CN114653381A - ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Preparation method and application of micron rod core-shell heterojunction catalyst - Google Patents

ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Preparation method and application of micron rod core-shell heterojunction catalyst Download PDF

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CN114653381A
CN114653381A CN202210138208.4A CN202210138208A CN114653381A CN 114653381 A CN114653381 A CN 114653381A CN 202210138208 A CN202210138208 A CN 202210138208A CN 114653381 A CN114653381 A CN 114653381A
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夏杰祥
严兴旺
王彬
尹盛
李华明
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
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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
    • 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
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
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    • C—CHEMISTRY; METALLURGY
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    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/00—Nature of the contaminant
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    • C02F2101/38—Organic compounds containing nitrogen
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention belongs to the field of catalysts, and discloses ZnIn2S4BiVO (bismuth oxide) wrapped by nanosheets4A preparation method and application of a micron rod core-shell heterojunction catalyst. The catalyst is synthesized by an oil bath method, and the preparation steps are as follows: BiVO (bismuth oxide) is added4And ZnCl2、InCl3·4H2Adding O and thioacetamide into dilute hydrochloric acid, adding a certain amount of glycerol, and addingReacting in a round-bottom flask at a certain temperature for a certain time, centrifuging, washing and drying the obtained product to obtain brown ZnIn2S4/BiVO4A composite material. The invention relates to mulberry-shaped BiVO4ZnIn with sheet-shaped in-situ grown on surface2S4The materials are in close contact with each other, and the effective separation and transfer of photo-generated charges can be realized. The matching band gap of the two is utilized, the light absorption range of the photocatalyst is widened, and the photocatalytic activity of the material is improved. The prepared composite material can be applied to the catalytic degradation of tetracycline TC under visible light. The method has the advantages of simple operation process, short material synthesis period and mild reaction conditions.

Description

ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Preparation method and application of micron rod core-shell heterojunction catalyst
Technical Field
The invention belongs to the technical field of photocatalysis and the field of environmental management, and particularly relates to ZnIn2S4BiVO (BiVO) wrapped by nanosheets4A preparation method and application of a micron rod core-shell heterojunction catalyst.
Background
With the continuous development and progress of medical technology, antibiotics are used in large quantities in the treatment of diseases. However, abuse of antibiotics also has serious consequences for the environment on which humans live: can not be degraded, and a large amount of organic pollutants remained cause serious pollution to water. Various antibiotics in the water body are transferred into the human body through different ways, which causes great harm to the health of people. Therefore, how to efficiently treat the organic pollutants remained in the water body becomes a problem of great concern. The traditional sewage treatment method has the defects of low removal efficiency, high cost, secondary pollution and the like. The photocatalytic oxidation sewage treatment technology has the advantages of low energy consumption, environmental friendliness, thorough pollutant degradation and the like, and is widely concerned by people in recent years, and semiconductor photocatalytic materials also become research hotspots in the field of materials. However, most intrinsic semiconductor materials have the defects of poor visible light response capability, high recombination rate of photogenerated electrons and holes and the like, which seriously limits the application of the intrinsic semiconductor materials in the field of photocatalysis. Therefore, the research of the novel photocatalytic material has important significance.
BiVO4The material has controllable shape and strong sunlight absorption (lambda)<550nm) and a relatively narrow band gap (2.3-2.4 eV), and the like, and is a very attractive material in the field of photocatalysis. However, the original BiVO4The material has high recombination rate of photogenerated electrons and holes, which seriously inhibits the photocatalysis of the materialAnd (4) performance is improved. How to achieve spatial separation of photo-generated charges is a difficult problem to be solved. Conventionally, it has been reported that heterojunction formation is an effective strategy for suppressing charge recombination and promoting charge separation. The strategy can not only improve the mobility of the photo-generated electrons and holes, but also enable the photo-generated electrons and holes to have stronger reduction and oxidation capabilities. Thus, BiVO can be constructed4The base heterojunction photocatalyst can realize the purpose of efficiently degrading antibiotics. ZnIn2S4Are reported to be excellent photocatalysts due to their suitable valence and conduction band positions and good optical properties. In BiVO4Surface in-situ growth of flaky ZnIn2S4The research of forming a compact heterostructure to degrade the organic pollutant TC has no literature report at home and abroad.
Disclosure of Invention
The invention provides a ZnIn2S4BiVO (BiVO) wrapped by nanosheets4The synthesis method of the micron rod core-shell heterojunction catalyst is used for efficiently catalyzing and degrading organic pollutants in water under visible light.
ZnIn2S4BiVO (BiVO) wrapped by nanosheets4The preparation method of the micron rod core-shell heterojunction catalyst comprises the following specific steps:
step one, BiVO4The preparation of (1):
adding Bi (NO)3)3·5H2Dissolving O in glycol to obtain a solution A; reacting NH4VO3Dissolving in deionized water to obtain solution B; slowly dripping the solution B into the solution A and stirring, transferring the obtained mixture into a polytetrafluoroethylene lining autoclave for constant-temperature thermal reaction, centrifuging the reacted solution, washing the centrifuged product with deionized water and absolute ethyl alcohol for multiple times, and drying in vacuum to obtain BiVO4A material;
step two, ZnIn2S4/BiVO4Preparing a composite photocatalyst:
weighing a certain mass of BiVO obtained according to the step one4Dispersing in glycerol and dilute hydrochloric acid solution, and sequentially adding ZnCl2、InCl3·4H2O and the thioacetamide, and the N-acetyl-L-methyl-N-methyl-ethyl-N-methyl-ethyl-N-methyl-ethyl-N-methyl-ethyl-methyl-N-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-N-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl,ultrasonic stirring to dissolve the ZnIn, putting the solution into an oil bath pot for constant temperature reaction, centrifuging the mixed solution after the reaction, washing the mixed solution for a plurality of times by deionized water and absolute ethyl alcohol, and drying the mixed solution in vacuum to finally obtain the ZnIn2S4/BiVO4Composite materials, i.e. ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Micron rod core-shell heterojunction catalyst.
Preparation of ZnIn2S4The material steps are the same as those of the second step, except that BiVO is not added4。
In step one, Bi (NO)3)3·5H2The dosage ratio of O to glycol is 1-3 mmol: 15-45 mL. NH (NH)4VO3The dosage ratio of the deionized water to the deionized water is 1-3 mmol: 15-45 mL.
In step one, Bi (NO)3)3·5H2O and NH4VO3The mass ratio of substances is 1: 1.
in the first step, the reaction temperature is 100-200 ℃, and the reaction time is 6-24 h.
In the second step, BiVO4The dosage ratio of the glycerol to the dilute hydrochloric acid solution is 0.05-0.2 mmol: 2-4 mL: 10-30 mL, wherein the pH value of the dilute hydrochloric acid solution is 1-4.
In the second step, BiVO4、ZnCl2、InCl3·4H2The dosage ratio of O to thioacetamide is 0.05-0.2 mmol:0.1 to 0.3mmol, 0.3 to 0.5 mmol.
In the second step, the temperature of the oil bath reaction is 60-100 ℃, and the reaction time is 1-6 h.
In the second step, the drying temperature is 40-60 ℃, and the drying time is 10-24 h.
ZnIn prepared by the invention2S4/BiVO4The photocatalyst is used for photocatalytic degradation of organic pollutants TC.
The beneficial effects of the invention are as follows:
the petal-shaped ZnIn prepared by the invention2S4Nano-sheet modified mulberry-shaped BiVO4On the surface, may be ZnIn2S4And BiVO4Between which a z-type heterojunction boundary is establishedThe unique interface synergistic characteristic not only can realize the spatial separation of redox centers, but also is beneficial to improving the reduction and oxidation capacities of photo-generated electrons and holes. Surface grown ZnIn2S4The nano sheet has larger specific surface area and can adsorb more pollutants to participate in the reaction. The combination of the two materials is beneficial to widening the absorption range of the material to visible light, thereby improving the utilization rate of the material to visible light. Under the irradiation of visible light, ZnIn2S4/BiVO4The composite material shows much higher ZnIn2S4And BiVO4The degradation performance of the two monomers is that the ZIS/BVO-0.10 composite material with the optimal proportion can degrade 60 percent of tetracycline under 3 hours of illumination.
Drawings
FIG. 1 is BiVO4、ZnIn2S4And ZnIn2S4/BiVO4XRD pattern of the composite.
FIG. 2 is BiVO4(a)、ZIS/BVO-0.10(b)、ZnIn2S4(c) ZIS/BVO-0.10 low power (d, e) and high power (f) transmission electron micrographs.
FIG. 3 is BiVO4、ZnIn2S4And ZnIn2S4/BiVO4The composite material degrades TC activity pattern under visible light.
Detailed description of the preferred embodiments
The invention will be described in more detail with reference to the drawings and the following examples, but the scope of the invention is not limited thereto.
Example 1:
(1) 1mmol of Bi (NO)3)3·5H2O was dissolved in 15ml of ethylene glycol to obtain a solution A. Adding 1mmol of NH4VO3Dissolved in 15ml of deionized water to give solution B. The solution B was slowly added dropwise to the solution A with stirring, and the resulting mixture was transferred to a 40ml Teflon-lined autoclave and heated at 140 ℃ for 24 h. Washing the reacted material with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain BiVO4A material.
(2) Weighing 0.05mmol of BiVO obtained according to the first step4Dispersed in 20ml of dilute hydrochloric acid solution at pH 2.5, 3ml of glycerol was added and stirred. Then 0.2mmol of ZnCl is added in turn2、0.2mmol InCl3·4H2O and 0.4mmol thioacetamide, and dissolving the thioacetamide by ultrasonic stirring. Putting the solution into an oil bath pan, heating at 80 ℃ for 2h, centrifuging the reacted mixed solution, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain ZnIn2S4/BiVO4The composite material was named ZIS/BVO-0.05.
Example 2:
(1) 1mmol of Bi (NO)3)3·5H2O was dissolved in 15ml of ethylene glycol to obtain a solution A. Adding 1mmol of NH4VO3Dissolved in 15ml of deionized water to give solution B. The solution B was slowly added dropwise to the solution A with stirring, and the resulting mixture was transferred to a 40ml Teflon-lined autoclave and heated at 140 ℃ for 24 h. Washing the reacted material with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain BiVO4A material.
(2) Weighing 0.10mmol of BiVO obtained according to the step one4Dispersed in 20ml of dilute hydrochloric acid solution at pH 2.5, 3ml of glycerol was added and stirred. Then 0.2mmol of ZnCl is added in turn2、0.2mmol InCl3·4H2O and 0.4mmol thioacetamide, and dissolving the thioacetamide by ultrasonic stirring. Putting the solution into an oil bath pan, heating at 80 ℃ for 2h, centrifuging the reacted mixed solution, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain ZnIn2S4/BiVO4The composite material was named ZIS/BVO-0.10.
Example 3:
(1) 1mmol of Bi (NO)3)3·5H2O was dissolved in 15ml of ethylene glycol to obtain a solution A. Adding 1mmol of NH4VO3Dissolved in 15ml of deionized water to give solution B. The solution B was slowly added dropwise to the solution A with stirring, and the resulting mixture was transferred to a 40ml Teflon-lined autoclave and heated at 140 ℃ for 24 h. The reacted material was washed 3 times with deionized water and absolute ethanol, respectively, inDrying at 60 ℃ for 10h to obtain BiVO4A material.
(2) Weighing 0.15mmol of BiVO obtained according to the step one4Dispersed in 20ml of dilute hydrochloric acid solution at pH 2.5, 3ml of glycerol are added and stirred. Then 0.2mmol of ZnCl is added in turn2、0.2mmol InCl3·4H2O and 0.4mmol thioacetamide, and dissolving the thioacetamide by ultrasonic stirring. Putting the solution into an oil bath pan, heating at 80 ℃ for 2h, centrifuging the reacted mixed solution, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain ZnIn2S4/BiVO4The composite material was named ZIS/BVO-0.15.
Example 4:
(1) 1mmol of Bi (NO)3)3·5H2O was dissolved in 15ml of ethylene glycol to obtain a solution A. 1mmol of NH4VO3Dissolved in 15ml of deionized water to give solution B. The solution B was slowly added dropwise to the solution A with stirring, and the resulting mixture was transferred to a 40ml Teflon-lined autoclave and heated at 140 ℃ for 24 h. Washing the reacted material with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain BiVO4A material.
(2) Weighing 0.20mmol of BiVO obtained according to the step one4Dispersed in 20ml of dilute hydrochloric acid solution at pH 2.5, 3ml of glycerol was added and stirred. Then 0.2mmol of ZnCl is added in turn2、0.2mmol InCl3·4H2O and 0.4mmol thioacetamide, and dissolving the thioacetamide by ultrasonic stirring. Putting the solution into an oil bath pan, heating at 80 ℃ for 2h, centrifuging the reacted mixed solution, washing with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 10h to obtain ZnIn2S4/BiVO4The composite material was named ZIS/BVO-0.20.
Example 5:
20ml of a dilute hydrochloric acid solution having a pH of 2.5 are weighed into a 50ml round-bottomed flask, 3ml of glycerol are added and stirred. Sequentially adding 0.2mmol of ZnCl2、0.2mmol InCl3·4H2O and 0.4mmol thioacetamide, and dissolving the thioacetamide by ultrasonic stirring. Putting the solution into an oil bath pan, heating at 80 deg.C for 2 hr, and reactingCentrifuging, washing with deionized water and anhydrous ethanol for 3 times respectively, and drying at 60 deg.C for 10 hr to obtain ZnIn2S4A material.
FIG. 1 is BiVO4、ZnIn2S4And ZnIn2S4/BiVO4XRD pattern of the composite. BiVO can be seen from the figure4、ZnIn2S4Two monomers have been successfully prepared, and only BiVO exists in the composite material4Without the characteristic peaks of ZnIn2S4Is a characteristic peak of (1), probably due to ZnIn2S4Too little load.
FIG. 2 is BiVO4(a)、ZIS/BVO-0.10(b)、ZnIn2S4(c) ZIS/BVO-0.10 low power (d, e) and high power (f) transmission electron micrographs; BiVO can be seen from the figure4The monomer is in a mulberry-like structure, ZnIn2S4ZnIn with a ball flower-shaped structure and a flower-shaped structure when the two materials are compounded2S4Uniformly growing in BiVO4A surface between which an intimate contact is formed.
FIG. 3 is BiVO4、ZnIn2S4And ZnIn2S4/BiVO4The composite material degrades TC activity under visible light. After 3 hours of light irradiation, the removal efficiency of ZIS/BVO-0.10 material with the best performance in the composite material on TC is 60 percent compared with BiVO4And ZnIn2S4The monomer performance is improved by 34 percent and 15 percent. Thus, by constructing ZnIn2S4/BiVO4The composite material effectively improves the photocatalytic degradation efficiency of the material on organic pollutants TC.

Claims (9)

1. ZnIn2S4BiVO (BiVO) wrapped by nanosheets4The preparation method of the micron rod core-shell heterojunction catalyst is characterized by comprising the following steps of:
step one, BiVO4The preparation of (1):
adding Bi (NO)3)3·5H2Dissolving O in glycol to obtain a solution A; reacting NH4VO3Dissolving in deionized waterAdding water to obtain solution B; slowly dripping the solution B into the solution A and stirring, transferring the obtained mixture into a polytetrafluoroethylene lining autoclave for constant-temperature thermal reaction, centrifuging the reacted solution, washing the centrifuged product with deionized water and absolute ethyl alcohol for multiple times, and drying in vacuum to obtain BiVO4A material;
step two, ZnIn2S4/BiVO4Preparing a composite photocatalyst:
weighing a certain mass of BiVO obtained according to the step one4Dispersing in glycerol and dilute hydrochloric acid solution, and sequentially adding ZnCl2、InCl3·4H2Dissolving O and thioacetamide by ultrasonic stirring, putting the solution into an oil bath pan for constant-temperature reaction, centrifuging the reacted mixed solution, washing the mixed solution by deionized water and absolute ethyl alcohol for multiple times, and drying the mixed solution in vacuum to finally obtain ZnIn2S4/BiVO4Composite materials, i.e. ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Micron rod core-shell heterojunction catalyst.
2. The method according to claim 1, wherein in the first step, Bi (NO)3)3·5H2The ratio of O to ethylene glycol is 1-3 mmol: 15-45 mL, NH4VO3The ratio of the deionized water to the deionized water is 1-3 mmol: 15-45 mL.
3. The method according to claim 1, wherein in the first step, Bi (NO)3)3·5H2O and NH4VO3The mass ratio of substances is 1: 1.
4. the preparation method according to claim 1, wherein in the first step, the reaction temperature is 100-200 ℃ and the reaction time is 6-24 h.
5. The method according to claim 1, wherein in step two, BiVO is prepared4The dosage ratio of the glycerol to the dilute hydrochloric acid solution is 0.05-0.2 mmol: 2-4 mL: 10 to 30mL, wherein,the pH value of the dilute hydrochloric acid solution is 1-4.
6. The method according to claim 1, wherein in step two, BiVO is prepared4、ZnCl2、InCl3·4H2The dosage ratio of O to thioacetamide is 0.05-0.2 mmol: 0.1-0.3 mmol: 0.1-0.3 mmol:0.3 to 0.5 mmol.
7. The preparation method according to claim 1, wherein in the second step, the temperature of the oil bath reaction is 60 to 100 ℃ and the reaction time is 1 to 6 hours.
8. The preparation method according to claim 1, wherein in the second step, the drying temperature is 40-60 ℃ and the drying time is 10-24 h.
9. ZnIn prepared according to the method of any one of claims 1 to 82S4BiVO (BiVO) wrapped by nanosheets4The micron rod core-shell heterojunction catalyst is applied to photocatalytic degradation of TC in water.
CN202210138208.4A 2022-02-15 2022-02-15 ZnIn2S4BiVO (BiVO) wrapped by nanosheets4Preparation method and application of micron rod core-shell heterojunction catalyst Pending CN114653381A (en)

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CN116440926A (en) * 2023-04-28 2023-07-18 重庆工商大学 Modified ZnIn 2 S 4 /BiVO 4 Heterojunction between benzyl alcohol and CO 2 Application in photocatalytic carboxylation

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