CN106955721B - A kind of preparation method of the Bi5O7Br nano-photocatalyst material of banded structure - Google Patents
A kind of preparation method of the Bi5O7Br nano-photocatalyst material of banded structure Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 58
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002086 nanomaterial Substances 0.000 claims abstract description 12
- 150000001621 bismuth Chemical class 0.000 claims abstract description 9
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 8
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 claims description 5
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 4
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 4
- -1 bismuth salt Chemical class 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 18
- 238000006731 degradation reaction Methods 0.000 abstract description 18
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 11
- 229940012189 methyl orange Drugs 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 238000002474 experimental method Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000001000 micrograph Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 54
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 22
- 229940106691 bisphenol a Drugs 0.000 description 11
- 238000001878 scanning electron micrograph Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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
- C02F2305/08—Nanoparticles or nanotubes
-
- 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 nano material and solar energy photocatalytic fields, specifically disclose a kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material.It is primary raw material using soluble bismuth salt and bromine-containing compound, banded structure Bi is prepared by solvent-thermal method5O7Br nano-photocatalyst material, crystalline state is good, purity is high, without obvious impurity thing phase, the Bi of scanning electron microscope image display synthesis5O7The microstructure of Br is a kind of especially regular banded structure.The Bi of banded structure obtained by the present invention5O7Br nano-photocatalyst material has preferable visible light activity, shows high photocatalytic activity in the experiment of simulated visible light degradation methyl orange.The Bi for the banded structure that the present invention synthesizes5O7The synthetic method of Br nano-photocatalyst material is simple, it is easy to operate, be conducive to large-scale industrial production.
Description
Technical field
The present invention relates to nano material and solar energy photocatalytic fields, and in particular to a kind of Bi of banded structure5O7Br receives
The preparation method of rice catalysis material.
Background technique
BixOyBrzNano material is due to its unique optics, electrical properties etc., by as a kind of novel semiconductor material
Material, is widely used in photocatalysis field.
In recent years, have much about BixOyBrzThe research of synthetic method and characters and appearances reports that synthetic method mainly includes
Solid-phase synthesis, hydro-thermal method, microwave assisting method etc., characters and appearances mainly include one-dimensional nanobelt, nanotube, two-dimensional nanometer
Piece, nanometer plate and nanosphere of three-dimensional etc..Wherein, Li Yadong seminar Surfactant CTAB makees chlorine source, utilizes hydro-thermal
Method has synthesized the BiOBr of nano strip and tubulose, Bi by the pH value and reaction temperature of control system24O31Br10, Bi3O4Br,
Bi12O17Br2[Yadong Li et al.Chem. Eur.J.2005,11,6519-6524]；Keller E et al. uses Bi2O3
And BiBr3, Bi has been obtained for the first time under pyroreaction5O7Br monocrystal nanostructure [Keller E et al.Acta
Crystallographica Section C: Crystal Structure Communications,2007,63(12):
i109-i111]；Li Liqun seminar Surfactant CTAB makees bromine source, passes through control using hydro-thermal method under water solution system
The pH value and reaction temperature of system processed have synthesized the Bi of nano bar-shape5O7Br, [Yeling Qun et al.Applied
Surface Science. 2015,346,311–316].Existing research shows that Bi5O7Br material under visible light all have compared with
Good photocatalytic activity, can effectively pollutants such as rhodamine B degradation, methyl orange, phenol, saligenin, administering or repairing
It can play the role of in terms of ecological environment good.
Research has shown that, Bi5O7Br nano material is a kind of ideal and up-and-coming catalysis material.Chinese patent
Apply for " visible light catalyst Bi5O7Br and preparation method thereof " (number of patent application 201410029932.9) utilizes bismuth salt and CTAB
For raw material, hydro-thermal method is taken to be prepared for the star-like visible light catalyst Bi of cross5O7Br.However, this patent that there are products is impure,
The defects of microscopic appearance is irregular uniform, present application addresses these defects, prepared high-purity, regular appearance is uniform,
Band-like Bi with high light catalytic activity5O7Br nano material, such band-like Bi5O7Br nano material is domestic and international so far still
It has not been reported.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of Bi of banded structure5O7Br
The preparation method of nano-photocatalyst material.The Bi that the present invention prepares5O7Br nano-photocatalyst material has typical nanobelt knot
Structure.
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) soluble bismuth salt is dissolved in small-molecular-weight alcohol, small-molecular-weight alcohol ratio used in soluble bismuth salt/this step
It for 2mmol:(25-40) mL, is stirred continuously to soluble bismuth salt and is completely dissolved, obtain solution A；
The soluble bismuth salt is one of bismuth nitrate, bismuth bromide and bismuth sulfate or two to three kinds of arbitrary proportion mixing
Object, preferably bismuth nitrate；
(2) bromine-containing compound and polyvinylpyrrolidone are dissolved in small-molecular-weight alcohol, make solubility used in step (1)
Small-molecular-weight alcohol ratio used in bismuth salt/bromine-containing compound/polyvinylpyrrolidone/this step is 2mmol:2mmol:(0.6-
1.2) g:(25-40) mL, solution B is obtained after mixing evenly；
The small-molecular-weight alcohol is methanol or ethyl alcohol, preferably methanol；The ethyl alcohol is preferably dehydrated alcohol, and methanol is excellent
It is selected as anhydrous methanol；
The bromine-containing compound be one of CTAB (cetyl trimethylammonium bromide), potassium bromide and bromobenzene or two to
Three kinds of arbitrary proportion mixture；
(3) solution A is added in solution B, obtains solution C after mixing evenly, then the aqueous slkali of (1-3) mol/L is slowly added
Enter in solution C, adjusts pH=12.5-13.5, obtain solution D；
The aqueous slkali is sodium hydroxide solution or potassium hydroxide solution, preferably potassium hydroxide solution；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, the isothermal reaction 5- under the conditions of 150-200 DEG C
24h；
(5) obtained precipitating is successively washed with deionized water and dehydrated alcohol after reaction, each washing 3-4 times, so
Product is put afterwards and is dried in an oven, the Bi of banded structure is obtained5O7Br nano material.
Compared with prior art, the advantages of the present invention are as follows:
1, a kind of Bi of banded structure has successfully been prepared5O7Br nano material；
2, this Bi5O7Br nano material, purity is higher, has typical nanometer band structure, and regular appearance is uniform；
3, there is high light catalytic activity, can effectively degrade the pollutants such as methyl orange, BPA, administer or repairing life
It can play the role of in terms of state environment good.
Detailed description of the invention
Fig. 1 is banded structure Bi prepared by embodiment 15O7The XRD spectrum of Br nano-photocatalyst material shows system in figure
The Bi obtained5O7Br crystallinity is preferable, substantially the not presence of miscellaneous peak.
Fig. 2 is banded structure Bi prepared by embodiment 15O7The SEM image of Br nano-photocatalyst material, low power SEM in figure
Image shows Bi obtained5O7Br microstructure is evenly distributed and very regular, and high power SEM image can clearly be seen that its typical case
Beltlike nanostructures, the width of banded structure is about 300nm, and the length of banded structure is about 1-10 μm.
Fig. 3 is banded structure Bi prepared by embodiment 15O7The DRS map of Br nano-photocatalyst material, uv drs
Spectral detection shows Bi of the invention5O7Br has certain absorption, and absorption maximum edge from ultraviolet region to visible region
At 463 nanometers, forbidden band width is 2.68eV.
Fig. 4 is the Bi prepared with embodiment 15O7Br nano-photocatalyst material is under visible light to the degradation curve of methyl orange.
It can be seen from the figure that the Bi of banded structure under visible light illumination5O7Br nano-photocatalyst material is bright to methyl orange degradation effect
Aobvious, degradation rate is 93.7% when 50min.
Fig. 5 is the Bi prepared with embodiment 15O7Br nano-photocatalyst material is under visible light to the degradation curve of BPA.From
It can be seen that the Bi of banded structure under visible light illumination in figure5O7Br nano-photocatalyst material is obvious to BPA degradation effect,
Degradation rate is 96.1% when 25min.
Fig. 6 is novel strip-like structure Bi prepared by embodiment 25O7The XRD spectrum of Br nano-photocatalyst material is shown in figure
Show Bi obtained5O7Br crystallinity is preferable, substantially the not presence of miscellaneous peak.
Fig. 7 is novel strip-like structure Bi prepared by embodiment 25O7The SEM image of Br nano-photocatalyst material.
Fig. 8 is novel strip-like structure Bi prepared by embodiment 35O7The XRD spectrum of Br nano-photocatalyst material is shown in figure
Show Bi obtained5O7Br crystallinity is preferable, substantially the not presence of miscellaneous peak.
Fig. 9 is novel strip-like structure Bi prepared by embodiment 35O7The SEM image of Br nano-photocatalyst material.
Figure 10 is novel strip-like structure Bi prepared by embodiment 45O7The XRD spectrum of Br nano-photocatalyst material is shown in figure
Show Bi obtained5O7Br crystallinity is preferable, substantially the not presence of miscellaneous peak.
Figure 11 is novel strip-like structure Bi prepared by embodiment 45O7The SEM image of Br nano-photocatalyst material.
Figure 12 is novel strip-like structure Bi prepared by embodiment 55O7The XRD spectrum of Br nano-photocatalyst material is shown in figure
Show Bi obtained5O7Br crystallinity is preferable, substantially the not presence of miscellaneous peak.
Figure 13 is novel strip-like structure Bi prepared by embodiment 55O7The SEM image of Br nano-photocatalyst material.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, below applicant will in conjunction with the embodiments
The present invention is described in further details with attached drawing.
Raw material sources in following embodiment: polyvinylpyrrolidone, product number P110607, CAS 9003-39-8,
Sinopharm Chemical Reagent Co., Ltd..
Embodiment 1:
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) five water bismuth nitrate (Bi (NO of 2mmol is weighed3)3·5H2O) be dissolved in 25ml anhydrous methanol, be stirred continuously to
Bismuth nitrate obtains solution A after being completely dissolved；
(2) it weighs 2mmol CTAB and 0.6g polyvinylpyrrolidone to be dissolved in 25ml anhydrous methanol, after mixing evenly
Obtain solution B；
(3) solution A is added in solution B, obtains solution C after mixing evenly, then the sodium hydroxide solution of 1mol/L is slow
It is added in solution C, adjusts pH=13.10, obtain solution D；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, the isothermal reaction 5h under the conditions of 180 DEG C；
(5) obtained precipitating is first washed with deionized 3 times after reaction, then washs 4 times with dehydrated alcohol, so
Product is placed in 60 DEG C of baking ovens afterwards and is dried, a kind of Bi of novel strip-like structure is obtained5O7Br nano-photocatalyst material.XRD diagram
Spectrum as shown in Figure 1, SEM image as shown in Fig. 2, DRS map as shown in Fig. 3.
Embodiment 2:
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) five water bismuth nitrate (Bi (NO of 2mmol is weighed3)3·5H2O) be dissolved in 30ml dehydrated alcohol, be stirred continuously to
Bismuth nitrate obtains solution A after being completely dissolved；
(2) it weighs 2mmol CTAB and 0.8g polyvinylpyrrolidone to be dissolved in 30ml dehydrated alcohol, after mixing evenly
Obtain solution B；
(3) solution A is added in solution B, obtains solution C after mixing evenly, then the sodium hydroxide solution of 2mol/L is slow
It is added in solution C, adjusts pH=12.91, obtain solution D；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, isothermal reaction is for 24 hours under the conditions of 180 DEG C；
(5) obtained precipitating is first washed with deionized 5 times after reaction, then washs 3 times with dehydrated alcohol, so
Product is placed in 60 DEG C of baking ovens afterwards and is dried, a kind of Bi of novel strip-like structure is obtained5O7Br nano-photocatalyst material.XRD diagram
It composes as shown in fig. 6, SEM image is as shown in fig. 7, Bi5O7Br nano-photocatalyst material banded structure is regular, without obvious impurity thing phase,
Crystalline state is good, purity is high.
Embodiment 3:
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) 2mmol bismuth sulfate (Bi is weighed2(SO4)3) be dissolved in 40ml anhydrous methanol, it is stirred continuously complete to bismuth sulfate
Solution A is obtained after dissolution；
(2) it weighs 2mmol potassium bromide and 1.2g polyvinylpyrrolidone is dissolved in 40ml anhydrous methanol, after mixing evenly
Obtain solution B；
(3) solution A is added in solution B, obtains solution C after mixing evenly, then the potassium hydroxide solution of 1mol/L is slow
It is added in solution C, adjusts pH=13.21, obtain solution D；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, the isothermal reaction 12h under the conditions of 150 DEG C；
(5) obtained precipitating is first washed with deionized 3 times after reaction, then washs 3 times with dehydrated alcohol, so
Product is placed in 60 DEG C of baking ovens afterwards and is dried, a kind of Bi of novel strip-like structure is obtained5O7Br nano-photocatalyst material.XRD diagram
It composes as shown in figure 8, SEM image is as shown in figure 9, Bi5O7Br nano-photocatalyst material banded structure is regular, without obvious impurity thing phase,
Crystalline state is good, purity is high.
Embodiment 4:
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) 2mmol bismuth bromide (BiBr is weighed3) be dissolved in 25ml anhydrous methanol, it is stirred continuously completely molten to bismuth bromide
Solution A is obtained after solution；
(2) it weighs 2mmol potassium bromide and 0.6g polyvinylpyrrolidone is dissolved in 25ml anhydrous methanol, after mixing evenly
Obtain solution B；
(3) solution A is added in solution B, obtains solution C after mixing evenly, then the sodium hydroxide aqueous slkali of 3mol/L is delayed
It is slow to be added in solution C, pH=13.41 is adjusted, solution D is obtained；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, the isothermal reaction 9h under the conditions of 160 DEG C；
(5) obtained precipitating is first washed with deionized 4 times after reaction, then washs 3 times with dehydrated alcohol, so
Product is placed in 60 DEG C of baking ovens afterwards and is dried, a kind of Bi of novel strip-like structure is obtained5O7Br nano-photocatalyst material, XRD diagram
As shown in Figure 10, SEM image is as shown in figure 11, Bi for spectrum5O7Br nano-photocatalyst material banded structure is regular, without obvious impurity thing
Phase, crystalline state is good, purity is high.
Embodiment 5:
A kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) five water bismuth nitrate (Bi (NO of 2mmol is weighed3)3·5H2O) be dissolved in 30ml anhydrous methanol, be stirred continuously to
Bismuth nitrate obtains solution A after being completely dissolved；
(2) it weighs 2mmol bromobenzene and 0.9g polyvinylpyrrolidone is dissolved in 30ml anhydrous methanol, after mixing evenly
Solution B；
(3) solution A is added in solution B, obtains solution C after mixing evenly, the potassium hydroxide solution of 1mol/L is slowly added
Enter in solution C, adjusts pH=12.85, obtain solution D；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, the isothermal reaction 5h under the conditions of 200 DEG C；
(5) obtained precipitating is first washed with deionized 4 times after reaction, then washs 4 times with dehydrated alcohol, so
Product is placed in 60 DEG C of baking ovens afterwards and is dried, a kind of Bi of novel strip-like structure is obtained5O7Br nano-photocatalyst material, XRD diagram
As shown in figure 12, SEM image is as shown in figure 13, Bi for spectrum5O7Br nano-photocatalyst material banded structure is regular, without obvious impurity thing
Phase, crystalline state is good, purity is high.
Embodiment 6:
A kind of Bi of banded structure5O7The application of Br nano-photocatalyst material is used for photo-catalytic degradation of methyl-orange:
Banded structure Bi prepared by 50mg embodiment 1-5 is accurately weighed respectively5O7Br nano-photocatalyst material is added to
50mL concentration is stirring 1h to be protected from light after ultrasonic 10min, so that methyl orange is in Bi in the aqueous solution of the methyl orange of 20mol/L5O7Br
The surface of nano-photocatalyst material reaches adsorption-desorption balance, is then simulated after the optical filtering of 420nm optical filter with 350W xenon lamp
Radiation of visible light carries out photocatalytic degradation experiment, samples 4mL every 10min time interval, obtains after being centrifugated out catalyst
Layer clear liquid, is analyzed at 463nm with concentration of the ultraviolet-uisible spectrophotometer to supernatant liquor.In photocatalytic degradation experiment
The degradation rate of methyl orange=(concentration-residual methyl orange concentration of initial orange) × 100%/initial orange concentration.
As a result Fig. 4 is seen, figure 4, it is seen that the Bi of banded structure under visible light illumination5O7Br nano-photo catalytic material
Expect obvious to methyl orange degradation effect, degradation rate is 93.7% when 50min.
The Bi prepared with embodiment 2,3,4,55O7The basic phase of the degradation effect of Br nano-photocatalyst material and embodiment 1
Together, degradation rate is respectively 92.4%, 92.7%, 91.9%, 93.2% when 50min.
Embodiment 7:
A kind of Bi of banded structure5O7The application of Br nano-photocatalyst material is used for photocatalytic degradation BPA (bisphenol-A):
Banded structure Bi prepared by 50mg embodiment 1-5 is accurately weighed respectively5O7Br nano-photocatalyst material is added to
50mL concentration is 1 h of stirring to be protected from light after ultrasonic 10min, so that BPA is in Bi in the aqueous solution of the BPA of 20mol/L5O7Br nanometers of light
The surface of catalysis material reach adsorption-desorption balance, then with 350 W xenon lamps through 420nm optical filter filter after simulated visible light
Irradiation carries out photocatalytic degradation experiment, samples 4mL every 5min time interval, be centrifugated out after catalyst upper layer is clear
Liquid is analyzed at 275nm with concentration of the ultraviolet-uisible spectrophotometer to supernatant liquor.BPA in photocatalytic degradation experiment
Degradation rate=(concentration of initial BPA-residual BPA concentration) × 100%/initial BPA concentration.
As a result Fig. 5 is seen, from figure 5 it can be seen that the Bi of banded structure under visible light illumination5O7Br nano-photo catalytic material
Expect obvious to BPA degradation effect, degradation rate is 96.1% when 25min.
The Bi prepared with embodiment 2,3,4,55O7The basic phase of the degradation effect of Br nano-photocatalyst material and embodiment 1
Together, degradation rate is respectively 95.1%, 94.8%, 95.7%, 96.0% when 25min.
Claims (5)
1. a kind of Bi of banded structure5O7The preparation method of Br nano-photocatalyst material, its step are as follows:
(1) soluble bismuth salt is dissolved in small-molecular-weight alcohol, small-molecular-weight alcohol ratio used in soluble bismuth salt/step (1) is
2mmol:(25-40) mL is stirred continuously to soluble bismuth salt and is completely dissolved, and obtains solution A；
(2) bromine-containing compound and polyvinylpyrrolidone are dissolved in small-molecular-weight alcohol, make soluble bismuth used in step (1)
Small-molecular-weight alcohol ratio used in salt/bromine-containing compound/polyvinylpyrrolidone/step (2) is 2mmol:2mmol:(0.6-1.2)
G:(25-40) mL obtains solution B after mixing evenly；
The bromine-containing compound is one of cetyl trimethylammonium bromide, potassium bromide and bromobenzene or two to three kinds of is any
Scalemic thereof；
(3) solution A is added in solution B, obtains solution C after mixing evenly, the aqueous slkali of (1-3) mol/L is slowly added to solution C
In, pH=12.5-13.5 is adjusted, solution D is obtained；
(4) solution D is transferred in the reaction kettle of polytetrafluoroethyllining lining, 5-24h is reacted under the conditions of 150-200 DEG C；
(5) obtained precipitating is successively washed with deionized water and dehydrated alcohol after reaction, product is then placed on baking oven
Middle drying obtains the Bi of banded structure5O7Br nano material；
The soluble bismuth salt is one of bismuth nitrate, bismuth bromide and bismuth sulfate or two to three kinds of arbitrary proportion mixture；
The small-molecular-weight alcohol is methanol or ethyl alcohol.
2. the Bi of banded structure according to claim 15O7The preparation method of Br nano-photocatalyst material, it is characterised in that:
The soluble bismuth salt is bismuth nitrate.
3. the Bi of banded structure according to claim 15O7The preparation method of Br nano-photocatalyst material, it is characterised in that:
The small-molecular-weight alcohol is anhydrous methanol.
4. the Bi of banded structure according to claim 15O7The preparation method of Br nano-photocatalyst material, it is characterised in that:
The aqueous slkali is sodium hydroxide solution or potassium hydroxide solution.
5. the Bi of banded structure according to claim 15O7The preparation method of Br nano-photocatalyst material, it is characterised in that:
The aqueous slkali is potassium hydroxide solution.
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| CN107774285A (en) * | 2017-09-05 | 2018-03-09 | 天津大学 | A kind of preparation method and applications of high activity non-stoichiometric BiOBr catalysis materials |
| CN107983372A (en) * | 2017-12-06 | 2018-05-04 | 江南大学 | A kind of preparation method of richness bismuth bismuth oxybromide photocatalyst |
| WO2019178807A1 (en) * | 2018-03-22 | 2019-09-26 | 西南石油大学 | Photocatalyst for removing hydroxypropyl guar gum in backflow fluid of fracturing fluid, preparation method for photocatalyst, and applications thereof |
| CN109569669A (en) * | 2018-11-30 | 2019-04-05 | 长沙学院 | The porous Bi of the spongy monocrystalline of class5O7I nanosheet photocatalyst and preparation method thereof |
| CN109759096B (en) * | 2019-01-21 | 2021-06-29 | 陕西科技大学 | BiOBr nanosphere, preparation method and application of BiOBr nanosphere as photocatalyst in photodegradation of dye |
| CN110180565B (en) * | 2019-05-15 | 2022-04-22 | 太原理工大学 | Photocatalyst Bi5O7Synthetic method of Br and application thereof |
| CN110479336B (en) * | 2019-08-26 | 2022-06-07 | 太原理工大学 | Bi5O7Br/thin layer Ti3C2Preparation method and application of composite photocatalyst |
| CN112588304B (en) * | 2020-12-16 | 2023-04-07 | 江苏大学 | Preparation method of bismuth oxybromide efficient photocatalyst with homogenous crystal face junction |
| CN113998734B (en) * | 2021-11-09 | 2024-01-26 | 淮阴师范学院 | Bi 5 O 7 Preparation method of Br nanosheets |
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