CN113101954B - Bi 5 O 7 I/Bi 2 MoO 6 Composite photocatalyst and preparation method and application thereof - Google Patents
Bi 5 O 7 I/Bi 2 MoO 6 Composite photocatalyst and preparation method and application thereof Download PDFInfo
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- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 5
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/132—Halogens; Compounds thereof with chromium, molybdenum, tungsten or polonium
-
- B01J35/40—
-
- 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
-
- 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
- C02F2101/345—Phenols
-
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to Bi 5 O 7 I/Bi 2 MoO 6 A composite photocatalyst and a preparation method and application thereof. The photocatalyst prepared by the invention uses Bi 5 O 7 I nano-fiber as substrate, in Bi 5 O 7 Vertical growth of Bi on I nanofibers 2 MoO 6 Nanosheets, wherein Bi 5 O 7 The length of the I fiber is 0.5 to 10 mu m, the width is 50 to 1000nm, the thickness is 10 to 600nm 2 MoO 6 The size of the nano sheet is 20 to 1000nm, and the thickness of the nano sheet is 2 to 150nm. The invention has simple process, easy control and low cost; bi prepared by the invention 5 O 7 I/Bi 2 MoO 6 The heterojunction composite nano photocatalyst has high-efficiency visible light photocatalytic activity, good stability and reusability, and can still maintain high catalytic activity after being repeatedly used for catalysis.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to Bi 5 O 7 I/Bi 2 MoO 6 A composite photocatalyst and a preparation method and application thereof.
Background
With the rapid development of industrialization, sewage treatment has become an urgent problem to be solved. The semiconductor photocatalysis technology can convert solar energy into chemical energy and further decompose organic pollutants, so that the semiconductor photocatalysis technology is considered to be an environmental pollution treatment technology with wide application prospects. Since the visible light component occupies nearly half of the sunlight, the development of a photocatalyst having a visible light response is one of the research hotspots in the field of photocatalysis.
Bismuth-based semiconductors in recent yearsThe compound photocatalyst is continuously emerged in the field of photocatalytic research and shows good photocatalytic performance. Bi 5 O 7 I is Bi x O y X z The forbidden band width of an important photocatalyst in (X = Cl, br, I) series photocatalysts is generally 2.9-3.1 eV. Although the wide forbidden band width of the photo-generated carrier enables the photo-generated carrier to have high oxidation reduction capability, the photo-generated carrier has high ultraviolet light photocatalytic activity, but the photo-generated carrier is weak in visible light absorption, and the visible light photocatalytic activity of the photo-generated carrier is weak. Bi 2 MoO 6 The bismuth-based photocatalyst is another common bismuth-based semiconductor compound photocatalyst, the forbidden bandwidth of the bismuth-based photocatalyst is generally 2.4 to 2.8eV, and the bismuth-based photocatalyst has strong visible light absorption. However, bi 2 MoO 6 The defect that the service life of the photogenerated carrier is short and the photogenerated carrier is easy to recombine causes that Bi 2 MoO 6 The photocatalytic activity of (a) is greatly affected. In the prior art, bi does not exist yet 5 O 7 I and Bi 2 MoO 6 Related description of composite structures.
Disclosure of Invention
In view of the problems in the prior art, the present invention is to provide a Bi 5 O 7 I/Bi 2 MoO 6 The composite photocatalyst has high visible light photocatalytic activity and good reusability.
The invention also provides Bi 5 O 7 I/Bi 2 MoO 6 A preparation method of a composite photocatalyst.
The invention also provides Bi 5 O 7 I/Bi 2 MoO 6 Application of the composite photocatalyst.
The specific technical scheme of the invention is as follows:
the invention provides a Bi 5 O 7 I/Bi 2 MoO 6 A composite photocatalyst consisting of Bi 5 O 7 I nano-fiber as substrate, in Bi 5 O 7 Vertical growth of Bi on I nanofibers 2 MoO 6 Nanoplatelets of which Bi 5 O 7 The length of the I fiber is 0.5 to 10 mu m, the width is 50 to 1000nm, and the thickness of the I fiber isThe degree of the alloy is 10 to 600nm 2 MoO 6 The size of the nano sheet is 20 to 1000nm, and the thickness of the nano sheet is 2 to 150nm.
The invention also provides Bi 5 O 7 I/Bi 2 MoO 6 The preparation method of the composite photocatalyst comprises the following steps:
(1) Bi 5 O 7 i, preparation of nano-fibers: adding Bi (NO) 3 ) 3 •5H 2 Dispersing O into KI solution, performing ultrasonic dispersion, adding a certain amount of NaOH solution, performing magnetic stirring at room temperature, centrifuging the obtained product, washing with deionized water and ethanol, and drying to obtain Bi 5 O 7 And (I) nano fibers.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: bi prepared in the step (1) 5 O 7 Firstly dispersing the nano-fibers in an ethylene glycol solution to obtain a dispersion A; simultaneously taking a certain amount of Bi (NO) 3 ) 3 •5H 2 Dissolving O in the ethylene glycol solution to obtain a solution B; and Na is removed 2 MoO 4 •2H 2 Adding O into deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electrothermal blowing dry box for reaction, cooling to room temperature after the reaction is finished, centrifuging, washing and drying to obtain Bi 5 O 7 I/Bi 2 MoO 6 A composite photocatalyst is provided.
Further, in the step (1), the concentration of the KI aqueous solution is 0.035mol/L; the Bi (NO) 3 ) 3 •5H 2 The mass ratio of O to KI is 1; the concentration of the NaOH solution is 2mol/L, and the volume ratio of the NaOH solution to the KI aqueous solution is 6:80; the ultrasonic dispersion time is 2min; the magnetic stirring time is 3 hours; the drying is carried out at 60 ℃ for 8h.
Further, in the step (2), bi in the dispersion liquid A 5 O 7 Mole of I with ethylene glycolThe volume ratio is 0.2mmol; bi (NO) in the solution B 3 ) 3 •5H 2 The molar volume ratio of O to ethylene glycol is (0.05 to 0.2) mmol:10mL of Na in the solution C 2 MoO 4 •2H 2 The molar volume ratio of O to deionized water is (0.05 to 0.2) mmol:40mL.
Further, in the step (2), the Na 2 MoO 4 •2H 2 O and Bi (NO) 3 ) 3 •5H 2 The molar ratio of O is 1:1; na (Na) 2 MoO 4 •2H 2 O and Bi 5 O 7 The molar ratio of I is 0.25 to 1.
Further, in the step (2), the magnetic stirring time is 30 minutes; the reaction is carried out for 8 to 1697 h by hydrothermal treatment at the temperature of 120-180 ℃; the drying is carried out at 60 ℃ for 8 hours.
The invention also provides Bi prepared by the preparation method 5 O 7 I/Bi 2 MoO 6 The application of the composite photocatalyst in degrading organic pollutants.
The invention adopts a method of combining ion replacement and crystal growth under hydrothermal conditions to treat Bi in nano-fiber shape 5 O 7 I by Bi 2 MoO 6 Nano-sheet composite modification of Bi 5 O 7 Growth of Bi on I nanofibers 2 MoO 6 Nanosheets, preparation thereof to yield Bi 5 O 7 I/Bi 2 MoO 6 Heterojunction composite nano-photocatalyst. The composite photocatalyst and pure Bi 5 O 7 Compared with the pure Bi, the composite photocatalyst has enhanced visible light response, and the heterojunction of the composite photocatalyst is beneficial to the efficient separation of photo-generated electrons and holes in the catalyst, so that the composite photocatalyst and the pure Bi are further caused 5 O 7 I and Bi 2 MoO 6 Compared with the prior art, the photocatalyst shows obviously improved visible light photocatalytic activity.
The invention has the beneficial effects that:
(1) The invention adopts the method of combining ion replacement and crystal growth to prepare Bi 5 O 7 I/Bi 2 MoO 6 Heterojunction composite nano photocatalyst, and its preparing processSimple, easy to control and low in cost;
(2) Bi prepared by the invention 5 O 7 I/Bi 2 MoO 6 The heterojunction composite nano photocatalyst has good electron-hole separation capability and more surface oxygen vacancy defects, so that the heterojunction composite nano photocatalyst has high-efficiency visible light photocatalytic activity 5 O 7 I and Bi 2 MoO 6 Compared with the prior art, the method is remarkably improved;
(3) Bi prepared by the invention 5 O 7 I/Bi 2 MoO 6 The heterojunction composite nano photocatalyst has good stability and reusability, and can still maintain high catalytic activity after being recycled and used for multiple times.
Drawings
FIG. 1 Bi 5 O 7 I nanofibers and Bi 2 MoO 6 Nanosheet and Bi 5 O 7 I/Bi 2 MoO 6 (62.5%) XRD spectrum of photocatalyst.
FIG. 2 Bi 5 O 7 I nanofibers (a), bi 5 O 7 I/Bi 2 MoO 6 (62.5%) (b) SEM photograph of photocatalyst.
FIG. 3 Bi 5 O 7 I nanofibers and Bi 2 MoO 6 Nanosheet and Bi 5 O 7 I/Bi 2 MoO 6 (62.5%) the photocatalyst showed a visible photocatalytic degradation profile of salicylic acid.
FIG. 4 Bi 5 O 7 I nanofibers and Bi 2 MoO 6 Nanosheet and Bi 5 O 7 I/Bi 2 MoO 6 (62.5%) visible light catalytic degradation of tetracycline hydrochloride by photocatalyst.
FIG. 5 Bi 5 O 7 I/Bi 2 MoO 6 (62.5%) the photocatalyst can be used for degrading salicylic acid by visible light catalysis.
FIG. 6 Bi obtained in comparative example 1 5 O 7 I/Bi 2 MoO 6 SEM photograph of (62.5% -C1).
FIG. 7 Bi obtained in comparative example 2 5 O 7 I/Bi 2 MoO 6 (62.5% -C2)SEM photograph.
FIG. 8 Bi obtained in comparative example 3 5 O 7 I/Bi 2 MoO 6 SEM photograph of (62.5% -C3).
Detailed Description
The present invention will be further illustrated with reference to specific examples for better explaining the present invention, but the present invention is not limited to the following examples.
The specific test method of the photocatalytic activity of the invention is that 30mL of salicylic acid (5 multiplied by 10) is used -5 mol/L) and tetracycline hydrochloride (1X 10) -4 mol/L) solution as target contaminant, 20mg Bi was added 5 O 7 I/Bi 2 MoO 6 And (3) carrying out dark treatment on the heterojunction composite photocatalyst for 30min to ensure that the heterojunction composite photocatalyst reaches adsorption-desorption balance. And (3) irradiating by adopting visible light (lambda is more than 400 nm), measuring the concentration of residual salicylic acid or tetracycline hydrochloride by an ultraviolet-visible spectrophotometer, and calculating the degradation rate.
Example 1
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL of KI solution (0.035 mol/L), performing ultrasonic dispersion for 2min, adding 6mL of NaOH solution with the concentration of 2mol/L, performing magnetic stirring at room temperature for 3h, centrifuging the obtained product, washing the product with deionized water and ethanol, and drying the product at 60 ℃ for 8h to obtain Bi 5 O 7 I, nano-fiber.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 Dispersing the fiber I in 10ml of glycol solution to obtain dispersion A; simultaneously 0.05mmol of Bi (NO) is taken 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.05mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixture E to poly-tetra-polymerPlacing the stainless steel high-pressure reaction kettle with the vinyl fluoride lining into a constant-temperature electric heating air blowing drying oven to react for 16h at 120 ℃, cooling to room temperature after the reaction is finished, centrifuging, washing, and drying for 8h at 60 ℃ to obtain a sample, which is recorded as Bi 5 O 7 I/Bi 2 MoO 6 (25%). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM morphology test shows that the crystal is Bi 5 O 7 I nano-fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 A nanosheet.
Example 2
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL of KI solution (0.035 mol/L), performing ultrasonic dispersion for 2min, adding 6mL of NaOH solution with the concentration of 2mol/L, performing magnetic stirring at room temperature for 3h, centrifuging the obtained product, washing the product with deionized water and ethanol, and drying the product at 60 ℃ for 8h to obtain Bi 5 O 7 I, nano-fiber.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 Dispersing the I in 10ml of glycol solution to obtain a dispersion A; simultaneously taking 0.1mmol of Bi (NO) 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.1mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling to room temperature after the reaction is finished, centrifuging, washing, drying for 8 hours at 60 ℃ to obtain a sample, and marking the sample as Bi 5 O 7 I/Bi 2 MoO 6 (50%). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM appearance test shows that the crystal is Bi 5 O 7 I fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 A nanosheet.
Example 3
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL KI solution (0.035 mol/L), ultrasonically dispersing for 2min, adding 6mL NaOH solution with the concentration of 2mol/L, magnetically stirring for 3h at room temperature, centrifuging the obtained product, washing with deionized water and ethanol, and drying at 60 ℃ for 8h to obtain Bi 5 O 7 And (I) nano fibers.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 I, dispersing in 10ml of glycol solution to obtain a dispersion A; 0.125mmol of Bi (NO) is taken simultaneously 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.125mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying for 8 hours at 60 ℃ to obtain a sample, wherein the sample is recorded as Bi 5 O 7 I/Bi 2 MoO 6 (62.5%). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 Composite components (figure 1). SEM appearance test shows that the crystal is Bi 5 O 7 I fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 Nanoplatelets (fig. 2).
Example 4
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL KI (0.035 mol/L) solution, ultrasonic dispersing for 2min, adding 6mL concentrated solutionNaOH solution with the concentration of 2mol/L, magnetically stirring for 3 hours at room temperature, centrifuging the obtained product, washing with deionized water and ethanol, and drying at 60 ℃ for 8 hours to obtain Bi 5 O 7 And (I) nano fibers.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 I, dispersing in 10ml of glycol solution to obtain a dispersion A; simultaneously taking 0.15mmol of Bi (NO) 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.15mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a 80mL stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8 hours to obtain a sample, recording as Bi 5 O 7 I/Bi 2 MoO 6 (75%). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM morphology test shows that the crystal is Bi 5 O 7 I fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 Nanosheets.
Example 5
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL KI (0.035 mol/L) solution, carrying out ultrasonic dispersion for 2min, adding 6mL NaOH solution with the concentration of 2mol/L, then carrying out magnetic stirring for 3h at room temperature, centrifuging the obtained product, washing the product with deionized water and ethanol, and drying the product for 8h at 60 ℃ to obtain Bi 5 O 7 I, nano-fiber.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 I is first dispersed in 1Dispersing liquid A is obtained after 0ml of glycol solution; simultaneously 0.2mmol of Bi (NO) is taken 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.2mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a 80mL stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electric heating forced air drying oven to react for 9h at 180 ℃, cooling to room temperature after the reaction is finished, centrifuging, washing, and drying for 8h at 60 ℃ to obtain a sample, which is recorded as Bi 5 O 7 I/Bi 2 MoO 6 (100%). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM morphology test shows that the crystal is Bi 5 O 7 I fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 Nanosheets.
Bi prepared in all the above examples 5 O 7 I/Bi 2 MoO 6 Composite nano photocatalyst and pure Bi 5 O 7 I nanofibers and pure Bi 2 MoO 6 Compared with the nano-sheets, the nano-sheets have obviously improved activity of degrading salicylic acid and tetracycline hydrochloride by visible light photocatalysis, wherein Bi 5 O 7 I/Bi 2 MoO 6 (62.5%) sample has salicylic acid degradation rate up to 95% (pure Bi under the same condition) 5 O 7 I nanofibers and Bi 2 MoO 6 The degradation rate of the nano-sheets is only 29% and 34%, see figure 3), bi 5 O 7 I/Bi 2 MoO 6 (62.5%) the degradation rate of tetracycline hydrochloride of the sample can reach 66% (pure Bi under the same condition) 5 O 7 I nanofibers and Bi 2 MoO 6 The degradation rate of the nanoplatelets was only 27% and 30%, see fig. 4). In addition, the composite photocatalyst has good stability and reusability, and still maintains high catalytic activity after being used for multiple times of circular catalysis, for example, bi 5 O 7 I/Bi 2 MoO 6 (62.5%) samples were cycled 4 timesThe high catalytic activity is still maintained after the salicylic acid is catalytically degraded, and the figure 5 shows.
Comparative example 1
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL KI (0.035 mol/L) solution, carrying out ultrasonic dispersion for 2min, adding 6mL NaOH solution with the concentration of 2mol/L, then carrying out magnetic stirring for 3h at room temperature, centrifuging the obtained product, washing the product with deionized water and ethanol, and drying the product for 8h at 60 ℃ to obtain Bi 5 O 7 I, nano-fiber.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 I, dispersing in 10ml of glycol solution to obtain a dispersion A; simultaneously taking 0.25mmol of Bi (NO) 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.125mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a 80mL stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8 hours to obtain a sample, recording as Bi 5 O 7 I/Bi 2 MoO 6 (62.5% -C1). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM appearance test shows that the crystal is Bi 5 O 7 The surface of the I nano fiber still grows Bi 2 MoO 6 Nanosheets, but the number of nanosheets was significantly reduced (fig. 6). Under the same conditions, the efficiency of the visible light to degrade the salicylic acid and the tetracycline is 45 percent and 50 percent respectively, which is obviously lower than that of the Bi of the example 3 5 O 7 I/Bi 2 MoO 6 (62.5%) degradation efficiency.
Comparative example 2
(1) Bi 5 O 7 I, preparation of nano-fibers: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL of KI (0.035 mol/L) solution, performing ultrasonic dispersion for 2min, adding 6mL of NaOH solution with the concentration of 2mol/L, performing magnetic stirring at room temperature for 3h, centrifuging the obtained product, washing the product with deionized water and ethanol, and drying the product at 60 ℃ for 8h to obtain Bi 5 O 7 I, nano-fiber.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 Dispersing the I in 10ml of glycol solution to obtain a dispersion A; simultaneously 0.125mmol of Bi (NO) is taken 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.125mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a 80mL stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, drying at 60 ℃ for 8 hours, calcining the obtained sample at 300 ℃ for 0.5 hour to obtain a final sample, and marking the final sample as Bi 5 O 7 I/Bi 2 MoO 6 (62.5% -C2). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM appearance test shows that the crystal is Bi 5 O 7 I fiber surface is uniformly and vertically grown with a large amount of Bi 2 MoO 6 Nanoplatelets (fig. 7). Due to the calcination treatment, the oxygen vacancy on the surface of the photocatalyst material is reduced, so that the activity of the photocatalyst material for degrading salicylic acid and tetracycline by visible light is obviously reduced, the degradation efficiency is only 60 percent and 61 percent respectively, and the degradation efficiency is obviously lower than that of Bi in example 3 5 O 7 I/Bi 2 MoO 6 (62.5%) degradation efficiency.
Comparative example 3
(1) Bi 5 O 7 I sodiumPreparation of rice granules: 2.8mmol of Bi (NO) 3 ) 3 •5H 2 Dispersing O into 80mL of KI (0.035 mol/L) solution, ultrasonically dispersing for 2min, adding 6mL of NaOH solution with the concentration of 2mol/L, magnetically stirring at room temperature for 30min, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electric heating air blast drying oven to react for 12h at 160 ℃, cooling to room temperature after the reaction is finished, centrifuging and washing, putting the obtained product into the same reaction solution again, carrying out hydrothermal growth for 12h at 160 ℃, cooling to room temperature after the reaction is finished, centrifuging the obtained product, washing with deionized water and ethanol, drying at 60 ℃ for 8h, putting the obtained product into a mortar, and grinding for 20 min to obtain Bi 5 O 7 And (I) nanoparticles.
(2) Bi 5 O 7 I/Bi 2 MoO 6 Preparing a composite photocatalyst: 0.2mmol of Bi prepared in the step (1) 5 O 7 Dispersing I nano particles in 10ml of glycol solution to obtain a dispersion A; 0.125mmol of Bi (NO) is taken simultaneously 3 ) 3 •5H 2 Dissolving O in 10ml of glycol solution to obtain solution B; and adding 0.125mmol of Na 2 MoO 4 •2H 2 Adding O into 40ml of deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electrothermal blowing drying oven to react for 12 hours at 160 ℃, cooling to room temperature after the reaction is finished, centrifuging, washing, drying for 8 hours at 60 ℃ to obtain a sample, and marking the sample as Bi 5 O 7 I/Bi 2 MoO 6 (62.5% -C3). XRD test of the catalyst shows that the catalyst is Bi 5 O 7 I/Bi 2 MoO 6 And (3) compounding the components. SEM appearance test shows that the crystal is Bi 5 O 7 I nanoparticles surface coated with a large amount of Bi 2 MoO 6 Nanosheet coating (fig. 8). Due to the composite structure, bi 5 O 7 The I component is changed from nano-fiber to nano-particle, resulting in photo-generated carriers in the interior thereofThe transfer efficiency is reduced, the electron-hole recombination is increased, the activity of visible light catalytic degradation of salicylic acid and tetracycline is obviously reduced, the degradation efficiency is only 60 percent and 51 percent respectively, and the degradation efficiency is obviously lower than that of Bi in example 3 5 O 7 I/Bi 2 MoO 6 (62.5%) degradation efficiency.
Claims (2)
1. Bi 5 O 7 I/Bi 2 MoO 6 The preparation method of the composite photocatalyst is characterized in that the photocatalyst is Bi 5 O 7 I nano-fiber as substrate, in Bi 5 O 7 Vertical growth of Bi on I nanofibers 2 MoO 6 Nanoplatelets of which Bi 5 O 7 The length of the I fiber is 0.5 to 10 mu m, the width is 50 to 1000nm, the thickness is 10 to 600nm 2 MoO 6 The thickness of the nano sheet is 2 to 150nm;
the method specifically comprises the following steps:
(1) Bi 5 O 7 i, preparation of nano-fibers: adding Bi (NO) 3 ) 3 •5H 2 Dispersing O into KI solution, performing ultrasonic dispersion, adding a certain amount of NaOH solution, performing magnetic stirring at room temperature, centrifuging the obtained product, washing with deionized water and ethanol, and drying to obtain Bi 5 O 7 I, nano-fibers;
(2) Bi 5 O 7 I/Bi 2 MoO 6 preparing a composite photocatalyst: bi prepared in the step (1) 5 O 7 Firstly dispersing the nano-fibers in a glycol solution to obtain a dispersion A; simultaneously taking a certain amount of Bi (NO) 3 ) 3 •5H 2 Dissolving O in the ethylene glycol solution to obtain a solution B; and mixing Na 2 MoO 4 •2H 2 Adding O into deionized water, and magnetically stirring until the O is completely dissolved to obtain a solution C; then dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 5 minutes to obtain a mixed liquid D; dropwise adding the solution C into the mixed solution D, and magnetically stirring for 30 minutes to obtain a mixed solution E; transferring the mixed solution E into a stainless steel high-pressure reaction kettle containing a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into a constant-temperature electrothermal blowing drying oven for reaction, cooling to room temperature after the reaction is finished, centrifuging, washing and drying to obtain the polytetrafluoroethylene composite materialBi 5 O 7 I/Bi 2 MoO 6 A composite photocatalyst;
in the step (1), the concentration of the KI solution is 0.035mol/L; the Bi (NO) 3 ) 3 •5H 2 The ratio of the amounts of substances of O and KI is 1; the concentration of the NaOH solution is 2mol/L, and the volume ratio of the NaOH solution to the KI solution is 6:80; the ultrasonic dispersion time is 2min; the magnetic stirring time is 3 hours; the drying is drying for 8 hours at 60 ℃;
in the step (2), bi in the dispersion liquid A 5 O 7 The molar volume ratio of I to ethylene glycol is 0.2mmol; bi (NO) in the solution B 3 ) 3 •5H 2 The molar volume ratio of O to ethylene glycol is 0.05 to 0.2mmol:10mL; na in the solution C 2 MoO 4 •2H 2 The molar volume ratio of O to deionized water is 0.05 to 0.2mmol: 40mL;
in the step (2), the Na 2 MoO 4 •2H 2 O and Bi (NO) 3 ) 3 •5H 2 The molar ratio of O is 1:1; na (Na) 2 MoO 4 •2H 2 O and Bi 5 O 7 The molar ratio of I is 0.25 to 1;
in the step (2), the reaction is carried out for 8 to 1697 h by hydrothermal treatment at the temperature of 120 to 180 ℃; the drying is carried out at 60 ℃ for 8 hours.
2. Bi prepared by the preparation method of claim 1 5 O 7 I/Bi 2 MoO 6 The composite photocatalyst is applied to the degradation of organic pollutants.
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