CN107638886B - Method for preparing bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by ion exchange method - Google Patents

Method for preparing bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by ion exchange method Download PDF

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CN107638886B
CN107638886B CN201710721493.1A CN201710721493A CN107638886B CN 107638886 B CN107638886 B CN 107638886B CN 201710721493 A CN201710721493 A CN 201710721493A CN 107638886 B CN107638886 B CN 107638886B
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bismuth
solution
bismuth oxychloride
nanosheet
ultrathin
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CN107638886A (en
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武大鹏
王晓璐
安义鹏
徐芳
高志永
蒋凯
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Henan Normal University
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Abstract

The invention discloses a method for preparing a bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by an ion exchange method, which comprises the steps of dissolving bismuth nitrate pentahydrate and polyvinylpyrrolidone in an ethylene glycol solution, stirring at room temperature until the bismuth nitrate pentahydrate and the polyvinylpyrrolidone are completely dissolved, adding a saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the white turbid solution into a hydrothermal reaction kettle to react at 140-180 ℃, performing vacuum drying at 60 ℃ to obtain a product of the bismuth oxychloride ultrathin nanosheet, dispersing the bismuth oxychloride ultrathin nanosheet into a saturated potassium iodide solution, and stirring at 25-50 ℃ for 3-12 hours to obtain a target product of the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet. The method is simple and easy to operate and good in repeatability, the synthesized bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet has an ultrathin two-dimensional structure, the specific surface area is large, the band gap of the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet is appropriate, and the photoresponse range is wide, so that the method has a good application prospect in the related fields of optics, electricity, thermodynamics and the like.

Description

Method for preparing bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by ion exchange method
Technical Field
The invention belongs to the technical field of synthesis of composite photocatalytic materials, and particularly relates to a method for preparing a bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by an ion exchange method.
Background
In recent years, environmental pollution and energy shortage are major challenges facing human beings at present. The photocatalysis technology can directly utilize solar energy as light drive to carry out normal-temperature deep reaction, thereby having wide development prospect in the aspects of environmental purification and new energy development. The semiconductor oxide is used as a catalyst to convert light energy into electric energy and chemical energy, so that an ideal method for energy utilization and environmental pollution treatment is provided for people. However, the main problems in the research of semiconductor photocatalysts are high recombination probability of photo-generated electron-hole pairs and narrow photoresponse range.
The bismuth-based photocatalytic material has a special layered structure and a narrow forbidden band width, and therefore, separation of electrons and holes occurs under irradiation of visible light. At present, bismuth-based photocatalysts mainly comprise bismuth oxide, bismuth oxyhalide, bismuth oxysalt, a composite bismuth catalyst and the like, wherein the most representative is bismuth oxyhalide (BiOX, X = F, Cl, Br and I) series compounds, and the bismuth-based photocatalysts have potential practical values due to the advantages of low price, high photocatalytic performance, good stability and the like; the bismuth oxychloride has good and stable photocatalytic activity due to the highly anisotropic laminated structure, but the forbidden bandwidth is wide; the bismuth oxyiodide has the smallest band gap, has a unique structure with an open structure and an indirect transition mode, is favorable for effective separation of hole-electron pairs and charge transfer, and has very high visible light photocatalytic activity.
The patent with the application number of CN201210082112.7 discloses a preparation method of porous bismuth oxyiodide nano photocatalysis, which mainly aims to solve the technical problem that the existing bismuth oxyiodide has poor photodegradability in a visible light region, but the preparation process of the method is complicated, a large amount of organic solvent is used, the method is not beneficial to large-scale production, in addition, the method only prepares the bismuth oxyiodide with slightly large specific surface area, the photocatalysis performance of the bismuth oxyiodide is not fundamentally changed, and the promotion space is limited. The patent with publication number CN101724839A provides a method for preparing a BiOCl film by vapor deposition and chemical oxidation, and the prepared film has a flower-like structure, but the preparation process needs a complicated physical vapor deposition process, needs special instruments and equipment and uses high-purity gas as shielding gas, and has high cost and complicated operation. The patent with publication number CN101857382A adopts a continuous ion layer adsorption reaction method to prepare a BiOI thin film electrode, which has application potential in the field of solar cells, but the method needs to be repeated many times to prepare the required thin film, and the operation process is complicated. The patent publication No. CN 102974373A discloses a preparation method of a bismuth oxychloride/bismuth oxyiodide heterojunction visible light catalytic material, which mainly aims to provide a material with high catalytic activity and stability, but the preparation of a precursor bismuth oxychloride is time-consuming and long, and the subsequent reaction with bismuth oxyiodide is also required to be calcined, so that the formed nanosheet is thick and is not beneficial to effective separation of electron-hole.
Disclosure of Invention
The invention solves the technical problem of providing a method for preparing the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheets by an ion exchange method, which has simple preparation process and easily controlled conditions.
The invention adopts the following technical scheme for solving the technical problems, and the method for preparing the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by using the ion exchange method is characterized by comprising the following specific steps of: dissolving 0.2-0.6g of pentahydrate bismuth nitrate and 0.3-0.8g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the pentahydrate bismuth nitrate and the polyvinylpyrrolidone are completely dissolved, adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle to react at 140-180 ℃ for 3-6h, cooling to room temperature, centrifuging to respectively wash white precipitates generated by the reaction with deionized water and ethanol, performing vacuum drying at 60 ℃ to obtain a product bismuth oxychloride ultrathin nanosheet, dispersing 0.1-2g of the prepared bismuth oxychloride ultrathin nanosheet into 10-50mL of saturated potassium iodide solution, and stirring at 25-50 ℃ for 3-12h to obtain the target product bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet.
Further preferably, the preparation method of the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet is characterized by comprising the following specific steps: dissolving 0.486g of bismuth nitrate pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth nitrate pentahydrate and the polyvinylpyrrolidone are completely dissolved, adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3h at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by the reaction with deionized water and ethanol respectively, drying in vacuum at 60 ℃ to obtain the product ultrathin bismuth oxychloride nanosheet, dispersing 0.1-2g of the prepared ultrathin bismuth oxychloride nanosheet into 10-50mL of saturated potassium iodide solution, and stirring at 25-50 ℃ for 3-12h to obtain the target product ultrathin bismuth oxychloride/iodine oxidation composite nanosheet.
Compared with the prior art, the invention has the following beneficial effects: the method is simple and easy to operate and good in repeatability, the synthesized bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet has an ultrathin two-dimensional structure, the specific surface area is large, the band gap of the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet is appropriate, and the photoresponse range is wide, so that the method has a good application prospect in the related fields of optics, electricity, thermodynamics and the like.
Drawings
FIG. 1 is an SEM image of an ultrathin bismuth oxychloride nanosheet prepared in comparative example 1, with the magnification of the image being 20000 times and 5000 times respectively;
FIG. 2 is an SEM image of the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet prepared in example 1, with the magnification of the image being 2000 times and 10000 times respectively;
FIG. 3 is XRD patterns of the ultrathin bismuth oxychloride nanosheets prepared in comparative example 1 and the ultrathin bismuth oxychloride/bismuth oxyiodide nanosheets prepared in example 1.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Dissolving 0.486g of bismuth pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth pentahydrate and the polyvinylpyrrolidone are completely dissolved, slowly adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3h at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by the reaction with deionized water and ethanol respectively, drying at 60 ℃ in vacuum to obtain a product of bismuth oxychloride ultrathin nanosheet, dispersing 0.1g of the prepared bismuth oxychloride ultrathin nanosheet into 15mL of saturated potassium iodide solution, stirring at room temperature for 3h, and drying at 60 ℃ in vacuum to obtain the target product of bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet BOC/BOI-NS 1.
Example 2
Dissolving 0.486g of bismuth pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth pentahydrate and the polyvinylpyrrolidone are completely dissolved, slowly adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3h at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by the reaction with deionized water and ethanol respectively, drying at 60 ℃ in vacuum to obtain a product bismuth oxychloride ultrathin nanosheet, dispersing 0.5g of the prepared bismuth oxychloride ultrathin nanosheet into 50mL of saturated potassium iodide solution, stirring in a water bath at 40 ℃ for 6h, and drying at 60 ℃ in vacuum to obtain the target product bismuth oxychloride/bismuth iodide composite ultrathin nanosheet BOC/BOI-NS 2.
Example 3
Dissolving 0.486g of bismuth pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth pentahydrate and the polyvinylpyrrolidone are completely dissolved, slowly adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3h at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by the reaction with deionized water and ethanol respectively, drying at 60 ℃ in vacuum to obtain a product bismuth oxychloride ultrathin nanosheet, dispersing 2g of the prepared bismuth oxychloride ultrathin nanosheet into 50mL of saturated potassium iodide solution, stirring in a 50 ℃ water bath for 12h, and drying at 60 ℃ in vacuum to obtain the target product, namely the bismuth oxychloride/bismuth oxyiodide composite nanosheet BOC/BOI-NS 3.
Comparative example 1
Dissolving 0.486g of bismuth pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth pentahydrate and the polyvinylpyrrolidone are completely dissolved, slowly adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3 hours at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by reaction with deionized water and ethanol respectively, and then performing vacuum drying at 60 ℃ to obtain the product, namely the bismuth oxychloride ultrathin nanosheet BOC.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.

Claims (2)

1. The method for preparing the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by using the ion exchange method is characterized by comprising the following specific steps of: dissolving 0.2-0.6g of pentahydrate bismuth nitrate and 0.3-0.8g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the pentahydrate bismuth nitrate and the polyvinylpyrrolidone are completely dissolved, adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle to react at 140-180 ℃ for 3-6h, cooling to room temperature, centrifuging to respectively wash white precipitates generated by the reaction with deionized water and ethanol, performing vacuum drying at 60 ℃ to obtain a product bismuth oxychloride ultrathin nanosheet, dispersing 0.1-2g of the prepared bismuth oxychloride ultrathin nanosheet into 10-50mL of saturated potassium iodide solution, and stirring at 25-50 ℃ for 3-12h to obtain the target product bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet.
2. The method for preparing the bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet by the ion exchange method according to claim 1, which is characterized by comprising the following specific steps: dissolving 0.486g of bismuth pentahydrate and 0.4g of polyvinylpyrrolidone in 25mL of ethylene glycol solution, stirring at room temperature until the bismuth pentahydrate and the polyvinylpyrrolidone are completely dissolved, adding 5mL of saturated sodium chloride solution into the solution, continuously stirring to obtain a white turbid solution, transferring the obtained white turbid solution into a hydrothermal reaction kettle, reacting for 3h at 160 ℃, cooling to room temperature, centrifuging, washing white precipitates generated by the reaction with deionized water and ethanol respectively, drying at 60 ℃ in vacuum to obtain the product ultrathin bismuth oxychloride nanosheet, dispersing 0.1-2g of the prepared ultrathin bismuth oxychloride nanosheet into 10-50mL of saturated potassium iodide solution, and stirring at 25-50 ℃ for 3-12h to obtain the target product bismuth oxychloride/bismuth oxyiodide composite ultrathin nanosheet.
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CN108722446A (en) * 2018-06-14 2018-11-02 河南师范大学 A kind of preparation method of three-dimensional structure bismuth oxychloride@bismuth oxybromide composite ultra-thin nanometer sheets
CN108906085A (en) * 2018-07-17 2018-11-30 河南师范大学 A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material
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