CN109317177B - Method for synthesizing nitrogen-doped bismuth vanadate photocatalyst and application thereof - Google Patents
Method for synthesizing nitrogen-doped bismuth vanadate photocatalyst and application thereof Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 88
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 48
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
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- 238000003760 magnetic stirring Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 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 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 7
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- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 22
- 230000001699 photocatalysis Effects 0.000 description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 14
- 229940043267 rhodamine b Drugs 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 8
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- 239000007864 aqueous solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
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- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical group O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a preparation method and application of a nitrogen-doped bismuth vanadate photocatalyst synthesized by a hydrothermal method.
Description
Technical Field
The invention belongs to the field of environment functional materials, and particularly relates to a nitrogen-doped bismuth vanadate photocatalyst synthesized by a hydrothermal method, and a preparation method and application thereof.
Background
In recent years, the growing environmental pollution seriously threatens the survival and development of human beings. With the rapid increase of energy demand, development and research on new energy and new technology are imminent. The solar energy is a clean natural renewable energy source, is developed and utilized, has no pollution and does not influence ecological balance; the photocatalytic technology is a green technology and has important application prospects.
With the development of photocatalytic technology, many new visible light-responsive semiconductor materials have been developed. Among them, the vanadate photocatalysts such as bismuth vanadate, indium vanadate, silver vanadate and the like have attracted wide attention because of their narrow band gaps and are capable of responding to visible light. Among them, bismuth vanadate has good properties such as corrosion resistance, ionic conductivity, ferroelasticity, and photocatalysis, and is favored by researchers. There are three kinds of bismuth vanadateThe crystal forms are monoclinic scheelite type, tetragonal zircon type and tetragonal scheelite type respectively. The photocatalysis performances of the three crystal forms are different, bismuth vanadate becomes the best photocatalysis performance of the three crystal forms due to the smallest forbidden bandwidth (2.4eV), but the photocatalysis efficiency needs to be improved due to the high recombination rate of photo-generated electron-hole pairs of the bismuth vanadate catalyst. For this purpose, various methods are used to modify the bismuth vanadate catalyst, such as: ion doping, noble metal deposition, semiconductor compounding and the like, which improve the photocatalytic performance of the bismuth vanadate to a certain extent. Zhang ai Ping, etc. prepares Eu, Gd and Er doped bismuth vanadate composite photocatalyst, and analysis shows that the three rare earth elements are in respective oxide forms (Eu2O3、Gd2O3And Er2O3) The bismuth vanadate exists in the crystal, so that the crystallinity of the bismuth vanadate is changed, the specific surface area is increased, and the absorption edge is red-shifted. Preparation and activity study of Ln-doped bismuth vanadate (Ln ═ Eu, Gd, Er) photocatalyst [ J]Inorganic chemistry bulletin, 2009.11(25): 2040-.]. Qi Tianhao et al synthesizes the bismuth vanadate-titanium dioxide composite material by a hydrothermal method. Compared with the single bismuth vanadate and the single titanium dioxide, the light absorption range of the semiconductor material after the compounding has obvious red shift. Can better improve the photocatalytic activity of the titanium dioxide. [ Qi Tianhao, Yangyang, delicate and beautiful, etc. visible light responding bismuth vanadate/titanium dioxide nano composite photocatalyst [ J]. Spectroscopy and Spectroscopy 2010.7(30):1944-1947.]. The research on visible light activity caused by nitrogen replacing a small amount of lattice oxygen was reported in Science by Asahi et al in 2001, and the result shows that the visible light activity is improved as a result of doping a small amount of nitrogen into the titanium dioxide lattice and replacing the oxygen lattice to narrow the band gap of the titanium dioxide. [ Asahi R, Morikawa T, Ohwaki T, et al, visible-light photocatalysis in nitrogen polypeptides oxides [ J].Science,2001.293(5528):269-280.]. Since then, people begin to research the influence of non-metal element doping modification on semiconductor photocatalytic materials, and the non-metal element doping modification rapidly becomes a hot point of research.
Disclosure of Invention
The invention aims to provide a nitrogen-doped bismuth vanadate photocatalyst synthesized by a hydrothermal method, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for synthesizing a nitrogen-doped bismuth vanadate photocatalyst, which comprises the following steps:
step (1): dissolving bismuth nitrate pentahydrate in concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and uniformly stirring to obtain a solution A; dissolving ammonium metavanadate in an ammonia water solution, adding urea according to the molar ratio of N to Bi of 1-1.5: 1, and uniformly stirring to obtain a solution B; the concentration of the bismuth nitrate pentahydrate and the concentration of the ammonium metavanadate are both 2.5mmol and the concentration of the concentrated nitric acid and the concentration of the ammonia water are both 2 mol/L;
step (2): slowly adding the solution A obtained in the step (1) into the solution B, and after mixing, continuing to stir for 1h by magnetic force. Dropwise adding concentrated ammonia water to adjust the pH value of the solution to be about 7, carrying out ultrasonic treatment for 30min, and then carrying out magnetic stirring for 1h to obtain a precursor solution;
and (3): adding the precursor solution obtained in the step (2) into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, the time to be 24 hours, taking the reaction kettle out after the reaction is finished, naturally cooling the reaction kettle in the air, pouring out supernatant, and collecting precipitates;
and (4): and (4) centrifuging, washing and drying the precipitate obtained in the step (3) to obtain the nitrogen-doped bismuth vanadate photocatalyst.
Preferably, the stirring in step (1) of the method is magnetic stirring, and the stirring time is 30 min.
Preferably, the filling ratio of the precursor solution in the step (3) of the method of the present invention in the reaction kettle is 60-70%.
The washing in step (4) of the preferred method of the present invention is three times by alternately washing with secondary water and absolute ethanol.
Preferably, the drying in step (4) of the process of the present invention is carried out at 100 ℃ for 8 hours.
The bismuth vanadate prepared by the method is monoclinic scheelite type crystal.
The nitrogen-doped bismuth vanadate photocatalyst prepared by the method disclosed by the invention is applied to degradation of organic matters under visible light.
Has the advantages that: the invention takes bismuth nitrate pentahydrate as bismuth source, amine metavanadate as vanadium source and urea (H)2NCONH2) And (3) doping the bismuth vanadate with nitrogen as a nitrogen source. According to the invention, nitrogen is introduced into the crystal lattice of bismuth vanadate, so that the performance of photocatalytic degradation of organic matters of pure bismuth vanadate under visible light is improved, and the aim of modifying the bismuth vanadate is fulfilled. The preparation method has the advantages of simple operation, high reaction speed and no need of calcination, and the heat treatment furnace adopted by the hydrothermal reaction has great universality and is suitable for laboratories and industrial production.
Drawings
FIG. 1: a is the XRD spectrum of the sample obtained in example 2; b is the XRD spectrum of the sample obtained in comparative example 1;
FIG. 2: SEM image of the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 of the present invention;
FIG. 3: a Uv-vis profile of the sample; in the figure, a is the nitrogen-doped bismuth vanadate photocatalyst obtained in example 2, and b is the pure bismuth vanadate obtained in comparative example 1;
FIG. 4: a photocurrent density curve graph of the sample under visible light; in the figure, a is the nitrogen-doped bismuth vanadate photocatalyst obtained in example 2, and b is the pure bismuth vanadate obtained in comparative example 1;
FIG. 5: the nitrogen-doped bismuth vanadate photocatalyst prepared in the embodiment 2 of the invention degrades a rhodamine B test chart under visible light;
FIG. 6: the stability test chart of the nitrogen-doped bismuth vanadate photocatalyst prepared in the embodiment 2 of the invention is used for carrying out a decolorization experiment on rhodamine B under visible light.
Detailed Description
The invention will be described in more detail with reference to the following examples and the accompanying drawings
Example 1: a method for nitrogen doping bismuth vanadate photocatalyst comprises the following steps:
step 1: dissolving 2.5mmol of bismuth nitrate pentahydrate in 2mol/L concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and magnetically stirring for 30min to obtain a solution A; dissolving 2.5mmol of ammonium metavanadate in 2mol/L of ammonia water solution, and mixing urea according to the mol ratio of N to Bi of 0.5: 1, and magnetically stirring for 30min to obtain a solution B;
step 2: slowly adding the solution A into the solution B, and after mixing, continuing to stir for 1 hour by magnetic force. Dropwise adding concentrated ammonia water to adjust the pH value of the solution to be about 7, carrying out ultrasonic treatment for 30min, and then carrying out magnetic stirring for 1h to obtain a precursor solution;
and step 3: adding the precursor solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, setting the heating time to be 24 hours, taking out the reaction kettle after the reaction is finished, and naturally cooling in the air;
and 4, step 4: and taking out the sample, pouring out the supernatant, centrifuging the obtained precipitate, alternately washing the precipitate for three times by using secondary water and absolute ethyl alcohol, and drying the precipitate for 8 hours at the temperature of 100 ℃ to obtain the nitrogen-doped bismuth vanadate photocatalyst.
50mL of 10mg/L rhodamine B aqueous solution is placed in a cylindrical quartz container with a cooling jacket, 50mg of the nitrogen-doped bismuth vanadate photocatalyst prepared in the embodiment 1 is added, the mixed system is placed in a photocatalytic reaction device and stirred away from light for 60min to achieve adsorption-desorption balance, photocatalytic reaction is carried out under the irradiation of a visible light source (lambda is more than or equal to 420nm), liquid samples are taken at intervals, after centrifugal separation, supernatant is taken, and the absorbance of the sample clear solution is tested by an ultraviolet visible spectrophotometer. Because the concentration of rhodamine B and the absorbance thereof at the wavelength of 554nm are in a linear relationship, the degradation rate of rhodamine B can be finally calculated through the absorbance. After 2.5h, the degradation rate of the nitrogen-doped bismuth vanadate photocatalyst on rhodamine B is 28.5%.
Example 2: a method for nitrogen doping bismuth vanadate photocatalyst comprises the following steps:
step 1: dissolving 2.5mmol of bismuth nitrate pentahydrate in 2mol/L concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and magnetically stirring for 30min to obtain a solution A; dissolving 2.5mmol of ammonium metavanadate in 2mol/L ammonia water solution, adding urea according to the molar ratio of N to Bi of 1:1, and magnetically stirring for 30min to obtain solution B;
step 2: slowly adding the solution A into the solution B, and after mixing, continuing to stir for 1 hour by magnetic force. Dropwise adding concentrated ammonia water to adjust the pH value of the solution to be about 7, carrying out ultrasonic treatment for 30min, and then carrying out magnetic stirring for 1h to obtain a precursor solution;
and step 3: adding the precursor solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, setting the heating time to be 24 hours, taking out the reaction kettle after the reaction is finished, and naturally cooling in the air;
and 4, step 4: and taking out the sample, pouring out the supernatant, centrifuging the obtained precipitate, alternately washing the precipitate for three times by using secondary water and absolute ethyl alcohol, and drying the precipitate for 8 hours at the temperature of 100 ℃ to obtain the nitrogen-doped bismuth vanadate photocatalyst.
Under the same photocatalytic reaction conditions as in example 1, the degradation rate of the sample to rhodamine B after 2.5h is 80.05%.
Example 3: a method for nitrogen doping bismuth vanadate photocatalyst comprises the following steps:
step 1: dissolving 2.5mmol of bismuth nitrate pentahydrate in 2mol/L concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and magnetically stirring for 30min to obtain a solution A; dissolving 2.5mmol of ammonium metavanadate in 2mol/L ammonia water solution, adding urea according to the molar ratio of N to Bi of 2:1, and magnetically stirring for 30min to obtain solution B;
step 2: slowly adding the solution A into the solution B, and after mixing, continuing to stir for 1 hour by magnetic force. Dropwise adding concentrated ammonia water to adjust the pH value of the solution to be about 7, carrying out ultrasonic treatment for 30min, and then carrying out magnetic stirring for 1h to obtain a precursor solution;
and step 3: adding the precursor solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, setting the heating time to be 24 hours, taking out the reaction kettle after the reaction is finished, and naturally cooling in the air;
and 4, step 4: and taking out the sample, pouring out the supernatant, centrifuging the obtained precipitate, alternately washing the precipitate for three times by using secondary water and absolute ethyl alcohol, and drying the precipitate for 8 hours at the temperature of 100 ℃ to obtain the nitrogen-doped bismuth vanadate photocatalyst.
Under the same photocatalytic reaction conditions as in example 1, the degradation rate of the sample on rhodamine B after 2.5h is 62.54%.
Comparative example 1:
step 1: dissolving 2.5mmol of bismuth nitrate pentahydrate in 2mol/L concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and magnetically stirring for 30min to obtain a solution A; dissolving 2.5mmol of ammonium metavanadate in 2mol/L ammonia water solution, and magnetically stirring for 30min to obtain solution B;
step 2: slowly adding the solution A into the solution B, and after mixing, continuing to stir for 1 hour by magnetic force. Dropwise adding concentrated ammonia water to adjust the pH value of the solution to be about 7, carrying out ultrasonic treatment for 30min, and then carrying out magnetic stirring for 1h to obtain a precursor solution;
and step 3: adding the precursor solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, setting the heating time to be 24 hours, taking out the reaction kettle after the reaction is finished, and naturally cooling in the air;
and 4, step 4: and taking out the sample, pouring out the supernatant, centrifuging the obtained precipitate, alternately washing the precipitate with secondary water and absolute ethyl alcohol for three times, and drying the precipitate at 100 ℃ for 8 hours to obtain the pure bismuth vanadate photocatalyst.
Under the same photocatalytic reaction condition as that of the example 1, the degradation rate of pure bismuth vanadate to rhodamine B after 2.5h is 27.8%.
FIG. 1: is a sample XRD spectrum; wherein a is the nitrogen-doped bismuth vanadate photocatalyst prepared by the method of example 2, and b is the pure bismuth vanadate prepared by the comparative example 1; as can be seen from fig. 1, the nitrogen-doped bismuth vanadate is a pure monoclinic scheelite-type crystal, and compared with pure bismuth vanadate, diffraction peaks of the sample after doping are all shifted to the left, which indicates that the doped nitrogen enters into crystal lattices of the bismuth vanadate and replaces part of oxygen atoms, so that the number of lattice oxygen is reduced, a certain influence is exerted on a valence bond structure of the bismuth vanadate, and the crystal structure of the bismuth vanadate is adjusted.
FIG. 2: as can be seen from fig. 2, the nitrogen-doped bismuth vanadate is in a flake shape and is interspersed together to form a cluster, and the particles have a certain uniform dispersibility.
FIG. 3: for the Uv-vis plots of the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 and the pure bismuth vanadate prepared in comparative example, wherein a is the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 and b is the pure bismuth vanadate prepared in comparative example 1, it can be seen from fig. 3 that the absorption edge of the nitrogen-doped bismuth vanadate is significantly red-shifted compared to the pure bismuth vanadate, and the band gap of the nitrogen-doped bismuth vanadate is 2.14eV, which is reduced compared to the pure bismuth vanadate (2.29eV) according to the band gap calculation formula.
FIG. 4: the photocurrent density curves for the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 and the pure bismuth vanadate photocatalyst prepared in comparative example 1 were shown, wherein a is the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2, and b is the pure bismuth vanadate photocatalyst prepared in comparative example 1. As can be seen from fig. 4, compared with pure bismuth vanadate, the curve of bismuth vanadate doped with nitrogen has a peak, which is caused by doping to change the surface state curve, so that a trap is formed on the surface, and a part of photons are captured by the trap at the moment of illumination, so that the current intensity is increased instantaneously, thus promoting the photodegradation capability of the catalyst to a certain extent.
FIG. 5: in order to test the degradation of rhodamine B under visible light for the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 and the pure bismuth vanadate prepared in comparative example 1, wherein a is the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2, and B is the pure bismuth vanadate prepared in comparative example 1, as can be seen from fig. 5, compared with the pure bismuth vanadate, the nitrogen-doped bismuth vanadate photocatalyst has a greatly improved photocatalytic effect on rhodamine B, and the degradation rate of rhodamine B aqueous solution is up to 80.05% after the rhodamine B aqueous solution is subjected to photocatalysis for 2.5 hours under the action of the nitrogen-doped bismuth vanadate. It can be seen that the nitrogen-doped bismuth vanadate obtained in example 2 has stronger photocatalytic activity than pure bismuth vanadate.
FIG. 6: for a stability test chart of the nitrogen-doped bismuth vanadate photocatalyst prepared in example 2 for carrying out a decolorization experiment on rhodamine B under visible light, as can be seen from fig. 6, after the nitrogen-doped bismuth vanadate photocatalyst is recycled for 4 times, the photocatalytic activity is not obviously reduced, which indicates that the photocatalyst has good stability in a photocatalytic process.
Claims (7)
1. A method for synthesizing a nitrogen-doped bismuth vanadate photocatalyst is characterized by comprising the following steps of:
step (1): dissolving bismuth nitrate pentahydrate in concentrated nitric acid, adding a certain amount of polyvinylpyrrolidone, and uniformly stirring to obtain a solution A; dissolving ammonium metavanadate in an ammonia water solution, adding urea according to the molar ratio of N to Bi of 1-1.5: 1, and uniformly stirring to obtain a solution B; the concentration of the concentrated nitric acid and the concentration of the ammonia water are both 2 mol/L;
step (2): slowly adding the solution A obtained in the step (1) into the solution B, continuously performing magnetic stirring for 1h after mixing, dropwise adding concentrated ammonia water to adjust the pH value of the solution to 7, performing ultrasonic treatment for 30min, and performing magnetic stirring for 1h to obtain a precursor solution;
and (3): adding the precursor solution obtained in the step (2) into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven for heating, setting the heating temperature to be 180 ℃, the time to be 24 hours, taking the reaction kettle out after the reaction is finished, naturally cooling the reaction kettle in the air, pouring out supernatant, and collecting precipitates;
and (4): and (4) centrifuging, washing and drying the precipitate obtained in the step (3) to obtain the nitrogen-doped bismuth vanadate photocatalyst.
2. The method for synthesizing the nitrogen-doped bismuth vanadate photocatalyst according to claim 1, wherein the stirring in the step (1) is magnetic stirring, and the stirring time is 30 min.
3. The method for synthesizing the nitrogen-doped bismuth vanadate photocatalyst according to claim 1, wherein the filling ratio of the reaction kettle precursor solution in the step (3) is 60-70%.
4. The method for synthesizing the nitrogen-doped bismuth vanadate photocatalyst according to claim 1, wherein the washing manner in the step (4) is three times of washing with secondary water and absolute ethyl alcohol alternately.
5. The method for synthesizing the nitrogen-doped bismuth vanadate photocatalyst according to claim 1, wherein the drying condition in the step (4) is drying at 100 ℃ for 8 h.
6. The method for synthesizing nitrogen-doped bismuth vanadate photocatalyst according to any one of claims 1 to 5, wherein the bismuth vanadate is monoclinic scheelite-type crystal.
7. The use of the nitrogen-doped bismuth vanadate photocatalyst prepared by the method for synthesizing the nitrogen-doped bismuth vanadate photocatalyst according to any one of claims 1 to 5 in degrading organic matters under visible light.
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