CN110560092B - MoS 2 /BiVO 4 Preparation method and application of heterojunction composite photocatalyst - Google Patents
MoS 2 /BiVO 4 Preparation method and application of heterojunction composite photocatalyst Download PDFInfo
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- 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
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- B01J35/23—
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- B01J35/39—
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- B01J35/51—
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the technical field of preparation of environmental materials, and relates to synthesis of MoS by a hydrothermal method 2 /BiVO 4 A preparation method and application of the composite photocatalyst; the method comprises the following steps: first, moS is prepared 2 Adding bismuth nitrate and polyvinylpyrrolidone into ethylene glycol, and performing ultrasonic dispersion and dissolution to obtain a mixed solution A; reacting NH 4 VO 3 Adding the mixture into deionized water, and performing ultrasonic dispersion and dissolution to obtain a mixed solution B; under the magnetic stirring, moS 2 Slowly adding the nanosheet, the 3-mercaptopropionic acid and the mixed solution B into the mixed solution A, transferring the mixed solution into an autoclave for constant-temperature reaction, centrifuging after reaction, washing and drying the obtained precipitate to obtain MoS 2 /BiVO 4 A composite photocatalyst; the method is simple and convenient to operate, safe and environment-friendly, and the catalyst is 0D BiVO in appearance 4 /2DMoS 2 The catalyst has the characteristic of large active specific surface area, and is used for degrading harmful substances in environmental wastewater.
Description
Technical Field
The invention belongs to the technical field of preparation of environmental materials, and relates to synthesis of MoS by a hydrothermal method 2 /BiVO 4 Preparation of composite photocatalystA method and use thereof.
Background
Antibiotics (Antibiotics) are pathogen-resistant secondary metabolites produced by bacteria, molds and other microorganisms or by higher animals and plants, and are chemical substances that impede the development of other cells. In the rapidly developing modern society of the pharmaceutical industry, antibiotics are used in a large number in the treatment and defense of diseases in humans and livestock. However, the hazards of antibiotic abuse cannot be ignored: cannot be easily biodegraded and a large amount of remaining waste can flow into the aquatic environment. Various antibiotics existing in the environment promote drug-resistant genes and bacteria to be transferred into human bodies through various different ways, and serious influence is caused on the balance of a natural ecological system and human health. Therefore, how to efficiently treat ecological damage caused by antibiotic residues and solve the problem of food safety caused by antibiotic enrichment effect becomes a key concern of many researchers.
Photocatalytic degradation utilizes solar energy which is easily obtained in natural environment to degrade all toxic and harmful organic substances and part of inorganic substances in water environment. The photocatalysis technology has the characteristics of high catalysis efficiency, simple operation, energy conservation, low cost and the like, and is one of the most effective advanced oxidation technologies in the field of removing aquatic pollutants. As can be seen from the related researches, one of the methods for improving the carrier separation efficiency is to couple two semiconductors, i.e. to form a heterojunction. The heterojunction formed by the extremely poor energy of the two semiconductors can effectively promote the separation, transfer and transfer of electron holes, so that the purpose of inhibiting the recombination of photo-generated electrons and holes is achieved, and the photocatalytic activity is improved.
Molybdenum disulfide (MoS) 2 ) Is a two-dimensional Transition Metal Disulfide (TMD) having a unique layered structure and specific properties. Recently, some reports have shown that MoS 2 Can be used as an effective cocatalyst for photocatalytic hydrogen production and degradation of organic pollutants under visible light irradiation [1-6] . And MoS 2 MoS consisting of weakly coupled S-Mo-S atomic interlayers, stacked face-to-face and weakly interacting 2 The lumpy molybdenum disulfide of the layer composition has an extremely adverse effect on the photocatalytic performance, considering twoFew-vitamin layer MoS 2 The nano-sheet is a feasible material of a heterojunction, has proper band gap energy of 1.9eV, and has high specific surface area and more edge positions compared with bulk molybdenum disulfide. The synthesis of oxygen-doped MoS through a hydrothermal method and a chemical plating solution deposition calcination process is reported in the literature 2 nanosphere/CdS quantum dot/g-C 3 N 4 The nano-sheet increases more active sites, and the formed heterojunction effectively inhibits the recombination of electron hole pairs; however, the CdS quantum dots have heavy metal ions and are slightly soluble in water due to photo-corrosion, so that secondary pollution is caused.
Bismuth vanadate (BiVO) 4 ) Has the following advantages: non-toxic, inexpensive and chemically stable; however, biVO is limited by defects such as poor separation of electron-hole pairs, slow charge carrier mobility, short carrier diffusion length and significant recombination of electron-holes during application 4 The performance of (c). Because of these problems, if a more efficient photocatalytic system is designed to promote BiVO 4 The charge separation of (a) will be of great significance. The heterostructure composite material mentioned above is beneficial to improving the performance and solves the BiVO 4 Poor separation of electron-hole pairs and slow charge carrier migration rate. The existing report shows that the novel heterojunction photocatalyst n-Bivo4@ p-MoS with the core-shell structure is successfully prepared by adopting an in-situ hydrothermal method 2 However, the core-shell structure catalyst has a smaller active specific surface area than the 0D/2D structure.
Disclosure of Invention
The invention aims to prepare MoS by taking a hydrothermal method as a technical means 2 /BiVO 4 A composite photocatalyst is provided.
The invention is realized by the following technical scheme:
method for synthesizing MoS by photolysis deposition method and hydrothermal method 2 /BiVO 4 The preparation method of the composite photocatalyst comprises the following steps:
step 1, preparation of MoS 2 Nanosheets;
will be (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and CH 4 N 2 S adding deionized waterStirring and dissolving to form a uniform solution; then transferring the mixture into a high-pressure kettle for constant-temperature reaction, naturally cooling the mixture to room temperature after the reaction, repeatedly washing the obtained product with water and ethanol, drying the washed product, grinding the dried product into fine powder to obtain MoS 2 Dispersing the powder in a mixed solution of water and ethanol, performing ultrasonic stirring to obtain a suspension, performing ultrasonic treatment on the suspension to obtain a sheet material with precipitate aggregation, namely MoS 2 Nanosheets;
mixing bismuth nitrate (Bi (NO) 3 ﹒5H 2 O) and polyvinylpyrrolidone are added into ethylene glycol, and ultrasonic dispersion and dissolution are carried out to obtain a mixed solution A; reacting NH 4 VO 3 Adding the mixture into deionized water, and performing ultrasonic dispersion and dissolution to obtain a mixed solution B; then, the MoS prepared in step (1) is stirred under magnetic force 2 Slowly adding the nanosheets, the 3-mercaptopropionic acid and the mixed solution B into the mixed solution A to obtain a mixed solution C, transferring the mixed solution C into an autoclave for constant-temperature reaction, centrifuging the reacted solution, cleaning the centrifuged precipitate with deionized water and absolute ethyl alcohol, and finally passing through a vacuum drying oven to obtain MoS 2 /BiVO 4 A composite photocatalyst is provided.
Preferably, in step 1, the (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O、CH 4 N 2 S and H 2 The dosage ratio of O is 0.1mmol:3mmol:70mL.
Preferably, in the step 1, the temperature of the isothermal thermal reaction is 220-250 ℃, and the reaction time is 20-24 h.
Preferably, in the step 1, the ultrasonic stirring time is 6-10h; the ultrasonic treatment time is 20-30min.
Preferably, in step 1, the volume ratio of water to ethanol is 3.
Preferably, in step 2, bi (NO) used in the mixed solution A 3 ﹒5H 2 The dosage ratio of O, polyvinylpyrrolidone and glycol is 0.094-0.886 g:0.4g:50mL.
Preferably, in step 2, NH in the mixed solution B 4 VO 3 The dosage ratio of the deionized water is 0.0253 g-0.034 g:30 mL.
Preferably, in step 2, the MoS 2 The dosage ratio of the nano-sheets, the 3-mercaptopropionic acid, the mixed solution B and the mixed solution A is 5-30 mg: 0.05-0.2 mL: 20-30 mL: 30-50 mL.
Preferably, in the step 2, the temperature of the isothermal thermal reaction is 160-200 ℃, and the reaction time is 1-6h.
Preferably, in the step 2, the rotation speed of the centrifugation is 8000-10000 r/s, and the time is 3-5 min.
Preferably, in step 2, the MoS is prepared 2 /BiVO 4 In the composite photocatalyst, moS 2 The mass fraction of (A) is 5-30%.
Prepared MoS 2 /BiVO 4 The composite photocatalyst is used for degrading tetracycline in wastewater.
Evaluation of photocatalytic activity: irradiating with visible light lamp in DW-01 type photochemical reactor (purchased from teaching instrument factory of Yangzhou university), adding 100mL tetracycline simulation wastewater into the reactor, measuring initial value, adding 100mg composite photocatalyst, magnetically stirring, starting aeration device, introducing air to keep the catalyst in suspension or floating state, sampling and analyzing at 20min interval during the irradiation process, centrifuging, collecting supernatant, and placing in spectrophotometer lambda max Absorbance at 356nm and determined by the formula: DR = [ (A) 0 -A i )/A 0 ]X 100% calculating the degradation rate, wherein A 0 Absorbance of the tetracycline solution to equilibrium for adsorption, A i The absorbance of the tetracycline solution was determined for the timed samples.
Ammonium molybdate tetrahydrate, 3-mercaptopropionic acid, bismuth nitrate pentahydrate, thiourea, ammonium metavanadate and ethylene glycol used in the invention are analytically pure, and polyvinylpyrrolidone is super-grade pure and purchased from national chemical reagent Limited; the tetracycline antibiotic is a standard product and is purchased from Shanghai Shubo bioengineering Co.
Has the advantages that:
the invention realizesBy MoS 2 /BiVO 4 For the purpose of degrading antibiotic wastewater by using a catalyst; the photocatalyst shows 0D BiVO in appearance by adding 3-mercaptopropionic acid dispersant 4 /2D MoS 2 The catalyst has the characteristics of large active specific surface area; the degradation rate of tetracycline antibiotics reaches 68.83 percent within 150 min. The invention takes semiconductor material as photocatalyst, the light excitation wave band is visible light wave band, and the catalytic driving or conversion effect is realized through the interface interaction with the antibiotic wastewater molecules, so that oxygen and water molecules entering the wastewater are excited to form free negative ions with oxidizing property, and further the harmful substances in the environmental wastewater are degraded. When the molybdenum disulfide is prepared by the method, an ultrasonic stirring mode is adopted, the operation is convenient and fast, the cost is low, the solvent selected by ultrasonic is a mixed solution of water and ethanol, the method is non-toxic and harmless, and no additional pollutant is formed.
Drawings
FIG. 1 is the MoS prepared in example 5 2 /BiVO 4 TEM image of composite photocatalyst, and FIG. a is MoS 2 The edges of the flower ball are in a thin sheet shape; FIG. b shows BiVO 4 Nanoparticles, which are seriously agglomerated because no dispersant is added; FIG. c shows MoS 2 /BiVO 4 Adding dispersant 3-mercaptopropionic acid and BiVO into a morphology chart of the composite photocatalyst 4 The nano particles are uniformly dispersed in the MoS 2 On the flower ball, the sample preparation is indicated to be successful.
FIG. 2 is the MoS prepared in example 5 2 /BiVO 4 The solid ultraviolet image of the composite photocatalyst shows that the photocatalyst has a good photoresponse interval, biVO 4 Improves MoS by adding 2 The sample itself is black in color, and the most preferable example is MoS in a mass fraction of 20wt% 2 /BiVO 4 Has a light response intensity higher than MoS 2 The sample has obvious response in a visible light region, and the prepared catalyst can effectively carry out photocatalytic reaction in the visible light region.
FIG. 3 is the MoS prepared in example 5 2 /BiVO 4 The XRD pattern of the composite photocatalyst can show MoS 2 And BiVO 4 All have better crystallinity and areQuasi-card JCPDS No.48-0744 and No.14-0688 correspond to MoS 2 /BiVO 4 The peak intensity of the composite photocatalyst is reduced, but the characteristic peak still exists, which indicates that the photocatalyst is indeed MoS 2 And BiVO 4 The complex of (1).
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
(1)MoS 2 preparing a nano sheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for carrying out constant temperature thermal reaction at 230 ℃ for 22 h; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of the bulk MoS 2 Dispersing the powder in 400mL of a water and ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 8h, then the suspension is placed in an ultrasonic cleaner and treated for 20min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 Nanosheets;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.0940g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution as a mixed solution A; 0.0307g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a mixed solution B; then, 15mg of MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.05mL of mercaptopropionic acid and 20mL of mixed solution B into 30mL of mixed solution A, transferring the final mixture into a 100mL stainless steel autoclave, reacting for 1h at 180 ℃, centrifuging the obtained mixture, wherein the rotation speed of the centrifugation is 8000 rpm, and the time is 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 ；
(3) And (3) carrying out a photocatalytic degradation test on the sample in the step (2) in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to the tetracycline antibiotic reaches 54.81 percent within 150 min.
Example 2:
(1)MoS 2 preparing a nano sheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for carrying out constant temperature thermal reaction at 220 ℃ for 24 hours; after the reaction is finished, cooling to room temperature, washing the solid product by using deionized water and ethanol, drying, and then grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a water and ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 8h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 Nanosheets;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.105g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution A;0.034g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a solution B; then, 5mg of MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.1mL of mercaptopropionic acid and 25mL of mixed solution B into 40mL of mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; after reacting for 3 hours at 180 ℃, centrifuging the obtained mixture, wherein the centrifugal rotating speed is 10000 r/s, and the time is 3min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) carrying out a photocatalytic degradation test on the sample in the step (2) in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 52.63% within 150 min.
Example 3:
(1)MoS 2 nano-sheetThe preparation of (1): 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for constant temperature thermal reaction at 240 ℃ for 22 hours; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a water and ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 10h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 Nanosheets;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.102g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g of polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution A; 0.0332g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a solution B; then, 5mg MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.2mL of mercaptopropionic acid and 30mL of the mixed solution B into 50mL of the mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; reacting at 200 deg.C for 4 hr, centrifuging at 8000 rpm for 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) taking the sample in the step (2) to carry out a photocatalytic degradation test in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 54.36% within 150 min.
Example 4:
(1)MoS 2 preparation of the nanosheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; the solution was then transferred to a teflon lined stainless steel autoclaveCarrying out constant temperature thermal reaction at 250 ℃ for 22 h; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a water and ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 6h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 Nanosheets;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.100g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g of polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution A; 0.0325g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a solution B; then, 10mg MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.1mL of mercaptopropionic acid and 20mL of the mixed solution B into 30mL of the mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; reacting at 160 ℃ for 6h, and centrifuging the obtained mixture at 10000 r/s for 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) taking the sample in the step (2) to carry out a photocatalytic degradation test in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 34.92% within 150 min.
Example 5:
(1)MoS 2 preparing a nano sheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for carrying out constant temperature thermal reaction at 220 ℃ for 24 hours; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a mixture of water and ethanolThe volume ratio is 3; then ultrasonic vibration stirring treatment is carried out for 6h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 A nanosheet;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.100g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g of polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution A; 0.0325g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a solution B; then, 8mg of MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.1mL of mercaptopropionic acid and 30mL of the mixed solution B into 50mL of the mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; reacting at 180 ℃ for 3h, and centrifuging the obtained mixture at 10000 r/s for 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) taking the sample in the step (2) to perform a photocatalytic degradation test in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 68.83% within 150 min.
Example 6:
(1)MoS 2 preparing a nano sheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and is vigorously stirred for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for constant temperature thermal reaction at 220 ℃ for 22 h; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a water-ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 6h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 Nanosheets;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: 0.831g of Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g of polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol, and performing ultrasonic dispersion for 40min to mark the solution A; 0.0271g of NH 4 VO 3 In 30mL deionized water subjected to ultrasonic dispersion for 40min, marking as a solution B; then, 25mg of MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.1mL of mercaptopropionic acid and 30mL of the mixed solution B into 50mL of the mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; reacting at 180 ℃ for 1h, and centrifuging the obtained mixture at 10000 r/s for 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) taking the sample in the step (2) to carry out a photocatalytic degradation test in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 64.52% within 150 min.
Example 7:
(1)MoS 2 preparing a nano sheet: 0.1mmol (NH) 4 ) 6 Mo 7 O 24 ﹒4H 2 O and 3mmol CH 4 N 2 S is dissolved in 70mL of water and stirred vigorously for 30min to form a uniform solution; then, transferring the solution into a stainless steel autoclave with a Teflon lining for constant temperature thermal reaction at 220 ℃ for 22 h; after the reaction is finished, cooling to room temperature, washing the solid product by deionized water and ethanol, drying, and grinding the dried product into fine powder; 80mg of MoS 2 Dispersing the powder in 400mL of a water and ethanol mixed solution, wherein the volume ratio of water to ethanol is 3; then ultrasonic vibration stirring treatment is carried out for 6h, then the suspension is placed in an ultrasonic cleaner and treated for 30min again to precipitate aggregated sheets, and then the sheets are washed and dried to obtain MoS 2 A nanosheet;
(2)MoS 2 /BiVO 4 preparing a composite photocatalyst: mixing 0.776g Bi (NO) 3 ﹒5H 2 Dissolving O and 0.4g of polyvinylpyrrolidone (PVP; MW-40K) in 50mL of glycol for 40min in ultrasonic dispersion, and marking the solution as a solution A; 0.0253g of NH 4 VO 3 In the ultrasoundDispersing in 30mL of deionized water for 40min, and marking as a solution B; then, 30mg of MoS was added under magnetic stirring 2 Slowly adding the nanosheets, 0.1mL of mercaptopropionic acid and 30mL of mixed solution B into 50mL of mixed solution A, and transferring the final mixture into a 100mL stainless steel autoclave; reacting at 180 ℃ for 6 hours, and centrifuging the obtained mixture, wherein the rotation speed of the centrifugation is 10000 r/s, and the time is 5min; centrifuging, washing with deionized water and anhydrous ethanol for 3 times, and drying at 60 deg.C to obtain MoS 2 /BiVO 4 。
(3) And (3) carrying out a photocatalytic degradation test on the sample in the step (2) in a photochemical reactor, and measuring that the degradation rate of the photocatalyst to tetracycline reaches 12.90% within 150 min.
FIG. 1 is the MoS prepared in example 5 2 /BiVO 4 TEM image of composite photocatalyst, and FIG. a is MoS 2 The edges of the flower ball are in a thin sheet shape; a graph b shows BiVO4 nano particles, and the particles are seriously agglomerated due to no addition of a dispersing agent; FIG. c shows MoS 2 /BiVO 4 Adding dispersant 3-mercaptopropionic acid and BiVO into a composite photocatalyst topography 4 The nano particles are uniformly dispersed in the MoS 2 On the ball, the successful preparation of the sample is indicated.
FIG. 2 is the MoS prepared in example 5 2 /BiVO 4 The solid ultraviolet image of the composite photocatalyst shows that the photocatalyst has a good photoresponse interval, biVO 4 Improves MoS by adding 2 The sample itself is black in color, and the most preferable example is MoS in a mass fraction of 20wt% 2 /BiVO 4 All the light response intensity is higher than MoS 2 The sample has obvious response in a visible light region, and the prepared catalyst can effectively carry out photocatalytic reaction in the visible light region.
FIG. 3 is the MoS prepared in example 5 2 /BiVO 4 The XRD pattern of the composite photocatalyst can show MoS 2 And BiVO 4 All have better crystallinity, which respectively correspond to standard cards JCPDS No.48-0744 and No.14-0688, moS 2 /BiVO 4 The peak intensity of the composite photocatalyst is reduced, but the characteristic peak still exists, which indicates that the photocatalyst is indeed MoS 2 And BiVO 4 The complex of (1).
Description of the invention: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all such modifications and variations that do not depart from the spirit and scope of the invention are intended to be included within the scope of the appended claims.
Claims (6)
1. MoS 2 /BiVO 4 The preparation method of the heterojunction composite photocatalyst is characterized by comprising the following steps:
step 1, mixing (NH) 4 ） 6 Mo 7 O 24 ﹒4H 2 O and CH 4 N 2 S, adding the mixture into deionized water, and stirring and dissolving the mixture to form a uniform solution; then transferring the mixture into an autoclave for constant temperature reaction, wherein the temperature of the constant temperature reaction is 220 to 250 ℃, and the reaction time is 20 to 24 hours; naturally cooling to room temperature after reaction, repeatedly cleaning the obtained product with water and ethanol, drying after cleaning, grinding the dried product into fine powder to obtain MoS 2 Dispersing the powder in a mixed solution of water and ethanol, performing ultrasonic stirring to obtain a suspension, performing ultrasonic treatment on the suspension to obtain a sheet material with precipitate aggregation, namely MoS 2 A nanosheet;
step 2, adding Bi (NO) 3 ﹒5H 2 Adding O and polyvinylpyrrolidone into ethylene glycol, and performing ultrasonic dispersion and dissolution to obtain a mixed solution A; bi (NO) used in the mixed solution A 3 ﹒5H 2 The dosage ratio of O, polyvinylpyrrolidone and glycol is 0.094 to 0.886g:0.4g:50mL; reacting NH 4 VO 3 Adding the mixture into deionized water, and performing ultrasonic dispersion and dissolution to obtain a mixed solution B; NH in the mixed solution B 4 VO 3 The dosage ratio of the deionized water is 0.0253 g-0.034 g:30mL;
then, the MoS prepared in step (1) is stirred under magnetic force 2 Nanosheet, 3-mercaptopropionic acid, and mixed solutionSlowly adding the solution B into the mixed solution A to obtain a mixed solution C, wherein MoS 2 The dosage ratio of the nanosheet to the 3-mercaptopropionic acid to the mixed solution B to the mixed solution A is 8 to 25mg: 0.1ml: 30mL of: 50mL; transferring the mixture into a high-pressure autoclave for constant-temperature reaction at 160-200 ℃ for 1-6 h; centrifuging the solution after reaction, cleaning the precipitate after centrifugation by using deionized water and absolute ethyl alcohol, and finally obtaining MoS through a vacuum drying oven 2 /BiVO 4 A composite photocatalyst.
2. A MoS according to claim 1 2 /BiVO 4 The preparation method of the heterojunction composite photocatalyst is characterized in that in the step 1, (NH) 4 ） 6 Mo 7 O 24 ﹒4H 2 O、CH 4 N 2 S and H 2 The dosage ratio of O is 0.1mmol:3mmol:70mL.
3. A MoS according to claim 1 2 /BiVO 4 The preparation method of the heterojunction composite photocatalyst is characterized in that the ultrasonic stirring time is 6-10h; the ultrasonic treatment time is 20-30min; the volume ratio of the water to the ethanol is 3.
4. A MoS according to claim 1 2 /BiVO 4 The preparation method of the heterojunction composite photocatalyst is characterized in that in the step 2, the rotation speed of the centrifugation is 8000-10000 r/s, and the time is 3-5min.
5. MoS according to claim 1 2 /BiVO 4 The preparation method of the heterojunction composite photocatalyst is characterized in that in the step 2, the prepared MoS 2 /BiVO 4 In the composite photocatalyst, moS 2 The mass fraction of (A) is 5-30%.
6. MoS prepared by the method according to any one of claims 1 to 5 2 /BiVO 4 Application of heterojunction composite photocatalyst in degradationTetracycline in wastewater.
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| CN114425370B (en) * | 2021-12-09 | 2023-10-27 | 伊犁师范大学 | MoS 2 @CuCo 2 S 4 Composite material and preparation method and application thereof |
| CN114308078B (en) * | 2021-12-27 | 2023-10-13 | 江苏大学 | BiVO (binary organic acid) 4 /MoS 2 Composite photo-catalytic material @ GO and preparation method and application thereof |
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