CN114289038A - BiOCl rich in defects0.5I0.5Solid solution photocatalyst and preparation method and application thereof - Google Patents
BiOCl rich in defects0.5I0.5Solid solution photocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a BiOCl rich in defects0.5I0.5Solid solution photocatalyst, preparation method and application thereof, and defect-rich BiOCl0.5I0.5The solid solution photocatalyst is prepared by the preparation method, is in a nano sheet shape, and has the thickness of 0.83 nm. The preparation method comprises the following steps: dispersing a proper amount of bismuth nitrate pentahydrate and polyvinylpyrrolidone into a mannitol aqueous solution to prepare a solution A; dispersing a proper amount of ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide into a mannitol solution to prepare a solution B; dropwise adding the obtained solution B into the solution A, and continuously stirring at room temperature; pouring the obtained mixed solution into a container with polytetrafluoroethylene liningPressing the mixture in a reaction kettle, and heating for reaction; centrifuging the obtained product, washing with deionized water and absolute ethyl alcohol for several times respectively, and drying to obtain defect-rich BiOCl0.5I0.5A solid solution photocatalyst can be used for degrading ciprofloxacin by photocatalysis.
Description
Technical Field
The invention relates to a preparation method of a photocatalytic material, and particularly relates to BiOCl0.5I0.5A method for preparing solid solution photocatalyst.
Background
Nowadays, the rapid development of industry promotes the progress of science and technology and society, and meanwhile, the problems of energy crisis, environmental pollution and the like are brought, wherein the water environment pollution influences the balance of an ecological system and seriously threatens the life and survival of human beings and organisms. Therefore, it is urgent to take necessary measures and techniques to solve the existing water pollution problem. In recent years, photocatalytic water treatment is a new advanced oxidation technology, and can realize wastewater treatment and deep purification of drinking water by taking solar energy as a direct driving force.
BiOX as a novel photocatalyst has received increasing attention in research on photocatalytic degradation of pollutants due to its stable layered structure and highly tunable energy band structure. However, the BiOX intrinsic material still has limitations, limiting its further applications, and therefore, the BiOX material still needs to be modified to obtain higher photocatalytic activity and expand its practical applications. At present, modification strategies aiming at the BiOX material mainly focus on energy band position regulation, morphology regulation, surface characteristic regulation, heterojunction construction and the like. The solid solution structure is constructed to attract the attention of researchers, and different from pure-phase BiOX, the bismuth oxyhalide-based solid solution material contains more than two halogen atoms, and the advantages of each BiOX are integrated and exerted to the maximum extent by adjusting the electronic state structure of the BiOX, so that the visible light absorption of a wide spectrum and the redox capability of an intrinsic photocatalyst are enhanced. In addition, it is considered that the introduction of oxygen vacancies can change the electronic structure of the surface of the oxygen-containing compound, and local electrons abundant on the oxygen vacancies can also serve as adsorption centers in the photoreaction process. Therefore, the bismuth oxyhalide solid solution photocatalyst with abundant surface oxygen vacancies is designed and prepared, and is expected to obtain excellent photocatalytic performance.
Disclosure of Invention
The invention aims to provide a BiOCl rich in defects0.5I0.5The preparation method of solid solution photocatalyst is used for treating water environment pollution.
BiOCl rich in defects0.5I0.5The preparation method of the solid solution photocatalytic material comprises the following steps:
s1, dispersing a proper amount of bismuth nitrate pentahydrate and polyvinylpyrrolidone into the mannitol aqueous solution to prepare a solution A;
s2, dispersing a proper amount of ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide into a mannitol solution to prepare a solution B;
s3, dropwise adding the solution B obtained in the step S2 into the solution A of the step S1, and continuously stirring at room temperature;
s4, pouring the mixed solution obtained in the step S3 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction;
s5 centrifuging the product obtained in S4, washing with deionized water and absolute ethyl alcohol for several times respectively, and drying to obtain defect-rich BiOCl0.5I0.5A solid solution photocatalyst.
Preferably, the dosage of the bismuth nitrate pentahydrate in S1 is 0.5-1mmol, the addition amount of the polyvinylpyrrolidone is 0.2-0.8g, the concentration of the mannitol aqueous solution is 0.01-0.15mol/L, and the addition amount of the mannitol aqueous solution is 0.005-0.015L.
Preferably, the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide added is 0.5-1 mmol.
Preferably, the concentration of the mannitol aqueous solution in S2 is 0.01-0.15 mol/L.
Preferably, the amount of the aqueous mannitol solution described in S2 is 0.005-0.015L.
Preferably, the stirring time at room temperature in S3 is 5 to 60 minutes.
Preferably, the reaction temperature in S3 is 120-180 ℃, and the reaction time is 5-24 h.
Preferably, the drying temperature in S4 is 60 ℃, and the drying time is 12-24 h.
Preferably, a defect-rich BiOCl0.5I0.5The solid solution photocatalyst is prepared by any one of the preparation methods, is in a nano sheet shape, and has the thickness of 0.83 nm.
Preferably, the BiOCl is rich in defects0.5I0.5The solid solution photocatalyst is used for degrading ciprofloxacin by photocatalysis.
Has the advantages that:
the invention is synthesized by an ionic liquid auxiliary solvent thermal method, bismuth nitrate pentahydrate is taken as a bismuth source, ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide are taken as halogen sources, and BiOCl with different oxygen vacancy concentrations is prepared0.5I0.5A solid solution photocatalyst. The preparation method disclosed by the invention is simple to operate, green and environment-friendly, and high in catalytic efficiency of photocatalytic degradation of organic antibiotic ciprofloxacin.
Drawings
FIG. 1 is a graph of BiOCl with different oxygen vacancy concentrations0.5I0.5XRD pattern of solid solution photocatalyst;
FIG. 2 is a high concentration oxygen vacancy BiOCl0.5I0.5TEM image of solid solution photocatalyst I;
FIG. 3 is BiOCl of low concentration oxygen vacancies0.5I0.5Solid solution photocatalyst HRTEM;
FIG. 4 is a high concentration oxygen vacancy BiOCl0.5I0.5TEM image of solid solution photocatalyst II;
FIG. 5 is the HRTEM image I of FIG. 4;
FIG. 6 is a HRTEM image II of FIG. 4;
FIG. 7 is a BiOCl with a high concentration of oxygen vacancies0.5I0.5AFM thickness profile of solid solution photocatalysts;
FIG. 8 is a BiOCl with a high concentration of oxygen vacancies0.5I0.5AFM profiles of solid solution photocatalysts;
FIG. 9 is BiOCl with different oxygen vacancy concentrations0.5I0.5The CIP activity diagram of the solid solution photocatalyst in photocatalytic degradation under long-wavelength light irradiation.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
The first embodiment is as follows:
bismuth nitrate pentahydrate is used as a raw material, the bismuth nitrate pentahydrate and polyvinylpyrrolidone are dispersed in 0.005-0.015L of mannitol solution to prepare solution A, wherein the dosage of the bismuth nitrate pentahydrate is 0.5-1mmol, the dosage of the polyvinylpyrrolidone is 0.2-0.8g, the concentration of the mannitol aqueous solution is 0.01-0.15mol/L, then ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide are used as halogen sources, the ionic liquid 1-butyl-3-methylimidazolium chloride and the ionic liquid 1-butyl-3-methylimidazolium iodide are dispersed in 0.005-0.015L of the mannitol solution to prepare solution B, the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and the ionic liquid 1-butyl-3-methylimidazolium iodide is 0.5-1mmol, the concentration of the mannitol aqueous solution is 0.01-0.15mol/L, the solution B is dripped into the solution A, and continuously stirring at room temperature for 5-60 min, pouring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction at the temperature of 120-180 ℃ for 5-24 h. Centrifuging the obtained product, washing with deionized water and anhydrous ethanol for several times, and drying at 60 deg.C for 12-24 hr.
Example two:
bismuth nitrate pentahydrate is used as a raw material, the bismuth nitrate pentahydrate and polyvinylpyrrolidone are dispersed in 0.01L of mannitol solution to prepare solution A, the dosage of the bismuth nitrate pentahydrate is 1mmol, the dosage of the polyvinylpyrrolidone is 0.2g, the concentration of the mannitol aqueous solution is 0.15mol/L, then ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide are used as halogen sources and are dispersed in 0.01L of mannitol solution to prepare solution B, the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide is 1mmol, the concentration of the mannitol aqueous solution is 0.15mol/L, the solution B is dripped into the solution A and is continuously stirred at room temperature, wherein the stirring time at room temperature is 10 minutes, pouring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction at the temperature of 140 ℃ for 12 hours. Centrifuging the obtained product, washing with deionized water and anhydrous ethanol for several times, and drying at 60 deg.C for 20 hr.
Example three:
bismuth nitrate pentahydrate is used as a raw material, the bismuth nitrate pentahydrate and polyvinylpyrrolidone are dispersed in 0.01L of mannitol solution to prepare solution A, the dosage of the bismuth nitrate pentahydrate is 1mmol, the dosage of the polyvinylpyrrolidone is 0.2g, the concentration of the mannitol aqueous solution is 0.15mol/L, then ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide are used as halogen sources and are dispersed in 0.01L of mannitol solution to prepare solution B, the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide is 1mmol, the concentration of the mannitol aqueous solution is 0.15mol/L, the solution B is dripped into the solution A and is continuously stirred at room temperature, wherein the stirring time at room temperature is 60 minutes, pouring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction at 160 ℃ for 20 hours. Centrifuging the obtained product, washing with deionized water and anhydrous ethanol for several times, and drying at 60 deg.C for 20 hr.
Example four:
bismuth nitrate pentahydrate is used as a raw material, the bismuth nitrate pentahydrate and polyvinylpyrrolidone are dispersed in 0.01L of mannitol solution to prepare solution A, the dosage of the bismuth nitrate pentahydrate is 1mmol, the dosage of the polyvinylpyrrolidone is 0.2g, the concentration of the mannitol aqueous solution is 0.15mol/L, then ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide are used as halogen sources and are dispersed in 0.01L of mannitol solution to prepare solution B, the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide is 1mmol, the concentration of the mannitol aqueous solution is 0.15mol/L, the solution B is dripped into the solution A and is continuously stirred at room temperature, wherein the stirring time at room temperature is 60 minutes, pouring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction at 180 ℃ for 24 hours. Centrifuging the obtained product, washing with deionized water and anhydrous ethanol for several times, and drying at 60 deg.C for 20 hr.
Comparative example:
a step of preparing a biocl0.5i0.5 solid solution photocatalyst having a low concentration of oxygen vacancies: adding 1mmol of bismuth nitrate pentahydrate into 10mL of absolute ethyl alcohol to prepare solution A, adding 1mmol of inorganic salt potassium iodide and potassium chloride into 5mL of absolute ethyl alcohol in another container to prepare solution B, dropwise adding the solution B into the solution A under the condition that the solution A is stirred for 30 minutes at room temperature, pouring the solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction at 160 ℃ for 24 hours. Centrifuging the obtained product, washing with deionized water and anhydrous ethanol for several times, and drying at 60 deg.C for 20 hr.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. BiOCl rich in defects0.5I0.5The preparation method of the solid solution photocatalytic material is characterized by comprising the following steps:
s1, dispersing a proper amount of bismuth nitrate pentahydrate and polyvinylpyrrolidone into the mannitol aqueous solution to prepare a solution A;
s2, dispersing a proper amount of ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide into a mannitol solution to prepare a solution B;
s3, dropwise adding the solution B obtained in the step S2 into the solution A of the step S1, and continuously stirring at room temperature;
s4, pouring the mixed solution obtained in the step S3 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and heating for reaction;
s5 centrifuging the product obtained in S4, washing with deionized water and absolute ethyl alcohol for several times respectively, and drying to obtain defect-rich BiOCl0.5I0.5A solid solution photocatalyst.
2. The defect-rich BiOCl of claim 10.5I0.5The preparation method of the solid solution photocatalysis material is characterized in that the dosage of the bismuth nitrate pentahydrate in S1 is 0.5-1mmol, the addition amount of the polyvinylpyrrolidone is 0.2-0.8g, the concentration of the mannitol aqueous solution is 0.01-0.15mol/L, and the addition amount of the mannitol aqueous solution is 0.005-0.015L.
3. The defect-rich BiOCl of claim 10.5I0.5The preparation method of the solid solution photocatalysis material is characterized in that the total amount of the ionic liquid 1-butyl-3-methylimidazolium chloride and 1-butyl-3-methylimidazolium iodide is 0.5-1 mmol.
4. The defect-rich BiOCl of claim 10.5I0.5A method for producing a solid solution photocatalytic material, characterized in that the concentration of the aqueous mannitol solution in S2 is 0.01 to 0.15 mol/L.
5. The defect-rich BiOCl of claim 10.5I0.5A method for producing a solid solution photocatalyst, characterized in that the amount of the aqueous mannitol solution added to S2 is 0.005 to 0.015L.
6. The defect-rich BiOCl of claim 10.5I0.5A method for producing a solid solution photocatalytic material, characterized in that the stirring time at room temperature in S3 is 5 to 60 minutes.
7. The defect-rich BiOCl of claim 10.5I0.5The preparation method of the solid solution photocatalytic material is characterized in that the reaction temperature in S3 is 120-180 ℃, and the reaction time is 5-24 h.
8. The method of claim 1BiOCl rich in defects0.5I0.5The preparation method of the solid solution photocatalytic material is characterized in that the drying temperature in S4 is 60 ℃, and the drying time is 12-24 h.
9. BiOCl rich in defects0.5I0.5A solid solution photocatalyst produced by the production method according to any one of claims 1 to 8, which is in the form of nanosheets having a thickness of 0.83 nm.
10. Subjecting the defect-rich BiOCl of claim 90.5I0.5The solid solution photocatalyst is used for degrading ciprofloxacin by photocatalysis.
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