CN104226339A - Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof - Google Patents
Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 11
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 11
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000003054 catalyst Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 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 claims description 10
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000010335 hydrothermal treatment Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 206010013786 Dry skin Diseases 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000003828 vacuum filtration Methods 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 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 3
- 229940012189 methyl orange Drugs 0.000 abstract description 3
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 230000000694 effects Effects 0.000 description 6
- 230000000593 degrading effect Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000001055 reflectance spectroscopy Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- -1 sodium halide Chemical class 0.000 description 3
- SRUWWOSWHXIIIA-UKPGNTDSSA-N Cyanoginosin Chemical compound N1C(=O)[C@H](CCCN=C(N)N)NC(=O)[C@@H](C)[C@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@H](C(O)=O)N(C)C(=O)[C@@H](C)[C@@H]1\C=C\C(\C)=C\[C@H](C)[C@@H](O)CC1=CC=CC=C1 SRUWWOSWHXIIIA-UKPGNTDSSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 108010067094 microcystin Proteins 0.000 description 2
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QKXCAKZMAORNSR-UHFFFAOYSA-N azane 1-chlorohexadecane Chemical compound N.CCCCCCCCCCCCCCCCCl QKXCAKZMAORNSR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 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 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachlorophenol Chemical compound OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Inorganic materials [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- UKHVLWKBNNSRRR-UHFFFAOYSA-M quaternium-15 Chemical compound [Cl-].C1N(C2)CN3CN2C[N+]1(CC=CCl)C3 UKHVLWKBNNSRRR-UHFFFAOYSA-M 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
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- Catalysts (AREA)
Abstract
The invention discloses a visible-light-induced photocatalyst Bi4O5Br2 and a preparation method thereof. According to the visible-light-induced photocatalyst Bi4O5Br2 and the preparation method thereof, an improved low-temperature hydrothermal method is adopted, composition of Bi, O and Br in BiOX is controlled by controlling amount of a bismuth source and a bromine source, and a novel layered-cake-shaped visible-light-induced photocatalyst Bi4O5Br2 is prepared successfully. The preparation method is simple in production process, easy to operate, low in synthesis temperature, high in reaction yield, environment-friendly and low in cost and meets the requirement of actual production, the reaction yield is 92%, and raw materials are easy to obtain. The visible-light-induced photocatalyst has good visible-light catalytic activity, can completely degrade various organic pollutants such as rhodamine b, methyl orange and methylene blue in short time under the visible light irradiation, is small in light corrosion and good in reusability, can be applied to industrial production and particularly has a better application value in organic pollutant degradation through solar photocatalysis, and the market potential is large.
Description
Technical field
The invention belongs to photocatalysis and material chemistry technical field, particularly relate to a kind of visible light catalyst Bi
4o
5br
2and preparation method thereof.
Background technology
Due to the potential application power in solar energy conversion and the depollution of environment etc., conductor photocatalysis two ten years in the past become one of academic research focus.Among various catalysis material, nano-TiO
2due to have strong oxidability, at a low price, nontoxic, biological and chemical inertia, and the characteristic such as long-term light and thermally stable and obtain maximum concerns and research.But, due to TiO
2be wide bandgap semiconductor, response can only be produced to the UV-irradiation of λ <380nm, this severely limits its practical application under sunshine or indoor light environment, because these radiation of light source are based on visible ray.Therefore, find, design and synthesize and new there is the research emphasis that visible light-responded and efficient photochemical catalyst is current photocatalysis field.
Because BiOX BiOX (X=Cl, Br, I) has special structure, the separation for photo-generate electron-hole is highly beneficial, therefore, it is possible to obtain high photocatalysis efficiency.Highly active BiOX compound photochemical catalyst can be obtained by the design and synthesis of crystal structure and band structure.Chinese patent " a kind of preparation method of bismuth oxybromide photocatalyst " (patent No. 201010141878.9 publication date 2010-07-28) utilizes bismuth nitrate and bromide sixteen alkyls pyridine to be raw material, BiOBr visible light catalyst has been prepared under hydro-thermal method condition, under radiation of visible light, all there is good degrading activity to dyeing waste water and Microcystin.Chinese patent application " a kind of preparation method possessing the BiOX photocatalyst of photocatalytic activity " (number of patent application 201210136733.9 publication date 2012-09-19) adopts pyridines cationic surfactant and sodium halide to be that BiOCl, BiOBr, BiOI tri-kinds of visible light catalysts prepared by raw material, and its Microcystin all has good degradation.The polyoxy halogenation oxygen bismuth complex compound of homoatomic composition (Bi, O, X) does not have superior visible light catalysis activity yet, causes interest and the concern of numerous researcher.Chinese patent " visible-light photocatalyst Bi
12o
17cl
2and preparation method thereof " (patent No. 201110444323.6 publication date 2012-07-11) have employed inorganic salts potassium chloride and substitute cetyl chloride ammonium (CTAC) as chlorine source, by the efficient visible light catalyst B i regulating the pH value of reaction solution to synthesize a kind of brand-new metering ratio
12o
17c
l2, this catalyst to pollutant pentachlorophenol (PCP) close to 100% degraded.Chinese patent application " visible light catalyst Bi
3o
4br and preparation method thereof " (number of patent application 201110435787.0 publication date 2012-07-11) utilize bismuth salt and quaternary ammonium salt to be raw material, and take hydrothermal reaction at low temperature to control not homoatomic metering ratio in oxyhalogen bismuth, prepare novel visible catalyst Bi
3o
4br, this catalyst has better degradation to rhodamine B.Chinese patent application " visible light catalyst Bi
5o
7br and preparation method thereof." (number of patent application 201410029932 publication date 2014-04-30) utilize bismuth source and bromine source to be raw material, take hydrothermal reaction at low temperature to control not homoatomic metering ratio in oxyhalogen bismuth, prepared and had by Bi
5o
7the cross star structure of Br micron film composition, this catalyst all has fine degradation to rhodamine B, methyl orange.Usually, the photocatalytic activity of conductor oxidate not only determined by its chemical composition, is also subject to the impact of the attributes such as its pattern, size and configuration simultaneously.As crystal structure and band structure, degree of crystallinity, crystallite dimension, specific area and pore structure etc.
Summary of the invention
The technical problem to be solved in the present invention is to provide the excellent visible light catalyst Bi of a kind of novel in shape, photocatalysis performance
4o
5br
2and preparation method thereof.
For solving the problems of the technologies described above, the present invention by the following technical solutions: visible light catalyst Bi
4o
5br
2, have by Bi
4o
5br
2the layer cake shape structure of micron film composition.
Layer cake shape physical dimension is at 2 ~ 5 microns.
Above-mentioned visible light catalyst Bi
4o
5br
2, under visible light illumination, in 15 minutes, rhodamine B 100% is degraded, and reuses 5 catalytic activitys without obvious reduction.
Above-mentioned visible light catalyst Bi
4o
5br
2preparation method, comprise the following steps:
The bismuth source that <1> takes 1.5 ~ 3.5 grams is dissolved in the concentrated acid of 1.0 ~ 3.0mL, is diluted with water to 8 ~ 15mL, stirs;
The bromine source that <2> takes 0.5 ~ 1.5 gram is dissolved in the deionized water of 10 ~ 20mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 4.0 ~ 9.0 by 1 ~ 3mol/L aqueous slkali adjust ph, stir 10 ~ 40min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 30 ~ 40mL, then carry out hydrothermal treatment consists, treatment temperature is 120 ~ 180 DEG C, constant temperature 18 ~ 36 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 50 ~ 80 DEG C of dryings 10 ~ 24 hours, faint yellow Bi is obtained
4o
5br
2pressed powder.
Bismuth source is five water bismuth nitrates, and concentrated acid is red fuming nitric acid (RFNA), and bromine source is softex kw, and aqueous slkali is sodium hydroxide solution.
Five water bismuth nitrates are 2.4 grams, and softex kw is 0.75 gram, and sodium hydroxide solution is 2mol/L.
Regulate reacting liquid pH value to be 5.0 in step <3>, hydrothermal treatment consists temperature is 160 DEG C, constant temperature 24 hours.
In step <4>, baking temperature is 80 DEG C, and drying time is 12 hours.
Inventor adopts improvement hydrothermal reaction at low temperature, by control bismuth source, bromine source consumption and change preparation condition and control the composition of Bi, O, Br in oxyhalogen bismuth, successfully prepare the Bi with layer cake shape structure
4o
5br
2novel visible catalyst, thus the photocatalysis performance that effectively improve catalyst.Bismuth source and bromine source are specifically dissolved in acidic aqueous solution by this method, adjust ph to certain limit, then by after hydrothermal synthesis method process.Preparation method's reaction of the present invention is carried out at low temperatures, without any need for heat treatment subsequent step, whole production technology is simple, processing ease, synthesis temperature are low, reaction yield is high (92%), and environmental friendliness, raw material be easy to get, with low cost, the needs of realistic production.That visible light catalyst system of the present invention does not adulterate, single-phase bismuth oxybromide, there is good visible light catalysis activity, under visible light illumination, can carry out degradable to Some Organic Pollutants (rhodamine B, methyl orange, methylene blue) in short time, material is easy to reclaim, and after repeatedly using, its stuctures and properties is substantially constant, there is good actual application value, for large-scale production visible light catalyst provides an effective approach.
Accompanying drawing explanation
Fig. 1 is Bi prepared by the present invention
4o
5br
2xRD collection of illustrative plates, this collection of illustrative plates correspond to Bi
4o
5br
2meet standard card JCPDS No.37-0699.
Fig. 2 is Bi prepared by the present invention
4o
5br
2sEM figure.
Fig. 3 is Bi prepared by the present invention
4o
5br
2uV Diffuse Reflectance Spectroscopy.
Fig. 4 is the Bi that under radiation of visible light prepared by the present invention
4o
5br
2for the degradation curve of rhodamine B.
Fig. 5 is Bi prepared by the present invention
4o
5br
2the ultraviolet-visible spectrum of rhodamine B solution curve map over time in photocatalytic process.
Fig. 6 recycles Bi prepared by the present invention
4o
5br
2during powder visible light photocatalytic degradation rhodamine B, degradation rate is with the change curve recycling number of times.
Detailed description of the invention
Embodiment 1
The five water bismuth nitrates that <1> takes 2.0 grams are dissolved in the red fuming nitric acid (RFNA) of 1.5mL, add a small amount of water and are diluted to 10mL, stir;
The softex kw that <2> takes 0.5 gram is dissolved in the deionized water of 10mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 5.0 by 2mol/L sodium hydroxide solution adjust ph, stir 30min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 40mL, then carry out hydrothermal treatment consists, treatment temperature is 160 DEG C, constant temperature 24 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 80 DEG C of dryings 10 hours, obtains faint yellow Bi
4o
5br
2pressed powder.
Embodiment 2
The five water bismuth nitrates that <1> takes 2.4 grams are dissolved in the red fuming nitric acid (RFNA) of 1.5mL, add a small amount of water and are diluted to 10mL, stir;
The softex kw that <2> takes 0.75 gram is dissolved in the deionized water of 10mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 5.0 by 2mol/L sodium hydroxide solution adjust ph, stir 30min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 40mL, then carry out hydrothermal treatment consists, treatment temperature is 160 DEG C, constant temperature 24 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 80 DEG C of dryings 24 hours, obtains faint yellow Bi
4o
5br
2pressed powder.
Embodiment 3
The five water bismuth nitrates that <1> takes 1.5 grams are dissolved in the red fuming nitric acid (RFNA) of 1.0mL, add a small amount of water and are diluted to 10mL, stir;
The softex kw that <2> takes 1.0 grams is dissolved in the deionized water of 15mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 6.0 by 2mol/L sodium hydroxide solution adjust ph, stir 40min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 40mL, then carry out hydrothermal treatment consists, treatment temperature is 160 DEG C, constant temperature 28 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 60 DEG C of dryings 12 hours, obtains faint yellow Bi
4o
5br
2pressed powder.
Embodiment 4
The five water bismuth nitrates that <1> takes 3.0 grams are dissolved in the red fuming nitric acid (RFNA) of 2.0mL, add a small amount of water and are diluted to 15mL, stir;
The softex kw that <2> takes 1.0 grams is dissolved in the deionized water of 15mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 7.0 by 2mol/L sodium hydroxide solution adjust ph, stir 30min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 40mL, then carry out hydrothermal treatment consists, treatment temperature is 150 DEG C, constant temperature 30 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 70 DEG C of dryings 20 hours, obtains faint yellow Bi
4o
5br
2pressed powder.
Embodiment 5
The five water bismuth nitrates that <1> takes 2.4 grams are dissolved in the red fuming nitric acid (RFNA) of 1.5mL, add a small amount of water and are diluted to 10mL, stir;
The softex kw that <2> takes 1.5 grams is dissolved in the deionized water of 15mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 5.0 by 2mol/L sodium hydroxide solution adjust ph, stir 40min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 40mL, then carry out hydrothermal treatment consists, treatment temperature is 180 DEG C, constant temperature 20 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 80 DEG C of dryings 12 hours, obtains faint yellow Bi
4o
5br
2pressed powder.
By embodiment 1 to 5 gained Bi
4o
5br
2carry out XRD, SEM, UV Diffuse Reflectance Spectroscopy detects and rhodamine B Degrading experiment, the results are shown in Figure 1 to 6 (because same detection or result of the test are similar to, therefore only choosing representative diagram to illustrate).
As shown in Figure 2, SEM detects and shows Bi of the present invention
4o
5br
2have the layer cake shape structure be made up of micron film, size is at 2 ~ 5 microns.
As shown in Figure 3, UV Diffuse Reflectance Spectroscopy detects and shows, Bi of the present invention
4o
5br
2from ultraviolet region to visible region, have certain absorption, and absorption maximum edge is in 486 nanometers, its forbidden band is wide is 2.55eV, than BiOBr (other conditions and preparation Bi
4o
5br
2identical, to prepare under pH=1.0 condition) forbidden band wide (2.75) eV little, be more conducive to the utilization of visible ray.
Use Bi of the present invention
4o
5br
2under visible light illumination Degrading experiment is carried out to rhodamine B, result as shown in Figs. 4-6, Bi of the present invention
4o
5br
2there is better Visible Light Induced Photocatalytic compared with Degussa (P25), BiOBr active, under visible light illumination, can realize in 15 minutes degrading to pollutant 100%; When recycling 5 times, Bi
4o
5br
2visible light catalysis activity kept stable.
In addition, inventor is also by embodiment 1 to 5 gained Bi
4o
5br
2carried out acidic methylene orange, methylene blue Degrading experiment, under visible light illumination, in 15 minutes, same realization is degraded to pollutant 100%; Comparative test shows, the BiOBr of sheet prepared by hydro-thermal method, and 15 minutes is about 92% to the degradation effect of acidic methylene orange solution, is about 88% to the degradation effect of methylene solution.
Claims (8)
1. a visible light catalyst Bi
4o
5br
2, it is characterized in that having by Bi
4o
5br
2the layer cake shape structure of micron film composition.
2. visible light catalyst Bi according to claim 1
4o
5br
2, it is characterized in that: described layer cake shape physical dimension is at 2 ~ 5 microns.
3. visible light catalyst Bi according to claim 2
4o
5br
2, it is characterized in that: under visible light illumination, in 15 minutes, rhodamine B 100% degraded.
4. visible light catalyst Bi according to claim 1
4o
5br
2preparation method, it is characterized in that comprising the following steps:
The bismuth source that <1> takes 1.5 ~ 3.5 grams is dissolved in the concentrated acid of 1.0 ~ 3.0mL, is diluted with water to 8 ~ 15mL, stirs;
The bromine source that <2> takes 0.5 ~ 1.5 gram is dissolved in the deionized water of 10 ~ 20mL, stirs;
The solution that step <2> obtains by <3> slowly joins in the solution that step <1> obtains, be 4.0 ~ 9.0 by 1 ~ 3mol/L aqueous slkali adjust ph, stir 10 ~ 40min; Mixture being transferred to 50mL has in teflon-lined stainless steel water heating kettle, and control liquor capacity 30 ~ 40mL, then carry out hydrothermal treatment consists, treatment temperature is 120 ~ 180 DEG C, constant temperature 18 ~ 36 hours;
<4> is after step <3> terminates, vacuum filtration separating solids product, gained solid matter with deionized water and absolute ethyl alcohol are washed respectively to neutrality, then 50 ~ 80 DEG C of dryings 10 ~ 24 hours, faint yellow Bi is obtained
4o
5br
2pressed powder.
5. preparation method according to claim 4, is characterized in that: described bismuth source is five water bismuth nitrates, and concentrated acid is red fuming nitric acid (RFNA), and bromine source is softex kw, and aqueous slkali is sodium hydroxide solution.
6. preparation method according to claim 5, is characterized in that: described five water bismuth nitrates are 2.4 grams, and softex kw is 0.75 gram, and sodium hydroxide solution is 2mol/L.
7. preparation method according to claim 6, is characterized in that: regulate reacting liquid pH value to be 5.0 in step <3>, hydrothermal treatment consists temperature is 160 DEG C, constant temperature 24 hours.
8. preparation method according to claim 7, is characterized in that: in step <4>, baking temperature is 80 DEG C, and drying time is 12 hours.
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