl10As an oxygen-enriched bismuth-based catalyst, the bismuth-based catalyst has the following advantages: the forbidden band width is small, about 2.8eV, and the energy can be excited by visible light; the chemical and physical stability is good; has a unique crystal structure and high quantum efficiency, and is becoming a research hotspot in recent years. Such as Jin et al, by hydrothermal method to prepare Bi with thickness of 300nm and width of 1-3 μm24O31Cl10Photocatalyst, Bi in comparison with BiOCl24O31Cl10In the visible light (>420 nm) can better absorb visible light under the irradiation and can effectively activate molecular oxygen to generate O2·-Thereby enhancing Bi24O31Cl10The photocatalytic activity of visible light. YIn and the like adopt a method of combining hydrothermal treatment and heat treatment to prepare Bi24O31Cl10The nano-sheet is used for degrading tetracycline hydrochloride, and the degradation rate of the tetracycline hydrochloride reaches over 80 percent when the nano-sheet is illuminated for 150min under visible light. However, pure Bi24O31Cl10The photo-electron holes are easy to recombine, the specific surface area is small, the photocatalytic activity is low, and the actual industrial application cannot be met, therefore, various measures are needed to improve the photocatalytic activity, for example, different semiconductor materials with matched energy band positions are recombined to form a heterojunction, and the recombination rate of electrons and holes in the materials can be reduced.
MoS2The graphene-like hexagonal close-packed layered structure material can absorb photons with visible light frequency, has high edge potential of a conduction band and a valence band, can effectively enhance the absorption capacity of light when being compounded with other photocatalysts, and can play a role in rapidly transmitting electrons. And g-C3N4Is a polymer semiconductor with a structure similar to graphene, and C, N atoms are hybridized by sp2 to form highly delocalized piA conjugated system. g-C3N4The material has the advantages of wide source, low price, chemical stability and the like of polymer materials, has certain absorption to visible light, and has better photocatalytic performance. And MoS2And g-C3N4Position of valence and conduction bands and Bi24O31Cl10Can be well matched to form a heterojunction, on one hand, enhances Bi24O31Cl10Can effectively reduce Bi24O31Cl10Recombination rate of internal electrons and holes, and in Bi24O31Cl10Thin layer MoS coated on particle surface2And g-C3N4The nano-sheet increases the specific surface area of the catalyst, and increases the pre-adsorption amount of the catalyst surface in organic pollutants, thereby being beneficial to improving the efficiency of photocatalytic reaction.
In view of the foregoing, there is a need for providing a MoS2/g-C3N4/Bi24O31Cl10A preparation method of a heterojunction photocatalyst.
Disclosure of Invention
To solve the above problems, the present invention provides a high activity MoS2/g-C3N4/Bi24O31Cl10A preparation method of a composite photocatalyst.
The preparation method of the invention firstly uses bismuth nitrate, ammonium chloride and citric acid as raw materials and adopts an improved solution combustion method to prepare Bi24O31Cl10Then ultrasonically dispersing in a methanol solution; secondly, melamine and acetic acid are used as raw materials, and a one-step thermal polymerization method is adopted to prepare g-C3N4Then ultrasonically dispersing in a methanol solution; ammonium molybdate and thiourea are used as raw materials, dimethylformamide is used as a solvent, and a hydrothermal method is adopted to prepare MoS2And carrying out ultrasonic dispersion treatment in a methanol solution. Finally, the Bi subjected to ultrasonic dispersion treatment24O31Cl10And g-C3N4、MoS2Ultrasonically mixing the mixture in a methanol solution for full reaction, washing, centrifuging and drying to obtain the MoS2/g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
The technical scheme of the invention is as follows:
high-activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of the composite photocatalyst comprises the following steps:
(1) bi is prepared by taking bismuth nitrate, ammonium chloride and citric acid as raw materials and adopting an improved solution combustion method24O31Cl10
Mixing bismuth nitrate pentahydrate and citric acid, and dissolving in dilute nitric acid to obtain a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid, wherein the molar ratio of bismuth nitrate pentahydrate to citric acid is 1: 2; dissolving ammonium chloride in distilled water until the ammonium chloride is completely dissolved to obtain an ammonium chloride solution; under the condition of stirring, adding an ammonium chloride solution into a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid, wherein the molar ratio of the bismuth nitrate pentahydrate to the ammonium chloride is 1: 1, uniformly mixing until the solution is in a clear state, and adjusting the pH value of the solution to 5-6 by using ammonia water; heating and stirring for 3-4 h at 60-80 ℃, and then calcining for 3h at 600 ℃ to obtain light yellow powder, namely pure Bi24O31Cl10；
(2) g-C is prepared from melamine and acetic acid by one-step thermal polymerization method3N4
Uniformly mixing melamine and acetic acid according to a molar ratio of 10:1, calcining for 2 hours at 500 ℃ to obtain light yellow powder, namely pure g-C3N4；
(3) Ammonium molybdate and thiourea are used as raw materials, dimethylformamide is used as a solvent, and a hydrothermal method is adopted to prepare MoS2
Preparing a mixed solution of ammonium molybdate tetrahydrate and dimethyl formamide of thiourea, wherein the concentration of the mixed solution is 4.8-5.0 g/L, and the mass ratio of the ammonium molybdate tetrahydrate to the thiourea is 1: 2; stirring until the mixed solution of ammonium molybdate tetrahydrate and dimethylformamide of thiourea is in a transparent state; reacting for 24 hours at 200 ℃ in a reaction kettle, and cooling to room temperature; washing with deionized water, centrifuging to obtain black solidDrying the colored solid at 60-100 ℃ for 12-24 h to obtain MoS2；
(4) Bi prepared in the step (1)24O31Cl10Adding the mixture into a methanol solution, and performing ultrasonic treatment to obtain Bi with the concentration of 40-50 g/L24O31Cl10A mixed solution with methanol; g-C prepared in the step (2)3N4Is added to Bi24O31Cl10In a mixed solution with methanol, wherein g-C3N4And Bi24O31Cl10The mass ratio is 0.01-0.1; continuing ultrasonic treatment, centrifuging, washing and centrifuging again to obtain a solid substance; drying the solid matter at 60-80 deg.c for 24-48 hr, cooling and grinding to obtain 1-10% g-C3N4/ Bi24O31Cl10A composite photocatalyst;
(5) 5% g-C prepared in step (4)3N4/Bi24O31Cl10Adding the mixture into a methanol solution, and performing ultrasonic treatment to obtain 5% g-C with the concentration of 40-50 g/L3N4/Bi24O31Cl10A mixed solution with methanol; the MoS prepared in the step (3) is used2Adding to 5% g-C3N4/Bi24O31Cl10In a mixed solution with methanol, wherein, MoS2With 5% g-C3N4/Bi24O31Cl10The mass ratio of (A) to (B) is 0.03-0.07; continuing ultrasonic treatment, centrifuging, washing and centrifuging again to obtain a solid substance; drying the solid substance at 60-80 ℃ for 24-48 h, cooling and grinding to obtain 3-7% MoS2/5％g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
The invention has the beneficial effects that: tested, 5% MoS2/5％g-C3N4/Bi24O31Cl10The catalytic degradation rate of rhodamine B can reach 99%, and the degradation rate of the composite catalyst to tetracycline can reach more than 90% in 50min, and the composite catalyst is relatively pure Bi24O31Cl10、5％MoS2/Bi24O31Cl10、5％g-C3N4/Bi24O31Cl10The photocatalytic efficiency is remarkably improved. The method is simple and easy to implement, low in cost and good in repeatability, and has wide application prospects in the fields of photolysis of water, photocatalytic oxidation of environmental pollutants and the like.
Drawings
FIG. 1 shows Bi24O31Cl1、MoS2、g-C3N4、5％g-C3N4/Bi24O31Cl10、5％MoS2/Bi24O31Cl10、 5％MoS2/5％g-C3N4/Bi24O31Cl10XRD pattern of photocatalyst;
FIG. 2(a) shows Bi24O31Cl10SEM image of photocatalyst;
FIG. 2(b) is 5% MoS2/5％g-C3N4/Bi24O31Cl10SEM spectra of the photocatalyst;
figure 2(c) is an EDS spectrum;
FIG. 3 is a UV-Vis spectrum of a photocatalyst; wherein a represents Bi24O31Cl10B represents 5% g-C3N4/Bi24O31Cl10C represents 5% MoS2/Bi24O31Cl10D represents 5% MoS2/5％g-C3N4/ Bi24O31Cl10And e represents MoS2UV-Vis spectra of the photocatalyst;
FIG. 4 shows Bi24O31Cl10、5％g-C3N4/Bi24O31Cl10、5％MoS2/Bi24O31Cl10、5％MoS2 /5％g-C3N4/Bi24O31Cl10PL spectrum of the photocatalyst;
FIG. 5 shows the degradation efficiency of a photocatalyst on rhodamine B under visible light irradiation(ii) a Wherein a represents Bi24O31Cl10B represents 1% g-C3N4/Bi24O31Cl10C represents 3% g-C3N4/Bi24O31Cl10D represents 5% g-C3N4/Bi24O31Cl10E represents 10% g-C3N4/Bi24O31Cl10And f represents 5% MoS2/Bi24O31Cl10G represents 3% MoS2/5％g-C3N4/Bi24O31Cl10H represents 5% MoS2/5％g-C3N4/Bi24O31Cl10And i represents 7% MoS2/5％g-C3N4/Bi24O31Cl10；
Bi prepared in FIG. 624O31Cl10、5％g-C3N4/Bi24O31Cl10、5％MoS2/Bi24O31Cl10、 5％MoS2/5％g-C3N4/Bi24O31Cl10The degradation efficiency of the photocatalyst to the tetracycline under the visible light illumination is improved.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
The preparation method of the invention is used for preparing 3-7% MoS2/5％g-C3N4/Bi24O31Cl10Composite photocatalyst and preparation of 5% MoS2/Bi24O31Cl10The composite photocatalyst has the effect of comparing with the effects of various composite photocatalysts.
Examples 1
(1)Bi24O31Cl10The preparation of (1): dissolving 0.01mol of pentahydrate bismuth nitrate into 50ml of 10% dilute nitric acid by volume, adding 0.02mol of citric acid, and uniformly mixing until the bismuth nitrate is completely dissolved; in addition, 0.01mol of ammonium chloride was dissolved in 50ml of distilled waterAnd (4) mixing uniformly in water until the mixture is completely dissolved. Slowly injecting an ammonium chloride solution into a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid under the stirring of a constant-temperature magnetic stirrer, uniformly mixing until the solution is in a clear state, adjusting the pH value of the mixed solution to 6 by using ammonia water, continuously heating and stirring at 60 ℃ for 4 hours, pouring the mixed solution into a crucible with a cover, and calcining at 600 ℃ for 3 hours in a muffle furnace to obtain light yellow powder, namely pure Bi24O31Cl10。
(2)g-C3N4The preparation of (1): uniformly mixing 3g of melamine and 10 ml of acetic acid (the concentration is 36 percent), placing the mixture into a crucible with a cover, and then calcining the mixture for 2 hours in a muffle furnace at 500 ℃ to obtain light yellow powder, namely pure g-C3N4。
(3)MoS2The preparation of (1): dissolving 80 mg of ammonium molybdate tetrahydrate and 160 mg of thiourea in 50ml of dimethylformamide solvent, magnetically stirring until the reaction raw materials are dissolved to be transparent, then transferring to a 100ml stainless steel hydrothermal reaction kettle with a tetrafluoroethylene lining, reacting for 24 hours at 200 ℃, cooling to room temperature, then carrying out high-speed centrifugation at 10000r/min, washing for 5 times with distilled water to obtain black solid, drying for 24 hours at 60 ℃ in a drying oven to obtain MoS2。
(4) 2 g of Bi obtained in step (1)24O31Cl10Adding into 40 ml of methanol solution respectively, performing ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl100.02 g, 0.06 g, 0.10 g, and 0.2 g of-C prepared in step (2) were added to the mixed solution with methanol, respectively3N4Performing ultrasonic treatment on the powder for 1 hour under 1000KW power, centrifuging the solid and a methanol solution at the rotating speed of 10000r/min, washing the solid with distilled water, centrifuging the washed solid again, repeating the centrifugation for four times to obtain the solid, drying the solid in a drying oven at the temperature of 60 ℃ for 24 hours, cooling and grinding the dried solid to obtain the 1-10% g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
(5) Subjecting 1 g of 5% g-C obtained in step (4)3N4/Bi24O31Cl10Sample is added with 20 ml of methanolIn liquid, ultrasonic treatment is carried out for 1h under 1000KW power, and then 5 percent of g-C3N4/Bi24O31Cl100.3g of MoS prepared in step (3) was added to the mixed methanol solution, respectively2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 60 deg.C for 48h in a drying oven, cooling, and grinding to obtain 3% MoS2/5％g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
(6) 1 g of Bi obtained in the step (1)24O31Cl10Adding into 20 ml of methanol solution, carrying out ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl10Adding 0.5 g of MoS prepared in step (3) into the mixed solution of methanol2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 60 deg.C for 24h in a drying oven, cooling, and grinding to obtain 5% MoS2/Bi24O31Cl10A composite photocatalyst is provided.
EXAMPLES example 2
(1)Bi24O31Cl10The preparation of (1): dissolving 0.01mol of pentahydrate bismuth nitrate into 50ml of 10% dilute nitric acid by volume, adding 0.02mol of citric acid, and uniformly mixing until the bismuth nitrate is completely dissolved; in addition, 0.01mol of ammonium chloride was dissolved in 50ml of distilled water and mixed until completely dissolved. Slowly injecting an ammonium chloride solution into a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid under the stirring of a constant-temperature magnetic stirrer, uniformly mixing until the solution is in a clear state, adjusting the pH value of the mixed solution to 5 by using ammonia water, continuously heating and stirring at 80 ℃ for 3 hours, pouring the mixed solution into a crucible with a cover, and calcining at 600 ℃ for 3 hours in a muffle furnace to obtain light yellow powder, namely pure Bi24O31Cl10。
(2)g-C3N4The preparation of (1): 3g of melamine were admixed with 10 ml of melamineMixing L acetic acid (concentration: 36%), placing in crucible with cover, calcining in muffle furnace at 500 deg.C for 2 hr to obtain light yellow powder, i.e. pure g-C3N4。
(3)MoS2The preparation of (1): dissolving 60 mg of ammonium molybdate tetrahydrate and 120 mg of thiourea in 36 ml of dimethylformamide solvent, magnetically stirring until the reaction raw materials are dissolved to be transparent, then transferring to a 50ml stainless steel hydrothermal reaction kettle with a tetrafluoroethylene lining, reacting for 24h at 200 ℃, cooling to room temperature, then carrying out high-speed centrifugation at 10000r/min, washing for 5 times with distilled water to obtain black solid, drying for 12h at 100 ℃ in a drying oven to obtain MoS2。
(4) 1 g of Bi obtained in the step (1)24O31Cl10Adding into 25 ml of methanol solution respectively, performing ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl100.01 g, 0.03g, 0.05 g, and 0.1 g of-C prepared in step (2) were added to the mixed solution with methanol, respectively3N4Performing ultrasonic treatment on the powder for 1 hour under 1000KW power, centrifuging the solid and a methanol solution at the rotating speed of 10000r/min, washing the solid with distilled water, centrifuging the washed solid again, repeating the centrifugation for four times to obtain the solid, drying the solid in a drying oven at the temperature of 80 ℃ for 48 hours, cooling and grinding the dried solid to obtain the 1-10% g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
(5) 1.8 g of 5% g-C obtained in step (4)3N4/Bi24O31Cl10The sample is added to 40 ml of methanol solution, sonicated for 1h at 1000KW power, then at 5% g-C3N4/Bi24O31Cl100.09g of MoS prepared in step (3) was added to the mixed methanol solution separately2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 80 deg.C for 24h in a drying oven, cooling, and grinding to obtain 5% MoS2/5％g-C3N4/Bi24O31Cl10Composite photocatalysisAnd (3) preparing.
(6) 1 g of Bi obtained in the step (1)24O31Cl10Adding into 20 ml of methanol solution, carrying out ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl10Adding 0.5 g of MoS prepared in step (3) into the mixed solution of methanol2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 60 deg.C for 24h in a drying oven, cooling, and grinding to obtain 5% MoS2/Bi24O31Cl10A composite photocatalyst is provided.
EXAMPLE 3
(1)Bi24O31Cl10The preparation of (1): dissolving 0.01mol of pentahydrate bismuth nitrate into 50ml of 10% dilute nitric acid by volume, adding 0.02mol of citric acid, and uniformly mixing until the bismuth nitrate is completely dissolved; in addition, 0.01mol of ammonium chloride was dissolved in 50ml of distilled water and mixed until completely dissolved. Slowly injecting an ammonium chloride solution into a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid under the stirring of a constant-temperature magnetic stirrer, uniformly mixing until the solution is in a clear state, adjusting the pH value of the mixed solution to 6 by using ammonia water, continuously heating and stirring for 3.5 hours at 60 ℃, pouring the mixed solution into a crucible with a cover, and calcining for 3 hours at 600 ℃ in a muffle furnace to obtain light yellow powder, namely pure Bi24O31Cl10。
(2)g-C3N4The preparation of (1): uniformly mixing 3g of melamine and 10 ml of acetic acid (the concentration is 36 percent), placing the mixture into a crucible with a cover, and then calcining the mixture for 2 hours in a muffle furnace at 500 ℃ to obtain light yellow powder, namely pure g-C3N4。
(3)MoS2The preparation of (1): dissolving 45 mg of ammonium molybdate tetrahydrate and 90 mg of thiourea in 27.5 ml of dimethylformamide solvent, magnetically stirring until the reaction raw materials are dissolved to be transparent, then transferring to a 50ml stainless steel hydrothermal reaction kettle with a tetrafluoroethylene lining, reacting for 24h at 200 ℃, cooling to room temperature, then centrifuging at high speed at 10000r/min, washing with distilled water for 5 timesThen obtaining black solid, drying for 18h at 80 ℃ in a drying oven to obtain MoS2。
(4) 9g of Bi obtained in step (1)24O31Cl10Respectively adding into 200 ml of methanol solution, performing ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl100.09g, 0.27 g, 0.45 g, and 0.9 g of-C prepared in step (2) were added to the mixed solution with methanol, respectively3N4Performing ultrasonic treatment on the powder for 1 hour under 1000KW power, centrifuging the solid and a methanol solution at the rotating speed of 10000r/min, washing the solid with distilled water, centrifuging the washed solid, repeating the centrifugation for four times to obtain the solid, drying the solid in a drying oven at 70 ℃ for 36 hours, cooling and grinding the dried solid to obtain the 1-10% g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
(5) 1.5 g of 5% g-C obtained in step (4)3N4/Bi24O31Cl10The sample is added to 30 ml of methanol solution, sonicated for 1h at 1000KW power, then at 5% g-C3N4/Bi24O31Cl100.105g of MoS prepared in step (3) was added to the methanol mixed solution, respectively2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 70 deg.C for 36h in a drying oven, cooling, and grinding to obtain 7% MoS2/5％g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
(6) 1 g of Bi obtained in the step (1)24O31Cl10Adding into 20 ml of methanol solution, carrying out ultrasonic treatment for 1h under 1000KW power, and then adding into Bi24O31Cl10Adding 0.5 g of MoS prepared in step (3) into the mixed solution of methanol2Performing ultrasonic treatment on the powder for 1h under 1000KW power, centrifuging the solid and methanol solution at 10000r/min, washing with distilled water, centrifuging, repeating for four times to obtain solid, drying at 60 deg.C for 24h in a drying oven, cooling, and grinding to obtain 5% MoS2/Bi24O31Cl10A composite photocatalyst is provided.
And (3) structural and morphological characterization:
as can be seen from FIG. 1, Bi was produced24O31Cl10Tetragonal system Bi of JCPDS standard card number (No.75-0887)24O31Cl10The diffraction peaks are identical. 5% g-C3N4/Bi24O31Cl10No g-C in the sample3N4Peak, 5% MoS2/Bi24O31Cl10No MoS in the sample2Peak of (5%), MoS2/5％g-C3N4/Bi24O31Cl105% of the total content of the extract is not observed to be g-C3N4And MoS2Mainly due to complexed g-C3N4And MoS2Less in the amount of the compound (A).
As can be seen from FIGS. 2(a), 2(b) and 2(c), 5% MoS was produced2/5％g-C3N4/Bi24O31Cl10In the sample, g-C is successfully compounded3N4And MoS2。
As can be seen from FIG. 3, when Bi is present24O31Cl10And MoS2Or g-C3N4After compounding, the light absorption performance of the sample is obviously improved, wherein MoS is compounded2The light absorption performance of the rear sample is higher than that of the composite g-C3N4The promotion is more remarkable when MoS2And g-C3N4Simultaneous recombination of Bi24O31Cl10The light absorption performance is improved to the maximum, and the light absorption is obvious within the range of 200-800 nm.
As can be seen from FIG. 4, 5% MoS2/5％g-C3N4/Bi24O31Cl10The lowest PL peak intensity shows that the photo-excited electron-hole recombination rate of the photocatalyst is the lowest, and the lower the recombination rate is, the photocatalytic activity is improved.
Photocatalytic activity test experiment:
taking the initial concentration as 5 mg.L-1The rhodamine B (RhB) solution is 100mL or 20 mg.L-150mL of tetracycline hydrochloride solution is taken as a target degradation product and placed in a 250mL beaker, and then 0.03g of photocatalyst is added into rhodamine B or tetracycline hydrochloride solution and mixed uniformly. Before illumination, the suspension is magnetically stirred in a dark room for 30min to ensure that adsorption-desorption balance is achieved between the photocatalyst and rhodamine B or tetracycline, and then the suspension is placed under a visible light source (250W metal halide lamp) 14cm away from the liquid level for a photocatalytic experiment. The illumination time is 50min, wherein supernatant liquid is taken by a clean rubber head dropper every 10min, the supernatant liquid is placed in a cuvette after centrifugation, the absorbance of the supernatant liquid is measured at the maximum absorption wavelengths of 554nm and 356nm of rhodamine B and tetracycline, and the removal rate D of the rhodamine B or tetracycline solution can be calculated according to the Lambert beer law by the formula (1):
D＝(C0-C)/C0×100％＝(A0’-A)/A0’×100％ (1)
in the formula: c0C is the concentration of rhodamine B or tetracycline solution before and after illumination;
A0', A-absorbance of rhodamine B or tetracycline solution before and after illumination
5% MoS as shown in FIG. 52/5％g-C3N4/Bi24O31Cl10The catalytic degradation rate of rhodamine B can reach 90% within 50min, and the degradation rate of the composite catalyst to tetracycline can also reach about 88% within 50min (as shown in figure 6), and the composite catalyst is relatively pure Bi24O31Cl10、5％MoS2/Bi24O31Cl10、5％g-C3N4/ Bi24O31Cl10The photocatalytic efficiency is obviously improved, which indicates that MoS is adopted2And g-C3N4Simultaneous recombination of Bi24O31Cl10The activity of the compound is obviously improved.
Claims (1)
1. High-activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of the composite photocatalyst is characterized in thatThe method comprises the following steps:
(1) bi is prepared by taking bismuth nitrate, ammonium chloride and citric acid as raw materials and adopting an improved solution combustion method24O31Cl10
Mixing bismuth nitrate pentahydrate and citric acid, and dissolving in dilute nitric acid to obtain a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid, wherein the molar ratio of bismuth nitrate pentahydrate to citric acid is 1: 2; dissolving ammonium chloride in distilled water until the ammonium chloride is completely dissolved to obtain an ammonium chloride solution; under the condition of stirring, adding an ammonium chloride solution into a mixed solution of bismuth nitrate pentahydrate and dilute nitric acid of citric acid, wherein the molar ratio of the bismuth nitrate pentahydrate to the ammonium chloride is 1: 1, uniformly mixing until the solution is in a clear state, and adjusting the pH value of the solution to 5-6 by using ammonia water; heating and stirring for 3-4 h at 60-80 ℃, and then calcining for 3h at 600 ℃ to obtain light yellow powder, namely pure Bi24O31Cl10；
(2) g-C is prepared from melamine and acetic acid by one-step thermal polymerization method3N4
Uniformly mixing melamine and acetic acid according to a molar ratio of 10:1, calcining for 2 hours at 500 ℃ to obtain light yellow powder, namely pure g-C3N4；
(3) Ammonium molybdate and thiourea are used as raw materials, dimethylformamide is used as a solvent, and a hydrothermal method is adopted to prepare MoS2
Preparing a mixed solution of ammonium molybdate tetrahydrate and dimethyl formamide of thiourea, wherein the concentration of the mixed solution is 4.8-5.0 g/L, and the mass ratio of the ammonium molybdate tetrahydrate to the thiourea is 1: 2; stirring until the mixed solution of ammonium molybdate tetrahydrate and dimethylformamide of thiourea is in a transparent state; reacting for 24 hours at 200 ℃ in a reaction kettle, and cooling to room temperature; washing with deionized water, centrifuging to obtain a black solid, and drying the black solid at 60-100 ℃ for 12-24 h to obtain MoS2；
(4) Bi prepared in the step (1)24O31Cl10Adding the mixture into a methanol solution, and performing ultrasonic treatment to obtain Bi with the concentration of 40-50 g/L24O31Cl10A mixed solution with methanol;g-C prepared in the step (2)3N4Is added to Bi24O31Cl10In a mixed solution with methanol, wherein g-C3N4And Bi24O31Cl10The mass ratio is 0.01-0.1; continuing ultrasonic treatment, centrifuging, washing and centrifuging again to obtain a solid substance; drying the solid matter at 60-80 deg.c for 24-48 hr, cooling and grinding to obtain 1-10% g-C3N4/Bi24O31Cl10A composite photocatalyst;
(5) 5% g-C prepared in step (4)3N4/Bi24O31Cl10Adding the mixture into a methanol solution, and performing ultrasonic treatment to obtain 5% g-C with the concentration of 40-50 g/L3N4/Bi24O31Cl10A mixed solution with methanol; the MoS prepared in the step (3) is used2Adding to 5% g-C3N4/Bi24O31Cl10In a mixed solution with methanol, wherein, MoS2With 5% g-C3N4/Bi24O31Cl10The mass ratio of (A) to (B) is 0.03-0.07; continuing ultrasonic treatment, centrifuging, washing and centrifuging again to obtain a solid substance; drying the solid substance at 60-80 ℃ for 24-48 h, cooling and grinding to obtain 3-7% MoS2/5％g-C3N4/Bi24O31Cl10A composite photocatalyst is provided.
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