CN107308957B - Spherical Bi2S3/Bi2WO6Preparation method of heterojunction photocatalytic material - Google Patents
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
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- 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 9
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Abstract
本发明公开了一种球状Bi2S3/Bi2WO6异质结光催化材料的制备方法，属于光催化材料的合成技术领域。本发明的技术方案要点为：一种球状Bi2S3/Bi2WO6异质结光催化材料的制备方法，具体包括球状Bi2WO6的制备和球状Bi2S3/Bi2WO6异质结光催化材料的制备等步骤，该球状Bi2S3/Bi2WO6异质结光催化材料是由Bi2WO6纳米片和Bi2S3纳米棒组成的粒径为3‑5μm的球状颗粒。本发明采用水热法和离子交换法合成球状Bi2S3/Bi2WO6异质结光催化材料，将两者复合充分发挥两种材料的优势，弥补彼此之间的缺点，既能有效促进电子与空穴的分离，又能拓宽复合材料对光的吸收范围，从而提高了铋系半导体光催化材料的能效及催化效率，表现出较高的可见光催化性能。
The invention discloses a preparation method of a spherical Bi 2 S 3 /Bi 2 WO 6 heterojunction photocatalytic material, which belongs to the technical field of photocatalytic material synthesis. The main point of the technical solution of the present invention is: a preparation method of spherical Bi 2 S 3 /Bi 2 WO 6 heterojunction photocatalytic material, which specifically includes the preparation of spherical Bi 2 WO 6 and spherical Bi 2 S 3 /Bi 2 WO 6 Steps such as the preparation of a heterojunction photocatalytic material, the spherical Bi 2 S 3 /Bi 2 WO 6 heterojunction photocatalytic material is composed of Bi 2 WO 6 nanosheets and Bi 2 S3 nanorods with a particle size of 3‑ 5μm spherical particles. The invention adopts the hydrothermal method and the ion exchange method to synthesize spherical Bi 2 S 3 /Bi 2 WO 6 heterojunction photocatalytic material, and the two materials are combined to give full play to the advantages of the two materials and make up for the shortcomings of each other, which can not only effectively The separation of electrons and holes is promoted, and the light absorption range of the composite material can be broadened, thereby improving the energy efficiency and catalytic efficiency of the bismuth-based semiconductor photocatalytic material, and showing high visible light catalytic performance.
Description
Technical Field
The invention belongs to the technical field of synthesis of photocatalytic materials, and particularly relates to spherical Bi2S3/Bi2WO6A preparation method of a heterojunction photocatalytic material.
Background
With the development of social economy, the three problems of environment, materials and energy are more and more prominent, and the photocatalytic technology has the characteristics of low cost, environmental friendliness and the like, so that more and more scientific researchers utilize the photocatalytic technology to solve the three problems. The photocatalytic technology mainly depends on a photocatalytic material, a single-component photocatalyst is difficult to effectively utilize visible light and ultraviolet light simultaneously, and the photo-generated electron-hole recombination probability is high, so that the photocatalytic activity is limited.
Bi2WO6Has a relatively simple crystal structure, is a typical n-type semiconductor material, and is composed of (Bi)2O2)2+And (WO)6)2-The oxide of the layered perovskite structure with the alternating composition can provide a place for photocatalysis. And Bi2WO6The valence band potential is 3.18eV, the conduction band is 0.54eV, and the forbidden band width is about 2.64eV, which shows that the bismuth tungstate can only utilize a small amount of visible light. As a typical bismuth-based multifunctional material, Bi2S3The band gap width of the material is between 1.2 and 1.7eV, and the material is easily excited to generate photo-generated electron-hole pairs under the irradiation of visible light, but is easy to recombine and is unstable in the reaction process.
Bi2S3/Bi2WO6Heterojunction photocatalytic material fully utilizes Bi2S3And Bi2WO6The synergistic effect of the two elements makes up the defects of the two elements, effectively promotes the separation of electrons and holes, widens the absorption range of the composite material to light, and improves the energy efficiency and the catalytic efficiency of the bismuth semiconductor photocatalytic material, but no synthetic spherical Bi2S3/Bi2WO6Heterojunction photocatalytic materialThe related report on the improvement of the photocatalytic performance of the material.
Disclosure of Invention
The invention solves the technical problem of providing the spherical Bi which is simple to operate, environment-friendly and has good visible light catalytic activity2S3/Bi2WO6A preparation method of a heterojunction photocatalytic material.
The invention adopts the following technical scheme to solve the technical problems2S3/Bi2WO6The preparation method of the heterojunction photocatalytic material is characterized by comprising the following specific steps:
(1) spherical Bi2WO6Dissolving polyvinylpyrrolidone and pentahydrate bismuth nitrate in a mixed solution of ethanol, glacial acetic acid and deionized water, stirring for 15min at room temperature to obtain a solution A, dissolving sodium tungstate dihydrate in deionized water to obtain a solution B, adding the solution B into the solution A under the stirring state, uniformly mixing, transferring the mixed solution into a reaction kettle, reacting for 3h at 180 ℃, cooling to room temperature, repeatedly washing precipitates with water and absolute ethyl alcohol, and then drying in vacuum at 60 ℃ to obtain spherical Bi stacked in sheets2WO6；
(2) Spherical Bi2S3/Bi2WO6Preparation of heterojunction photocatalytic material by mixing spherical Bi2WO6Dispersing in deionized water, and sequentially adding mercaptopropionic acid and thioacetamide, wherein Bi is2WO6The feeding molar ratio of the precipitate to thioacetamide is 2:1, the pH value of the mixed solution is adjusted to 10.5 by using a sodium hydroxide solution after the mixture is uniformly stirred and mixed, the mixed solution is transferred into a reaction kettle to react for 3 hours at 180 ℃, the obtained precipitate is centrifugally separated, washed by deionized water and absolute ethyl alcohol and then dried in vacuum at 60 ℃ to obtain spherical Bi2S3/Bi2WO6A heterojunction photocatalytic material, the spherical Bi2S3/Bi2WO6The heterojunction photocatalytic material is made of Bi2WO6Nanosheet and Bi2S3The nano rods form spherical particles with the particle size of 3-5 mu m.
Further preferably, in the step (1), the feeding molar ratio of the bismuth nitrate pentahydrate to the sodium tungstate dihydrate is 2:1, the volume ratio of the ethanol to the glacial acetic acid to the deionized water is 1:1:3, the feeding ratio of the bismuth nitrate pentahydrate to the ethanol is 1mmol:5mL, and the feeding ratio of the polyvinylpyrrolidone to the bismuth nitrate pentahydrate is 0.2g:1 mmol.
The invention adopts a hydrothermal method and an ion exchange method to synthesize spherical Bi2S3/Bi2WO6Heterojunction photocatalytic material, Bi2WO6Low visible light catalytic performance, Bi2S3Has excellent visible light response, but pure Bi2S3The electron-hole pairs are difficult to separate, the advantages and the disadvantages of the two photocatalytic materials are combined, the advantages of the two materials are fully exerted, the disadvantages of the two materials are made up, the separation of electrons and holes can be effectively promoted, the absorption range of the composite material to light can be widened, the energy efficiency and the catalytic efficiency of the bismuth semiconductor photocatalytic material are improved, and the bismuth semiconductor photocatalytic material has high visible light catalytic performance. The synthetic process is simple in process, green and environment-friendly, is suitable for large-scale production, and is expected to produce good social and economic benefits.
Drawings
FIG. 1 shows Bi obtained in example 1 of the present invention2S3/Bi2WO6FESEM images of heterojunction photocatalytic materials;
FIG. 2 shows Bi obtained in example 1 of the present invention2S3/Bi2WO6UV-Vis DRS spectra of the heterojunction photocatalytic material;
FIG. 3 shows Bi obtained in example 1 of the present invention2S3/Bi2WO6An XRD spectrum of the heterojunction photocatalytic material;
FIG. 4 shows Bi obtained in example 1 of the present invention2S3/Bi2WO6The heterojunction photocatalytic material degrades the ultraviolet visible absorption spectrum change curve of ciprofloxacin under the irradiation of visible light.
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
Weighing 0.2g of polyvinylpyrrolidone (PVP) and 1mmol of bismuth nitrate pentahydrate, dissolving the mixture in a mixed solution of 5mL of ethanol, 5mL of glacial acetic acid and 15mL of deionized water, stirring the mixture at room temperature for 15min to obtain a solution A, dissolving 0.5mmol of sodium tungstate dihydrate into 10mL of deionized water to obtain a solution B, slowly adding the solution B into the solution A while stirring, stirring the solution for 30min again to ensure that reaction reagents are uniformly mixed, finally pouring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting the mixture at 180 ℃ for 3h, cooling the reaction kettle to room temperature, washing precipitates with deionized water and absolute ethyl alcohol for a plurality of times, transferring the reaction kettle to a vacuum drying oven, and drying the precipitates at 60 ℃ for 10h to obtain spherical Bi2WO6(ii) a 0.5mmol of the spherical Bi prepared above was taken2WO6Dispersing in deionized water, sequentially adding 0.008mL of mercaptopropionic acid and 0.25mmol of thioacetamide, stirring and mixing uniformly, adjusting the pH value of the mixed solution to 10.5 by using a sodium hydroxide solution with the molar concentration of 0.02mol/L, stirring and mixing uniformly, transferring into a reaction kettle for reaction at 180 ℃ for 3 hours, centrifugally separating the obtained precipitate, washing with deionized water and absolute ethyl alcohol, and drying in vacuum at 60 ℃ to obtain spherical Bi2S3/Bi2WO6A heterojunction photocatalytic material.
FIG. 1 shows Bi obtained in this example2S3/Bi2WO6FESEM image of heterojunction photocatalytic material shows that the sample is spherical, the diameter is 3-5 μm, and the spherical Bi is2S3/Bi2WO6The heterojunction photocatalytic material is made of Bi2WO6Nanosheet and Bi2S3The nano rods form spherical particles with the particle size of 3-5 mu m.
FIG. 2 shows Bi obtained in this example2S3/Bi2WO6UV-Vis DRS spectra of the heterojunction photocatalytic material.
FIG. 3 shows the present embodimentBi obtained in example2S3/Bi2WO6The XRD pattern of the heterojunction photocatalytic material can be seen from the figure that stronger diffraction peaks appear at the crystal faces of (103), (200), (202), (220), (303), (102), (109) and (307), and Bi2WO6The standard card (JCPDS 26-1044) is consistent and is tetragonal phase bismuth tungstate, and the XRD pattern of the heterojunction photocatalytic material corresponds to Bi except for the Bi2WO6In addition to the diffraction peaks of (1), weaker diffraction peaks appear at 2 θ =15.741 °, 17.657 °, 22.471 °, 23.780 °, 25.040 °, 31.920 °, 35.751 °, 39.223 °, 45.666 °, 51.610 °, which are related to Bi2S3(JCPDS 65-2435) Standard cards were in agreement, indicating that Bi was also present in the product2S3And (4) generating. From the above analysis, the product prepared is Bi2S3/Bi2WO6A heterojunction photocatalytic material.
Example 2
Degrading ciprofloxacin by photocatalysis: A500W xenon lamp is used as a light source, a 420nm filter plate is arranged to obtain visible light, namely light with the wavelength less than 420nm cannot pass through, so that ultraviolet light interference can be effectively avoided, and a quartz cooling trap with cooling water introduced into the quartz cooling trap is arranged around the xenon lamp. The experimental procedure was as follows: weighing 40mg of sample by using an electronic balance, slowly pouring the sample into a quartz tube, then weighing 40mL of ciprofloxacin solution with the mass concentration of 5mg/L by using a measuring cylinder, pouring the ciprofloxacin solution into the quartz tube filled with the sample, carrying out ultrasonic treatment for 30min in ultrasonic waves to enable the sample to be uniformly distributed, and then fixing the quartz tube in a photocatalytic reactor. The method comprises the steps of firstly opening cooling water, then opening a bubbling machine, bubbling for 15min to enable the cooling water to reach adsorption-desorption balance, then starting a xenon lamp power supply, timing when a light source is stable, taking a sample every 15min, wherein the volume of the sample is about 4mL, centrifuging the taken solution on a centrifugal machine, pouring out supernatant liquid, and accurately measuring the absorbance of the supernatant liquid to obtain the degradation condition of ciprofloxacin, thereby evaluating the visible light catalytic performance of the sample.
FIG. 4 shows Bi obtained in example 12S3/Bi2WO6Heterojunction photocatalytic material irradiated by visible lightAnd (3) reducing the change curve of the ultraviolet-visible absorption spectrum of the degraded ciprofloxacin. As can be seen from the graph, the intensity of the maximum absorption peak at 277nm of ciprofloxacin gradually decreased with the increase of the photocatalytic reaction time, indicating that Bi2S3/Bi2WO6The heterojunction photocatalytic material has better visible light catalytic degradation activity on ciprofloxacin.
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.
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| CN108355678A (en) * | 2018-03-09 | 2018-08-03 | 南昌航空大学 | A kind of compound micron bouquet of artificial gold-bismuth tungstate and its preparation method and application |
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