CN107715896B - BiOI/BiVO4 composite photocatalyst and preparation method and application thereof - Google Patents
BiOI/BiVO4 composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 71
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 63
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002135 nanosheet Substances 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000007664 blowing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 9
- 230000000593 degrading effect Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 229910003206 NH4VO3 Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 21
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 230000015556 catabolic process Effects 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract 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 abstract description 13
- 229940043267 rhodamine b Drugs 0.000 abstract description 13
- 150000002500 ions Chemical class 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 description 8
- 238000013329 compounding Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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- 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
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/038—Precipitation; Co-precipitation to form slurries or suspensions, e.g. a washcoat
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to BiOI/BiVO4A composite photocatalyst and a preparation method and application thereof. The composite photocatalyst is a two-dimensional composite nanosheet, and BiVO grows on the BiOI nanosheet on the basis of the BiOI nanosheet4A nanosheet layer. The invention adopts a simple ion replacement method to prepare BiOI/BiVO4The heterojunction composite nanosheet photocatalyst has the advantages of simple preparation method, easy control and low cost; has good visible light absorption performance; the catalyst prepared by the invention is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4(V: I =80%) the degradation rate of the heterojunction composite photocatalyst on rhodamine B with the volume of 50mL and the concentration of 5mg/L can reach 97%, and complete degradation can be realized within 90 min.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to BiOI/BiVO4A composite photocatalyst and a preparation method and application thereof.
Background
With the rapid development of society, the shortage of energy and the increasingly strict environmental problems threaten the survival and health of human beings. Semiconductor photocatalytic technology is considered to be one of the most effective ways to solve energy crisis and environmental problems. But conventional semiconductors, e.g. TiO2ZnO and the like have the defects of wide forbidden band width, capability of only absorbing ultraviolet light, fast recombination of photon-generated carriers and the like. In order to better utilize sunlight and improve the photocatalytic activity of the sunlight, development of efficient visible light driven photocatalysts is a trend of photocatalytic technology development.
The bismuth-based photocatalyst has a unique structure and good light absorption performance,has attracted the attention of people. Such as bismuth oxyhalide (BiOX, X = Cl, Br, I), typically from [ Bi ]2O2]2+Layer and double X-The layer structure formed by the alternating layers is favorable for the rapid separation of electrons and holes. Among them, the BiOI as a p-type semiconductor has a small forbidden band width (1.7-1.9 eV), and can effectively absorb visible light, thereby attracting much attention of people. Bismuth vanadate (BiVO)4) The photocatalyst is an n-type semiconductor, and has high photocatalytic activity and good stability under visible light due to the appropriate forbidden bandwidth (-2.4 eV), so that the photocatalyst is one of the most widely researched visible light catalysts at present. Because of the single semiconductor photocatalyst, the photon-generated carriers are easy to compound and the separation efficiency is low, the absolute photocatalytic activity of the semiconductor photocatalyst is still low. The n-type semiconductor and the p-type semiconductor are compounded to form a p-n heterostructure, and a self-established electric field in the heterostructure is favorable for effectively separating photo-generated electrons from holes, so that the catalytic activity of the heterostructure is improved. Therefore, the preparation of the composite photocatalyst with the p-n heterojunction becomes a research hotspot in the preparation and application aspects of the existing photocatalyst.
Disclosure of Invention
Aiming at the problem of low activity of the existing photocatalyst, the invention provides BiOI/BiVO4The composite photocatalyst has high photocatalytic activity and good reusability.
The invention also provides a BiOI/BiVO4A preparation method and application of the composite photocatalyst.
The specific technical scheme of the invention is as follows:
the invention provides a BiOI/BiVO4A composite photocatalyst, said BiOI/BiVO4Is a two-dimensional composite nano-sheet, takes a BiOI nano-sheet as a base, and grows BiVO on the BiOI nano-sheet4A nanosheet layer.
The invention also provides a BiOI/BiVO4The preparation method of the composite photocatalyst comprises the following steps:
(1) preparing a BiOI nanosheet: adding Bi (NO)3)3·5H2O is dispersed intoUltrasonically dispersing in a KI solution, magnetically stirring for 5 hours at room temperature, centrifuging, washing with deionized water and ethanol, and drying to obtain the two-dimensional BiOI nanosheet.
（2）BiOI/BiVO4Preparing a two-dimensional heterojunction composite nanosheet photocatalyst: dispersing the BiOI prepared in the step (1) into deionized water to obtain a dispersion liquid A; simultaneously reacting NH4·VO3Adding the mixture into deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a solution B; dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 15 minutes to obtain a mixed liquid C; transferring the mixed solution C into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing dry box for reaction, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8 hours to obtain the BiOI/BiVO with the two-dimensional heterostructure4A nanosheet composite photocatalyst.
Further, in the step (1), Bi (NO)3)3·5H2The ratio of the amounts of O and KI substances was 1: 1.
Further, the time of ultrasonic dispersion is 2 min; the drying is carried out at 60 ℃ for 8 h.
Further, in the step (2), the NH4·VO3And the molar ratio of the BiOI to the BiOI is 0.2-0.9: 1.
Further, in the step (2), the reaction is carried out for 8-16 h under the condition of the temperature of 120-200 ℃.
Further, in the step (2), the drying is carried out at 60 ℃ for 8 h.
The invention also provides BiOI/BiVO prepared by the preparation method4The application of the composite photocatalyst in degrading organic dye.
The invention grows BiVO on the BiOI nano-chip by ion replacement4And the nano thin layer is constructed to form the composite nano sheet photocatalyst with a two-dimensional heterojunction structure, and the photocatalytic performance of the photocatalyst is obviously improved.
The invention has the beneficial effects that:
(1) the invention adopts a simple ion replacement method to prepare BiOI/BiVO4The heterojunction composite nanosheet photocatalyst has the advantages of simple preparation method, easy control and low cost;
(2) BiOI/BiVO prepared by the invention4The heterojunction composite nanosheet photocatalyst has a two-dimensional p-n heterogeneous interface, a large specific surface area, good electron-hole pair separation capacity, a wide visible light spectrum response range and good visible light absorption performance;
(3) BiOI/BiVO prepared by the invention4BiOI and BiVO with single visible light catalytic activity of heterojunction composite nanosheet photocatalyst4Are all obviously improved, and 30mg of BiOI/BiVO is irradiated under 75min of visible light4(V: I =80%) the degradation rate of the heterojunction composite photocatalyst on rhodamine B with the volume of 50mL and the concentration of 5mg/L can reach 97%, and complete degradation can be realized within 90 min.
(4) BiOI/BiVO prepared by the invention4The heterojunction composite photocatalyst has good stability and reusability, and still has higher photocatalytic activity after being recycled for 4 times.
Drawings
FIG. 1 BiOI, BiVO4、80％BiOI/BiVO4XRD spectrum of photocatalyst.
FIG. 2 BiOI (a), 80% BiOI/BiVO4(b) SEM photograph of the photocatalyst.
Graph 380% BiOI/BiVO4TEM photograph of the photocatalyst.
FIG. 4 BiOI, BiVO4、80％BiOI/BiVO4Ultraviolet-visible diffuse reflection absorption spectrum of the photocatalyst.
FIG. 5 pure BiOI, BiVO4、80％BiOI/BiVO4And (3) degrading the rhodamine B by the catalysis of the photocatalyst.
Graph 680% BiOI/BiVO4The photocatalyst catalyzes and degrades the reusability of rhodamine B.
Detailed Description
The present invention is further illustrated by the following specific examples, which are given solely for the purpose of illustration and are not intended to be limiting.
The specific test method for the photocatalytic activity comprises the following steps: adding 30mg of BiOI/BiVO into 50mL of rhodamine B solution with the concentration of 5mg/L as a target degradation product4Carrying out dark treatment on the heterojunction composite photocatalyst for 30 min to balance the adsorption of the photocatalyst on rhodamine B, and then adopting the wavelength lambda>Irradiating by a 400nm light source, sampling at certain time intervals in the illumination process, measuring the concentration of the residual rhodamine B by an ultraviolet-visible spectrophotometer, and calculating the degradation rate.
Example 1
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.3mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 160 ℃ for 12h, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8h to obtain a sample, which is marked as 30% BiOI/BiVO4. XRD test of the catalyst shows that the catalyst is BiOI/BiVO4And (3) compounding components, wherein SEM morphology test shows that the nano-sheet is a nano-sheet, and EDS element analysis test shows that Bi, I, V and O elements on the surface of the nano-sheet are uniformly distributed, so that the nano-sheet is a two-dimensional composite heterojunction nano-sheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The degradation rate of the heterojunction composite photocatalyst to rhodamine B with the volume of 50mL and the concentration of 5mg/L can reach 73.8 percent (pure BiOI and BiVO)4The degradation rate under the same conditions is only 42.4% and 11.1%, see fig. 5). The BiOI is-BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has higher photocatalytic activity after being recycled for 4 times.
Example 2
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.5mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 160 ℃ for 12h, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8h to obtain a sample, which is marked as 50% BiOI/BiVO4. XRD test of the catalyst shows that the catalyst is BiOI/BiVO4And (3) compounding components, wherein SEM morphology test shows that the nano-sheet is a nano-sheet, and EDS element analysis test shows that Bi, I, V and O elements on the surface of the nano-sheet are uniformly distributed, so that the nano-sheet is a two-dimensional composite heterojunction nano-sheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The degradation rate of the heterojunction composite photocatalyst to rhodamine B with the volume of 50mL and the concentration of 5mg/L can reach 89.4 percent (pure BiOI and BiVO)4The degradation rate under the same conditions is only 42.4% and 11.1%, see fig. 5). The BiOI/BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has higher photocatalytic activity after being recycled for 4 times.
Example 3
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.8mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 160 ℃ for 12h, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8h to obtain a sample, which is marked as 80% BiOI/BiVO4。
80% BiOI/BiVO prepared in this example4The XRD pattern of the photocatalyst is shown in figure 1, and from figure 1, the obvious BiOI and BiVO can be seen4The diffraction peak of (A) proves that the catalyst is BiOI/BiVO4And (3) compounding the components. 80% BiOI/BiVO4The SEM image of the photocatalyst is shown in FIG. 2, and it can be seen that the photocatalyst has a two-dimensional sheet structure; 80% BiOI/BiVO4The TEM photograph of the photocatalyst is shown in fig. 3, and it can be seen that the photocatalyst is a uniform BiVO having a uniform thickness of the base of the BiOI nanosheet4On which the replacement (epitaxial) growth (darker colored regions in the figure) takes place. EDS element analysis tests show that Bi, I, V and O elements on the surface of the nanosheet are uniformly distributed. Furthermore, the UV-visible diffuse reflectance absorption spectrum is shown in FIG. 4, 80% BiOI/BiVO4Having both BiOI and BiVO4Further proving that it is BiOI/BiVO4And (3) compounding the components. In conclusion, it is proved to be a two-dimensional composite heterojunction nanosheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4Heterojunction composite photocatalyst is 50mL for volume, concentration is 5mg/L luoThe degradation rate of the danming B can reach 97 percent (pure BiOI and BiVO)4The degradation rate under the same conditions was only 42.4% and 11.1%), as shown in FIG. 5. The BiOI/BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has high photocatalytic activity after 4 times of recycling (when the photocatalyst is reused for the fourth time, the photocatalytic degradation rate can still reach 74%), as shown in figure 6.
Example 4
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.75mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 120 ℃ for 16h, cooling the mixture to room temperature after the reaction is finished, centrifuging, washing, and drying at 60 ℃ for 8h to obtain a sample, which is marked as 75% BiOI/BiVO4. XRD test of the catalyst shows that the catalyst is BiOI/BiVO4And (3) compounding components, wherein SEM morphology test shows that the nano-sheet is a nano-sheet, and EDS element analysis test shows that Bi, I, V and O elements on the surface of the nano-sheet are uniformly distributed, so that the nano-sheet is a two-dimensional composite heterojunction nano-sheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The heterojunction composite photocatalyst is used for carrying out photocatalytic degradation on rhodamine B with the volume of 50mL and the concentration of 5mg/L, and the activity of the photocatalyst is superior to that of pure BiOI and BiVO4. The BiOI/BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has high light after being recycled for 4 timesAnd (3) catalytic activity.
Example 5
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.4mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 200 ℃ for 8h, cooling the mixture to room temperature after the reaction is finished, centrifuging the mixture, washing the mixture, and drying the mixture for 8h at 60 ℃ to obtain a sample, which is recorded as 40% BiOI/BiVO4. XRD test of the catalyst shows that the catalyst is BiOI/BiVO4And (3) compounding components, wherein SEM morphology test shows that the nano-sheet is a nano-sheet, and EDS element analysis test shows that Bi, I, V and O elements on the surface of the nano-sheet are uniformly distributed, so that the nano-sheet is a two-dimensional composite heterojunction nano-sheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The heterojunction composite photocatalyst is used for carrying out photocatalytic degradation on rhodamine B with the volume of 50mL and the concentration of 5mg/L, and the activity of the photocatalyst is superior to that of pure BiOI and BiVO4. The BiOI/BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has higher photocatalytic activity after being recycled for 4 times.
Example 6
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2O is dispersed in 80mL KI (0.035mol/L) solution, dispersed by ultrasonic for 2min, then stirred magnetically for 5h at room temperature, then centrifuged, washed with deionized water and ethanol, anddrying for 8 hours at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 0.7mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 160 ℃ for 12h, cooling the mixture to room temperature after the reaction is finished, centrifuging the mixture, washing the mixture, and drying the mixture for 8h at 60 ℃ to obtain a sample, which is marked as 70% BiOI/BiVO4. XRD test of the catalyst shows that the catalyst is BiOI/BiVO4And (3) compounding components, wherein SEM morphology test shows that the nano-sheet is a nano-sheet, and EDS element analysis test shows that Bi, I, V and O elements on the surface of the nano-sheet are uniformly distributed, so that the nano-sheet is a two-dimensional composite heterojunction nano-sheet.
The catalyst prepared in the example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The degradation rate of the heterojunction composite photocatalyst to rhodamine B with the volume of 50mL and the concentration of 5mg/L can reach 94.2 percent (pure BiOI and BiVO)4The degradation rate under the same conditions is only 42.4% and 11.1%, see fig. 5). The BiOI/BiVO4The heterojunction composite photocatalyst has good stability and reusability, and still has higher photocatalytic activity after being recycled for 4 times.
Comparative example 1
(1) Preparing a BiOI nanosheet: 2.8mmol of Bi (NO)3)3·5H2Dispersing O into 80mL of KI (0.035mol/L) solution, performing ultrasonic dispersion for 2min, then performing magnetic stirring for 5h at room temperature, then centrifuging, washing with deionized water and ethanol, and drying for 8h at 60 ℃ to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite photocatalyst: dispersing 1mmol of BiOI prepared in the step (1) into 30mL of deionized water to obtain a dispersion liquid; simultaneously adding 1.1 mmol of NH4·VO3Adding the mixture into 30mL of deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a dissolved solution; then NH is added4·VO3Dropwise adding the dissolved solution into the BiOI dispersion liquid, and magnetically stirring for 15min to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the mixture into a constant-temperature electrothermal blowing drying oven for heat treatment at 160 ℃ for 12h, cooling the mixture to room temperature after the reaction is finished, centrifuging the mixture, washing the mixture, and drying the mixture for 8h at 60 ℃ to obtain a sample, which is marked as 110% BiOI/BiVO4. XRD test shows that the main component of the catalyst is BiVO4And contains a small amount of BiOI component. SEM morphology tests show that the sheet morphology of the photocatalyst is damaged to a great extent.
The catalyst prepared in the comparative example is irradiated by visible light for 75min, and 30mg of BiOI/BiVO4The degradation rate of the heterojunction composite photocatalyst to rhodamine B with the volume of 50mL and the concentration of 5mg/L is only 25.2 percent and is lower than the degradation rate of 42.4 percent of pure BiOI under the same condition (see figure 5).
Claims (6)
1. BiOI/BiVO4The preparation method of the composite photocatalyst is characterized in that the BiOI/BiVO4Is a two-dimensional composite nano-sheet, takes a BiOI nano-sheet as a base, and grows BiVO on the BiOI nano-sheet4A nanosheet layer;
the method specifically comprises the following steps:
(1) preparing a BiOI nanosheet: adding Bi (NO)3)3·5H2Dispersing O into a KI solution, performing ultrasonic dispersion, then magnetically stirring at room temperature for 5 hours, centrifuging, washing with deionized water and ethanol, and drying to obtain a two-dimensional BiOI nanosheet;
（2）BiOI/BiVO4preparing a two-dimensional heterojunction composite nanosheet photocatalyst: dispersing the BiOI prepared in the step (1) into deionized water to obtain a dispersion liquid A; simultaneously reacting NH4VO3Adding the mixture into deionized water, and magnetically stirring until the mixture is completely dissolved to obtain a solution B; dropwise adding the solution B into the dispersion liquid A, and magnetically stirring for 15 minutes to obtain a mixed liquid C; transferring the mixed solution C into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the 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 at 60 ℃ for 8 hours to obtain the BiOI/BiVO with the two-dimensional heterostructure4A nanosheet composite photocatalyst.
2. The method according to claim 1, wherein in the step (1), the Bi (NO) is3)3·5H2The ratio of the amounts of O and KI substances was 1: 1.
3. The production method according to claim 2, wherein in the step (1), the time for the ultrasonic dispersion is 2 min; the drying is carried out at 60 ℃ for 8 h.
4. The method according to claim 1, wherein in the step (2), the NH is4VO3And the molar ratio of the BiOI to the BiOI is 0.2-0.9: 1.
5. The preparation method according to claim 1 or 4, wherein in the step (2), the reaction is carried out at a temperature of 120 ℃ to 200 ℃ for 8 to 16 hours.
6. BiOI/BiVO prepared by the preparation method of any one of claims 1 to 44The application of the composite photocatalyst in degrading organic dye.
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| CN111686767B (en) * | 2020-05-21 | 2021-11-23 | 华南理工大学 | Microspherical Bi3O4Preparation and application of Cl/BiOI compound |
| CN113070057B (en) * | 2021-03-31 | 2022-05-17 | 中南大学 | Photoelectric-piezoelectric composite material and preparation method thereof |
| CN113101954B (en) * | 2021-04-02 | 2022-11-11 | 济南大学 | Bi 5 O 7 I/Bi 2 MoO 6 Composite photocatalyst and preparation method and application thereof |
| CN113181937A (en) * | 2021-04-27 | 2021-07-30 | 新乡学院 | Bi5O7I/Bi2SiO5Preparation method and application of nano composite photocatalyst |
| CN113403642B (en) * | 2021-05-24 | 2022-09-16 | 江苏大学 | BiVO 4 /Co 1-X Preparation method and application of S composite photoelectrode |
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