CN114797856A - Preparation method and application of floating type hydrogel photocatalyst - Google Patents
Preparation method and application of floating type hydrogel photocatalyst Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
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Abstract
The invention provides a preparation method and application of a floating type hydrogel photocatalyst, which firstly carries out BiVO 4 /Ag 3 VO 4 Synthesizing a powder photocatalyst, and preparing a photocatalyst material for enhancing the photocatalytic inactivation of microcystis aeruginosa under visible light through a floating preparation process. The photocatalyst has the characteristics of strong photocatalytic performance, good stability, strong visible light absorption capacity, high separation efficiency of photo-generated charges and the like. The synthesis method is simple and easy to implement, is green and environment-friendly, can effectively control the cyanobacterial bloom, and has good prospects in the technical field of water treatment.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a floating BiVO for removing algae in water 4 /Ag 3 VO 4 A preparation method of hydrogel photocatalyst.
Background
In recent years, the development of photocatalytic technology has led to its wider and wider application in the environmental field, and has become one of the most advanced technologies in water treatment. Photocatalysis has the advantages of environmental sustainability and low use cost, and has been widely used for solving various environmental problems. Conventional photocatalysts tend to have the disadvantages of only reacting to ultraviolet light and the corresponding rapid photoexcited electron-hole recombination, resulting in such photocatalysts exhibiting limited algae removal performance under visible light, which limits their practical applications. In addition, the traditional photocatalyst is generally in a powder shape, is difficult to recover, is easy to cause secondary pollution, and cannot be applied to an actual water body environment, so that the preparation of the photocatalyst which is strong in photocatalytic performance under visible light, good in stability, high in separation efficiency of photo-generated charges and easy to recover is imperative.
At present, a floating BiVO is not available 4 /Ag 3 VO 4 Hydrogel photocatalysts and related patent reports of preparation thereof.
Disclosure of Invention
The invention aims to provide a floating BiVO for removing algae in water 4 /Ag 3 VO 4 A preparation method of hydrogel photocatalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
floating type BiVO 4 /Ag 3 VO 4 The preparation method of the hydrogel photocatalyst comprises the following steps：
(1) First is BiVO 4 The preparation of (1): preparing a nitric acid solution with the concentration of 1.84M; then, 0.02mol (9.8 g) of Bi (NO) 3 ) 3 ·5H 2 Adding O into 50mL of 1.84M nitric acid solution to obtain solution A; 0.02mol (2.34 g) of Na is added 3 VO 4 ·12H 2 O was added to 50mL of a 1.84M nitric acid solution to give solution B. After the solution A and the solution B are fully dissolved, mixing the two solutions, adding urea, and stirring at 95 ℃; after completion, the mixture was washed with deionized water and dried at 80 ℃.
(2) Then BiVO 4 /Ag 3 VO 4 The preparation of (1): under the ultrasonic condition, 0.3g of BiVO is obtained 4 Dispersed in 50mL of ultrapure water. To the above dispersion was added 0.174g of AgNO 3 The solution was stirred for 30 min. Thereafter 0.1368g of Na dissolved in 50mL of water 3 VO 4 ·12H 2 Dropwise adding O into the solution, adjusting the pH to 10 by using 0.1M NaOH solution, and finally stirring for 6 hours under the dark condition to obtain BiVO 4 /Ag 3 VO 4 A catalyst.
(3) Finally, preparing the hydrogel photocatalyst: dissolving 2.5g of PVA and 0.3g of sodium alginate in water, and heating in a water bath at 95 ℃ for 5 hours to obtain a transparent and uniform solution; then adding a proper amount of BiVO into the solution 4 /Ag 3 VO 4 Quickly stirring the photocatalyst for 3min, adding 0.5g of hollow glass microspheres to enhance the floatability and compressive strength, quickly stirring for 30s, immediately pouring into a mold, freezing at-20 ℃ for 6h, unfreezing at room temperature for 2h, and performing freeze-unfreezing cycle for 3 times to obtain the floating BiVO 4 /Ag 3 VO 4 A hydrogel photocatalyst.
The application comprises the following steps: floating BiVO 4 /Ag 3 VO 4 The hydrogel photocatalyst can be applied to remove toxic and harmful algae and pollutants under visible light or sunlight.
The invention has the advantages that:
BiVO is firstly carried out in the invention 4 /Ag 3 VO 4 Synthesizing powder photocatalyst, and preparing floating type by loadingA floating type photocatalyst material capable of removing toxic and harmful algae in water under visible light is provided. Because of the traditional simple BiVO 4 /Ag 3 VO 4 The invention discloses a floating photocatalyst which is applicable to removing microcystis aeruginosa floating on water surface, can be suspended in an algae suspension well and is in more full contact with algae cells. Meanwhile, the electronic conduction rule of the hydrogel is similar to that of powder, and the hydrogel is a Z-type electronic conduction path, BiVO 4 The potential of the upper conduction band (2.86 eV) can satisfy the requirement of H 2 The potential condition of O to OH, and the hole on the conduction band can also inactivate the algae cells. OH and h, the main active substances produced during photocatalysis + Attack algae cell, make algae cell break, cell content flows out, and simultaneously some algae cell organic matters also can be degraded by active substance. The hydrogel is added in the process of preparing the photocatalyst, and a proper amount of hollow glass beads are innovatively added in the process of preparing the hydrogel, so that the hollow glass beads have the advantages of low density and high strength, not only have excellent floating effect in water, but also overcome the defects that other types of photocatalysts are difficult to recover and are easy to cause secondary pollution to water environment, more importantly, the microcystis aeruginosa floating on the water surface is favorably removed, and meanwhile, the hollow glass beads have the characteristics of strong photocatalytic performance, good stability, strong visible light absorption capacity, high separation efficiency of photo-generated charges and the like. The synthesis method is simple and feasible, the floating type photocatalytic material solves the problems that the powdery nano material cannot be recycled and has toxicity to the aquatic environment, is green and environment-friendly, can effectively control the cyanobacterial bloom, and has good prospect in the technical field of water treatment.
Drawings
FIG. 1 is the floating type BiVO of example 1 4 /Ag 3 VO 4 Hydrogel photocatalyst (ABVH-0.05, ABVH-0.08, ABVH-0.1. Note: ABVH represents 33% BiVO 4 /Ag 3 VO 4 Hydrogel, 0.05 represents the dosage of the material, and the unit is gram) the corresponding time-degradation rate relation of the photocatalytic degradation of chlorophyll aAs is clear from FIG. 1, the floating type BiVO produced by the present invention 4 /Ag 3 VO 4 The hydrogel photocatalyst (ABVH-0.05), (ABVH-0.08) and (ABVH-0.1) are subjected to a photocatalytic degradation experiment in a photochemical reactor, and the removal rates of the photocatalyst to chlorophyll a reach 88%, 96% and 99.6% within 4 hours.
FIG. 2 is the floating type BiVO of example 1 4 /Ag 3 VO 4 Fig. 2 shows that the degradation efficiency of the hydrogel photocatalyst (ABVH-0.1) on chlorophyll a is 99.5%, 93.4%, 92.1%, 90.1% and 87.5% respectively in 5-cycle experiments. It can be seen that the algae removal efficiency of ABVH-0.1 is kept above 90% for the first four times, which shows that the floating type BiVO of the invention 4 /Ag 3 VO 4 The hydrogel photocatalyst has better stability.
FIG. 3 is the floating type BiVO of example 1 4 /Ag 3 VO 4 SEM image of hydrogel photocatalyst.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below. The method of the present invention is a method which is conventional in the art unless otherwise specified.
Example 1
Floating type BiVO 4 /Ag 3 VO 4 The preparation method of the hydrogel photocatalyst comprises the following steps:
(1) first is BiVO 4 The preparation of (1): preparing a nitric acid solution with the concentration of 1.84M; then, 0.02mol (9.8 g) of Bi (NO) 3 ) 3 ·5H 2 Adding O into 50mL of 1.84M nitric acid solution to obtain solution A; 0.02mol (2.34 g) of Na is added 3 VO 4 ·12H 2 O was added to 50mL of a 1.84M nitric acid solution to give solution B. After the solution A and the solution B are fully dissolved, mixing the two solutions, adding urea, and stirring at 95 ℃; after completion, the mixture was washed with deionized water and dried at 80 ℃.
(2) Then BiVO 4 /Ag 3 VO 4 The preparation of (1): on the ultrasonic stripUnder the conditions, 0.3g of BiVO was obtained 4 Dispersed in 50mL of ultrapure water. To the above dispersion was added 0.174g of AgNO 3 The solution was stirred for 30 min. Thereafter 0.1368g of Na dissolved in 50mL of water 3 VO 4 ·12H 2 Dropwise adding O into the solution, adjusting the pH to 10 by using 0.1M NaOH solution, and finally stirring for 6 hours under the dark condition to obtain BiVO 4 /Ag 3 VO 4 A catalyst.
(3) Finally, preparing the hydrogel photocatalyst: dissolving 2.5g of PVA and 0.3g of sodium alginate in water, and heating in a water bath at 95 ℃ for 5 hours to obtain a transparent and uniform solution; then adding a proper amount of BiVO into the solution 4 /Ag 3 VO 4 Quickly stirring the photocatalyst for 3min, adding 0.5g of hollow glass microspheres, quickly stirring for 30s, immediately pouring into a mold, freezing at-20 ℃ for 6h, unfreezing at room temperature for 2h, and performing freeze-unfreezing cycle for 3 times to obtain the floating BiVO 4 /Ag 3 VO 4 Hydrogel photocatalyst, noted ABVH, where BiVO 4 /Ag 3 VO 4 The dosage of the hydrogel photocatalyst accounts for 33 percent of the mass of the hydrogel photocatalyst.
Comparative example 1
The hollow glass microspheres are not added in the preparation of the hydrogel, the rest of the operation is the same as that of the example 1, the obtained hydrogel photocatalyst is marked as ABVH, the photocatalytic performance comparison is carried out, the content of chlorophyll a in three experimental groups without the hollow glass microspheres is obviously reduced after the photocatalytic reaction starts, and the removal rate of 4h reaches 79 percent (ABVH-0.05), 85 percent (ABVH-0.08) and 88 percent (ABVH-0.1) respectively.
The photocatalytic algae removal reactor used in the research is a DY-D type photocatalytic reactor produced by Shanghai Densey Pont instruments Co., Ltd, and integrates functions of simulating visible light, cooling circulation and stirring. Prepared with 100mW cm -2 The metal halide lamp is used as a visible light source, and a light filter is arranged at the position of 30cm away from the light source, so that the effect of simulating visible light is achieved.
In the experiment for removing microcystis aeruginosa through photocatalysis, the research object is typical microcystis aeruginosa, and the algae density is 5.0x10 9 cells/L (OD680 ≈ 0.71). Firstly, a certain amount of photocatalyst is takenUniformly suspending the photocatalyst suspension in a centrifuge tube filled with 5mL of deionized water, accurately measuring the uniformly dispersed photocatalyst suspension according to the required photocatalyst dosage, and then adding the photocatalyst suspension into a quartz test tube; next, an algal density of about 5.0x10 was added to the tube 9 The cell/L algae suspension is fully mixed with the nano photocatalyst and is put into a photocatalytic reactor; thirdly, starting a reactor stirring device and a cooling circulation device; and finally, turning on a metal halide lamp to start the photocatalytic algae removal reaction. Floating photocatalysts with different doping amounts are added into an experimental group to carry out an experiment, ABVH-0.05, ABVH-0.08 and ABVH-0.1 are respectively added to carry out a photocatalytic algae removal experiment, and a control group is not added with any photocatalyst to carry out the experiment. Sampling time interval of each experiment is 30min, a 180 min photocatalysis experiment is carried out, the content of chlorophyll a is uniformly measured after the experiment is finished, and the algae removal effect of the floating photocatalyst with different doping amounts is analyzed.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (2)
1. Floating BiVO for removing algae in water 4 /Ag 3 VO 4 The preparation method of the hydrogel photocatalyst is characterized by comprising the following steps:
（1）BiVO 4 the preparation of (1): 0.02mol of Bi (NO) 3 ) 3 ·5H 2 Adding O into 50mL of 1.84M nitric acid solution to obtain solution A; then 0.02mol of Na is added 3 VO 4 ·12H 2 Adding O into 50mL of 1.84M nitric acid solution to obtain solution B; mixing the solution A and the solution B, adding urea, and stirring at 95 ℃; washing with deionized water, and drying at 80 deg.C;
（2）BiVO 4 /Ag 3 VO 4 the preparation of (1): under the ultrasonic condition, 0.3g of BiVO 4 Dispersed in 50mL of ultrapure water, and then 0.174g of AgNO was added 3 After stirring for 30min, 50mL of a solution containing 0.1368g of Na 3 VO 4 ·12H 2 The aqueous solution of O is added dropwise, thenThen adjusting the pH value to 10 by using 0.1M NaOH solution, and finally stirring for 6 hours under the dark condition to obtain BiVO 4 /Ag 3 VO 4 A catalyst;
(3) preparation of hydrogel photocatalyst: dissolving 2.5g of PVA and 0.3g of sodium alginate in 30 mL of water, and heating in a water bath at 95 ℃ for 5 hours to obtain a transparent and uniform solution; then adding a proper amount of BiVO 4 /Ag 3 VO 4 Quickly stirring the photocatalyst for 3min, adding 0.5g of hollow glass microspheres, quickly stirring for 30s, immediately pouring into a mold, freezing at-20 ℃ for 6h, unfreezing at room temperature for 2h, and performing freeze-unfreezing cycle for 3 times to obtain the floating BiVO 4 /Ag 3 VO 4 A hydrogel photocatalyst.
2. Floating BiVO prepared by the preparation method according to claim 1 4 /Ag 3 VO 4 A hydrogel photocatalyst.
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