CN108786808B - Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalyst and preparation method and application thereof - Google Patents
Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalyst and preparation method and application thereof Download PDFInfo
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- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 96
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000003756 stirring Methods 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 239000000725 suspension Substances 0.000 claims abstract description 36
- 238000005286 illumination Methods 0.000 claims abstract description 34
- 239000002243 precursor Substances 0.000 claims abstract description 34
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 238000001228 spectrum Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 4
- 230000000593 degrading effect Effects 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 54
- 229910021641 deionized water Inorganic materials 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 16
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 239000002135 nanosheet Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 101710134784 Agnoprotein Proteins 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 12
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 29
- 238000009210 therapy by ultrasound Methods 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 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 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- 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
- 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
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/681—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with arsenic, antimony or bismuth
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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 relates to Ag/BiO2‑x/Bi2O3/Bi2O2.75A composite photocatalyst, a preparation method and application thereof. Mixing NaBiO3Adding the mixture into NaOH solution, dispersing the mixture into water to obtain reaction precursor solution, and preparing Bi through hydrothermal reaction2O2.75/BiO2‑x(ii) a Adding Bi2O2.75/BiO2‑xDispersing in water, and stirring under natural illumination to obtain a suspension A; mixing AgNO3Dispersing into water to obtain solution B; dispersing the solution B into the suspension A to obtain Ag/BiO under the natural illumination condition2‑x/Bi2O3/Bi2O2.75。Ag/BiO2‑x/Bi2O3/Bi2O2.75The composite photocatalyst has oxygen vacancy, and the oxygen vacancy and the surface plasmon resonance effect of the noble metal Ag have synergistic effect to enable the composite photocatalyst to respond to the full solar spectrum and be used for catalytically degrading organic pollutants.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst, a preparation method and application thereof.
Background
At present, the environmental pollution, especially air pollution and water pollution, is more serious, and the normal life of human beings is influenced. The most common methods for treating polluted water bodies so far, such as flotation, evaporation, extraction, redox, flocculation and the like, can remove suspended matters and part of organic pollutants, but have very poor effect on refractory organic matters and often cause secondary pollution. Compared with the method, the semiconductor photocatalysis technology can thoroughly degrade organic matters into nontoxic inorganic micromolecules, has good effect, takes sunlight as a driving force, has low cost and obvious advantages, and thus, the semiconductor photocatalysis technology is a potential sewage treatment technology.
However, most of the currently reported photocatalysts only respond to ultraviolet light or ultraviolet visible light, but are difficult to utilize near infrared light and far infrared light which account for about 43% of sunlight, and the utilization rate of sunlight is low.
Disclosure of Invention
The invention aims to provide Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalyst, preparation method and application thereof, the method is simple to operate, and the prepared Ag/BiO2-x/Bi2O3/Bi2O2.75In the composite photocatalyst, the oxygen vacancy and the surface plasmon resonance effect of Ag have a synergistic effect, so that the composite photocatalyst has the characteristic of full solar spectrum response and excellent photocatalytic activity.
The invention is realized by the following technical scheme:
Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalyst, Ag/BiO2-x/Bi2O3/Bi2O2.75In the composite photocatalyst, the bismuth oxide is in a nano-sheet shape, the Ag is in a nano-particle shape, and the Bi is2O2.75The space point group is I4-3 m; BiO2-xIs cubic phase, the space point group is Fm-3m, Bi2O3The phase is hexagonal phase, and the space point group is P-3m 1; Ag/BiO2-x/Bi2O3/Bi2O2.75Oxygen vacancies exist in the composite photocatalyst.
Preferably, the Ag loading rate is 5-30%.
The Ag/BiO2-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst comprisesThe method comprises the following steps:
step 1, adding NaBiO3Adding the mixture into NaOH solution with the concentration of 2.8 to 4.8mol/L, and uniformly stirring to obtain NaBiO3Dispersing the NaOH solution of NaBiO3 into water, stirring uniformly to obtain reaction precursor solution, and preparing Bi from the reaction precursor solution through hydrothermal reaction2O2.75/BiO2-xA composite photocatalyst;
step 2, adding Bi2O2.75/BiO2-xDispersing the composite photocatalyst into water, and stirring under a natural illumination condition to obtain a suspension A; mixing AgNO3Uniformly dispersing the mixture into water to obtain a solution B;
step 3, dispersing the solution B into the suspension A, and stirring for reaction under the natural illumination condition;
step 4, washing and drying the product obtained in the step 3 to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst is provided.
Preferably, in step 1, the filling ratio of the hydrothermal reaction is 60-70%, the hydrothermal reaction temperature is 150-175 ℃, and the reaction time is 20-360 min.
Preferably, Bi is contained in the suspension A obtained in the step 22O2.75/BiO2-xThe concentration of (A) is 5-15 g/L.
Preferably, AgNO is present in solution B obtained in step 23The concentration of (A) is 0.5-3 g/L.
Preferably, the stirring reaction time in the step 3 is 0.5-4 h.
Preferably, step 4 specifically comprises: washing the product obtained by the reaction in the step 3 with deionized water and absolute ethyl alcohol for three times respectively, and drying at 70 ℃ for 12 hours to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst is provided.
The Ag/BiO2-x/Bi2O3/Bi2O2.75The application of the composite photocatalyst is used for catalytically degrading organic pollutants under the irradiation of full solar spectrum.
Compared with the prior art, the invention has the following beneficial technical effects:
the Ag/BiO of the invention2-x/Bi2O3/Bi2O2.75Composite photocatalyst in Bi2O2.75And BiO2-xThe bismuth oxide photocatalyst contains oxygen vacancies with certain concentration, under the condition of natural illumination, an Ag simple substance can still be loaded on the surface of the bismuth oxide, and the oxygen vacancies and the surface plasmon resonance effect (LSPR effect) of the noble metal Ag can improve the light absorption intensity of the photocatalyst in the near infrared light range.
Bi is prepared by adopting a hydrothermal method through proper sodium hydroxide concentration2O2.75/BiO2-xThe composite photocatalyst adopts the prepared Bi2O2.75/BiO2-xComposite photocatalyst and AgNO3Adopts a simple method of natural light illumination and stirring as raw materials to successfully prepare the full solar spectral response Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst is characterized in that a large number of local state electrons exist in oxygen vacancies, and the electrons can jump to a conduction band and Ag only by capturing photons with smaller energy+Reacting to obtain Ag+Reducing Ag into Ag simple substance to be attached on the bismuth oxide nano-sheet layer. The method has the advantages of simple process, simple operation, short reaction time, mild reaction conditions and capability of preparing Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst has the characteristic of full-spectrum response and has good application prospect.
The composite photocatalyst prepared by the invention has higher degradation activity to rhodamine B under both visible light irradiation and near infrared light irradiation.
Drawings
FIG. 1 is an XRD pattern of a composite photocatalyst powder prepared according to the present invention, wherein a to g are XRD patterns of powders prepared in examples 1 to 7, respectively.
FIG. 2 is an SEM image of the powder prepared in example 5.
FIG. 3 is high resolution XPS spectra of (a) O1s and (b) Ag3d for the powder prepared in example 4.
FIG. 4 is a diagram of UV-vis-NIR DRS of the composite photocatalyst powder prepared by the present invention, wherein a-g are diagrams of UV-vis-NIR DRS of the powder prepared in examples 1-7, respectively.
FIG. 5 is a degradation curve of the composite photocatalyst powder prepared by the present invention under (a) visible light and (b) near infrared light irradiation.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Ag/BiO2-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst comprises the following steps:
step 1: mixing NaBiO3Adding the mixture into NaOH solution with the concentration of 2.8 to 4.8mol/L, and uniformly stirring to obtain NaBiO3Dispersing the NaOH solution of NaBiO3 into water, stirring uniformly to obtain reaction precursor solution, and preparing Bi from the reaction precursor solution through hydrothermal reaction2O2.75/BiO2-xA composite photocatalyst;
step 2: a certain amount of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into deionized water, and stirring for 30min under the condition of natural illumination to obtain a suspension A;
and step 3: a certain amount of AgNO3Dispersing in deionized water, and performing ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for a certain time under the natural illumination condition;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst is provided.
In the step 1, the filling ratio of the hydrothermal reaction is 60-70%, the hydrothermal reaction temperature is 150-175 ℃, and the reaction time is 20-360 min.
Bi in the suspension A obtained in the step 22O2.75/BiO2-xThe concentration of (A) is 5-15 g/L.
AgNO in the solution B obtained in the step 33The concentration of (A) is 0.5-3 g/L.
The stirring time in the step 4 is 0.5-4 h.
In the step 4, the dosage of the suspension A and the solution B is matched according to the Ag loading rate of 5-30%, and preferably the Ag loading rate is 10-25%.
The prepared Ag/BiO2-x/Bi2O3/Bi2O2.75In the composite photocatalyst, the bismuth oxide is in a nano-sheet shape, the Ag is in a nano-particle shape, and the Bi is contained in the bismuth oxide2O2.75The space point group is I4-3 m; BiO2-xIs cubic phase, the space point group is Fm-3m, Bi2O3The phase is hexagonal phase, and the space point group is P-3m 1; the loading rate of Ag is 5-30%.
The prepared Ag/BiO2-x/Bi2O3/Bi2O2.75Bi in the composite photocatalyst2O2.75And BiO2-xOxygen vacancies exist, the concentration of the oxygen vacancies reaches 22.25 percent, the noble metal Ag has a surface plasmon resonance effect, and the synergistic effect of the oxygen vacancies in the composite photocatalyst and the surface plasmon resonance effect of the noble metal Ag ensures that the composite photocatalyst has good light absorption characteristics in the full solar spectrum of 200-2100 nm.
The prepared Ag/BiO2-x/Bi2O3/Bi2O2.75After the visible light irradiation for 60min or the near infrared light irradiation for 120min, the degradation rate of the composite photocatalyst on RhB can reach 90%. Has excellent photocatalytic activity under the full solar spectrum.
Specific examples are as follows.
Example 1
Step 1: 0.5g of NaBiO3Dissolving the powder into 20mL of 3.0mol/L NaOH solution, and magnetically stirring to obtain a solution A;
step 2: slowly dispersing the solution A into 20mL of deionized water under the condition of magnetic stirring to obtain reaction precursor solution;
and step 3: adding the reaction precursor solution into a hydrothermal reaction kettle, placing the hydrothermal reaction kettle into a hydrothermal synthesizer, and reacting for 40min at 170 ℃; the filling ratio of the reaction precursor liquid is 60 percent;
and 4, step 4: after the reaction is finished, naturally cooling to 70 ℃, taking out the precipitate in the hydrothermal reaction kettle, washing with deionized water and absolute ethyl alcohol, and finally drying at constant temperature of 70 ℃ to obtain Bi2O2.75/BiO2-xComposite photocatalysts, designated BiO-OVs.
Example 2
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 40min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.015g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, noted as 5% Ag/BiO-OVs.
Example 3
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 40min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.03g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 10% Ag/BiO-OVs.
Example 4
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 40min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.045g AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 15% Ag/BiO-OVs.
Example 5
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 40min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.06g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 20% Ag/BiO-OVs.
Example 6
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 40min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.075g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalysts, designated as 25% Ag/BiO-OVs.
Example 7
Step 1: 0.5g of NaBiO3Adding the mixture into 20mL of NaOH solution with the concentration of 3mol/L, and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 300min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; wherein the filling ratio of the reaction precursor liquid is 60%;
step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.09g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 30% Ag/BiO-OVs.
Example 8
Step 1: 0.224g of NaBiO was added3Adding the mixture into 20mL of 2.8mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 150 ℃ for 360min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 60%.
Step 2: 0.2g of Bi2O2.75/BiO2-xThe composite photocatalyst is dispersed in 30mL deionized waterStirring for 30min under indoor illumination conditions to obtain suspension A;
and step 3: 0.015g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at high speed for 0.5h under the condition of natural light illumination;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, noted as 5% Ag/BiO-OVs.
Example 9
Step 1: 0.448g of NaBiO3Adding the mixture into 20mL of 3.6mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 120min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 65%.
Step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.03g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 1h under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 10% Ag/BiO-OVs.
Example 10
Step 1: 0.672g of NaBiO3Adding the mixture into 20mL of 4.8mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, and uniformly stirringObtaining reaction precursor liquid, and carrying out reaction for 40min at 175 ℃ by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 65%.
Step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.045g AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 15% Ag/BiO-OVs.
Example 11
Step 1: 0.448g of NaBiO3Adding the mixture into 20mL of 3.2mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 120min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 70%.
Step 2: 0.3g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.06g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at a high speed for 2 hours under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 20% Ag/BiO-OVs.
Example 12
Step 1: 0.900g of NaBiO3Adding the mixture into 20mL of 4.8mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 175 ℃ for 180min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 70%.
Step 2: 0.4g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.075g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at high speed for 4h under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photocatalysts, designated as 25% Ag/BiO-OVs.
Example 13
Step 1: 0.448g of NaBiO3Adding the mixture into 20mL of 2.8mol/L NaOH solution and uniformly stirring to obtain NaBiO3Dispersing the solution into 20mL of deionized water, uniformly stirring to obtain a reaction precursor solution, and reacting at 170 ℃ for 20min by a hydrothermal method to obtain Bi2O2.75/BiO2-xA composite photocatalyst; the filling ratio of the reaction precursor solution was 70%.
Step 2: 0.6g of Bi2O2.75/BiO2-xDispersing the composite photocatalyst into 30mL of deionized water, and stirring for 30min under indoor illumination conditions to obtain a suspension A;
and step 3: 0.09g of AgNO3Dispersing the solution in 30mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
and 4, step 4: slowly dispersing the solution B into the suspension A, and stirring at high speed for 4h under the illumination condition of natural light;
and 5: after the reaction is finished, the obtained powder is respectively washed three times by deionized water and absolute ethyl alcohol, and then dried for 12 hours at 70 ℃ to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst, designated 30% Ag/BiO-OVs.
FIG. 1 is an XRD pattern of a composite photocatalyst powder prepared according to the present invention, wherein a to g are XRD patterns of powders prepared in examples 1 to 7, respectively. Diffraction peaks at diffraction angles 2 θ of 31.9 °, 32.9 °, 36.1 °, 47.2 °, and 58.1 ° respectively correspond to tetragonal phase Bi2O2.75(JCPDF No.27-0049) has (103), (110), (112), (200), and (213) crystal planes, and diffraction peaks at about 28.2 °, 32.7 °, 46.9 °, 55.6 °, and 58.3 ° of 2 θ respectively correspond to cubic phase BiO2-xThe (111), (200), (220), (311), and (222) crystal planes of (JCPDF No.47-1057) have diffraction peaks around 30.1 ° 2 θ corresponding to hexagonal phase Bi2O3(JCPDF No.51-1161) (101) crystal face, Ag-supported, Bi2O2.75Decrease in diffraction peak intensity of, BiO2-xAnd Bi2O3Increase in diffraction peak intensity of (B), indicating that Bi is present under aqueous conditions2O2.75Tendency towards BiO2-xAnd Bi2O3And (4) phase transition. The diffraction peak of Ag does not appear in the XRD pattern, mainly because the Ag content in the material is less and the Ag is uniformly dispersed on the surface of the nanosheet.
FIG. 2 is an SEM photograph of the composite photocatalyst powder prepared in example 5. Wherein the nano flaky substance is bismuth oxide, and the granular substance is Ag.
FIG. 3 is a high resolution XPS spectrum of the composite photocatalyst powders O1s and Ag3d prepared in example 4. The sample can be found to contain 3 oxygen species by peak fitting processing of a high-resolution XPS spectrum of O1s by using Avantage software, wherein O1 is lattice oxygen, O2 is oxygen vacancy, O3 is adsorbed oxygen, and the concentration of the oxygen vacancy is 22.25%. The presence of Ag in the sample is evident from the high resolution XPS spectrum of Ag3 d.
FIG. 4 is a preparation of the present inventionThe UV-vis-NIR DRS diagram of the composite photocatalyst powder. In the figure, a to g are the powders prepared in the examples 1 to 7 respectively, and the Ag/BiO prepared by the method can be seen from the figure2-x/Bi2O3/Bi2O2.75The composite photocatalyst has good light absorption characteristic in the whole solar spectrum of 200-2100nm, and Bi2O2.75/BiO2-xThe absorption strength of the composite photocatalyst is obviously increased mainly due to the synergistic effect of the oxygen vacancies and the surface plasmon resonance effect of the noble metal Ag.
FIG. 5 is a degradation rate-time curve of rhodamine B degradation of the composite photocatalyst powder prepared by the present invention, wherein a-g in the graph are degradation diagrams of the powders prepared in examples 1-7 under visible light and near infrared light irradiation, respectively. C/C of ordinate in FIG. 50Is the ratio of the concentration of degraded rhodamine B to the initial concentration of the degraded rhodamine B. As can be seen from the figure, the prepared Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst has higher degradation activity under the irradiation of visible light and near infrared light, and has Bi2O2.75/BiO2-xCompared with the photocatalytic activity, the photocatalytic activity of the composite photocatalyst is also obviously improved, and the degradation of RhB can reach 90% after visible light irradiation for 60min or near infrared light irradiation for 120 min.
Claims (9)
1. Ag/BiO2-x/Bi2O3/Bi2O2.75The composite photocatalyst is characterized in that Ag/BiO2-x/Bi2O3/Bi2O2.75In the composite photocatalyst, the bismuth oxide is in a nano-sheet shape, the Ag is in a nano-particle shape, and the Bi is2O2.75The space point group is I4-3 m; BiO2-xIs cubic phase, the space point group is Fm-3m, Bi2O3The phase is hexagonal phase, and the space point group is P-3m 1; Ag/BiO2-x/Bi2O3/Bi2O2.75Oxygen vacancies exist in the composite photocatalyst.
2. According to the rightAg/BiO according to claim 12-x/Bi2O3/Bi2O2.75The composite photocatalyst is characterized in that the loading rate of Ag is 5-30%.
3. Ag/BiO according to any one of claims 1 to 22-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized by comprising the following steps:
step 1, adding NaBiO3Adding the mixture into NaOH solution with the concentration of 2.8 to 4.8mol/L, and uniformly stirring to obtain NaBiO3NaOH solution of (2), and then adding NaBiO3Dispersing the NaOH solution into water, uniformly stirring to obtain a reaction precursor solution, and preparing Bi from the reaction precursor solution through a hydrothermal reaction2O2.75/BiO2-xA composite photocatalyst; wherein the hydrothermal reaction temperature is 150-175 ℃;
step 2, adding Bi2O2.75/BiO2-xDispersing the composite photocatalyst into water, and stirring under a natural illumination condition to obtain a suspension A; mixing AgNO3Uniformly dispersing the mixture into water to obtain a solution B;
step 3, dispersing the solution B into the suspension A, and stirring for reaction under the natural illumination condition;
step 4, washing and drying the product obtained in the step 3 to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst is provided.
4. Ag/BiO according to claim 32-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized in that in the step 1, the filling ratio of the hydrothermal reaction is 60-70%, and the reaction time is 20-360 min.
5. Ag/BiO according to claim 32-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized in that Bi in the suspension A obtained in the step 22O2.75/BiO2-xIn a concentration of 5 to 15g/L。
6. Ag/BiO according to claim 32-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized in that AgNO in the solution B obtained in the step 23The concentration of (A) is 0.5-3 g/L.
7. Ag/BiO according to claim 32-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized in that the stirring reaction time in the step 3 is 0.5-4 h.
8. Ag/BiO according to claim 32-x/Bi2O3/Bi2O2.75The preparation method of the composite photocatalyst is characterized in that the step 4 specifically comprises the following steps: washing the product obtained by the reaction in the step 3 with deionized water and absolute ethyl alcohol for three times respectively, and drying at 70 ℃ for 12 hours to obtain Ag/BiO2-x/Bi2O3/Bi2O2.75A composite photocatalyst is provided.
9. Ag/BiO according to any one of claims 1 to 22-x/Bi2O3/Bi2O2.75The application of the composite photocatalyst is characterized in that the composite photocatalyst is used for catalyzing and degrading organic pollutants under the irradiation of full solar spectrum.
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