CN107335452A - The method that bismuth oxybromide ultrathin nanometer piece photochemical catalyst is synthesized under room temperature condition - Google Patents
The method that bismuth oxybromide ultrathin nanometer piece photochemical catalyst is synthesized under room temperature condition Download PDFInfo
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- CN107335452A CN107335452A CN201710450252.8A CN201710450252A CN107335452A CN 107335452 A CN107335452 A CN 107335452A CN 201710450252 A CN201710450252 A CN 201710450252A CN 107335452 A CN107335452 A CN 107335452A
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- ultrathin nanometer
- bismuth oxybromide
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- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002608 ionic liquid Substances 0.000 claims abstract description 12
- 125000001246 bromo group Chemical group Br* 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 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 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000015556 catabolic process Effects 0.000 claims abstract description 4
- 238000006731 degradation reaction Methods 0.000 claims abstract description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 8
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 7
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000031709 bromination Effects 0.000 claims description 4
- 238000005893 bromination reaction Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- KYCQOKLOSUBEJK-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;bromide Chemical compound [Br-].CCCCN1C=C[N+](C)=C1 KYCQOKLOSUBEJK-UHFFFAOYSA-M 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- -1 1- octyl group Chemical group 0.000 claims description 2
- JRRNETAQGVDLRW-UHFFFAOYSA-N 1-hexadecyl-3-methyl-2h-imidazole Chemical class CCCCCCCCCCCCCCCCN1CN(C)C=C1 JRRNETAQGVDLRW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004098 Tetracycline Substances 0.000 claims description 2
- 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 claims description 2
- 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 2
- 229940043267 rhodamine b Drugs 0.000 claims description 2
- 229960002180 tetracycline Drugs 0.000 claims description 2
- 229930101283 tetracycline Natural products 0.000 claims description 2
- 235000019364 tetracycline Nutrition 0.000 claims description 2
- 150000003522 tetracyclines Chemical class 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 7
- 229930185605 Bisphenol Natural products 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 23
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000011259 mixed solution Substances 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 238000007704 wet chemistry method Methods 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 4
- 239000005456 alcohol based solvent Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229960003405 ciprofloxacin Drugs 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000009418 renovation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/30—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to wet chemistry to prepare nano metal material field, is related to a kind of visible light-responded bismuth oxybromide ultrathin nanometer sheet material and preparation method.The present invention uses response type bromo ionic liquid and bismuth nitrate as raw material, is reacted in water, in ethanol and acetic acid mixed solution and obtains product.Product is filtered and washs, in atmosphere drying to obtain bismuth oxybromide ultrathin nanometer sheet material.This method is carried out at room temperature, it is not necessary to which extra energy supply, whole building-up process are reacted one hour.The species selection of ionic liquid, ionic liquid dosage, the formation to bismuth oxybromide ultrathin nanometer piece play a key effect.The bismuth oxybromide ultrathin nanometer sheet material thickness of the inventive method synthesis is in 0.7~2nm.The bismuth oxybromide ultrathin nanometer piece photochemical catalyst of design synthesis has splendid photocatalysis property, under radiation of visible light of the wavelength more than 400nm, it is possible to achieve to the efficient degradation of organic pollution.This method synthetic route is simple, and whole technical process is easily controlled.
Description
Technical field
The invention belongs to wet chemistry prepare field of nanometer material technology, be related to bismuth oxybromide ultrathin nanometer piece photochemical catalyst from
It is prepared by sub- liquid auxiliary room temperature.
Background technology
Since graphene is since 2004 are found, due to its unique and tempting physicochemical properties, cause
Great concern.In addition to graphene, the nanostructured of class graphene-like ultra-thin two-dimension (2D) has higher ratio due to it
The surface atom of example, cause extensive concern so as to show the light of novelty, electricity, mechanics and biocompatibility.[4-8]
In view of the special structure of two-dimensional ultrathin nano material and charming property, if structure has visible light-responded band
Wide similar superthin structure, and be used for photocatalysis, its effect are very Worth Expectings.Relative on semiconductor surface side
Photo-generated carrier caused by edge, it may require that longer Time Transmission to semiconductor in photo-generated carrier caused by the inside of semiconductor
Surface, so that can be easily compound in transmittance process.Therefore, the ultrathin of ultrathin nanometer piece can ensure photo-generated carrier
Surface quickly is transferred to from body phase, so as to reduce the compound of electronics and hole.Meanwhile compared to block materials or nanometer
Grain, for ultrathin nanometer piece by with big specific surface area and abundant non-coordination surface atom, this can absorb more visible rays.
Although ultrathin nanometer sheet material can bring excellent photocatalysis performance, but the controllable stripping of stratified material is considered as from block
Material obtains the peculiar mode of ultrathin nanometer piece.And the stripping of block materials is very difficult, peel off on a large scale into uniform
Nanometer sheet is even more then a huge challenge.Therefore, develop a simple bottom-up strategy and carry out direct controllable preparation two dimension
Ultrathin nanometer structure is necessary.
BiOX BiOX (X=Cl, Br and I), one kind have the stratified material of appropriate band structure, have been applied to light
It is catalyzed energy conversion and environmental renovation.It has high chemistry and optical stability, and nontoxic, cost is low, and corrosion-resistant.BiOX
It is by [Bi2O2] layer and intersecting at what double halogen atom layers therein were formed along [001] direction, this special construction assigns it and produced
It is born from and builds internal electrostatic field, so as to ensures its superior photocatalysis performance.Up to the present, the BiOX of various micro/nano structures,
Such as nano wire, [R.S.Yuan, C.Lin, B.C.Wu and X.Z.Fu, Eur.J.Inorg.Chem., 2009,3537-
3540.] nanometer sheet, [J.Jiang, K.Zhao, X.Y.Xiao and L.Z.Zhang, J.Am.Chem.Soc., 2012,134,
4473.] nanobelt, [X.Y.Xiao, J.Jiang, L.Z.Zhang, Applied Catalysis B:Environmental
142-143 (2013) 487-493.] class flower/near-spherical superstructure, [J.Y.Xiong, Z.B.Jiao, G.X.Lu, W.Ren,
J.H.Ye and Y.P.Bi, Chem.-Eur.J., 2013,19,9472-9475.] and hollow superstructure [J.Di, J.X.Xia,
Y.P.Ge,L.Xu,H.Xu,M.Q.He,Q.Zhang and H.M.Li,J.Mater.Chem.A,2014,2,15864-
15874.], successful controllable preparation.And for ultrathin nanometer piece, then it is rarely reported.Xie seminars are in 160 DEG C of solvent heats
Under the conditions of be made BiOCl ultrathin nanometers pieces [M.L.Guan, C.Xiao, J.Zhang, S.J.Fan, R.An, Q.M.Cheng,
J.F.Xie,M.Zhou,B.J.Ye and Y.Xie,J.Am.Chem.Soc.,2013,135,10411.].Leaf et al. is at 250 DEG C
Down by chemical vapor transport route prepare BiOI films (BiOI TF) [L.Q.Ye, J.N.Chen, L.H.Tian, J.Y.Liu,
T.Y.Peng,K.J.Deng and L.Zan,Appl.Catal.,B,2013,130-131,1.].However, currently without in room
The document report and patent report of BiOX ultrathin nanometer pieces are synthesized under the conditions of temperature.In view of high energy in other preparation systems
Consumption, for saving the energy and being easy to industrialized purpose, exploitation is a kind of novel, quickly prepares BiOX at ambient temperature and surpasses
The method of thin nanometer sheet is highly significant.
The content of the invention
To surpass in view of the deficienciess of the prior art, it is an object of the invention to provide a kind of visible light-responded bismuth oxybromide
Thin nanometer sheet material and preparation method, are synthesized using direct precipitation method at room temperature, and specific preparation process is as follows：
(1) bismuth nitrate is used as raw material, in water and the in the mixed solvent wiring solution-forming A of acetic acid；
(2) in another container, bromo ionic liquid is used as raw material, the wiring solution-forming B in alcohol solvent；
(3) under conditions of the solution A obtained by step (1) is in stirring, step (2) resulting solution B is added dropwise to dropwise
In step (1) resulting solution A；Continue to be stirred at room temperature；
(4) after step (3) reaction terminates, product is centrifuged, is washed for several times, dried with deionized water and absolute ethyl alcohol,
Obtain solid powder.
In step (1), in the solution A, the content of bismuth is 0.01-0.2mol/L.
In step (1), the in the mixed solvent of the water and acetic acid, the volume ratio of water and acetic acid is 9:1.
In step (2), described bromo ionic liquid is 1-butyl-3-methylimidazolium bromide, bromination 1- octyl group -3- methyl
Imidazoles or bromination 1- cetyl -3- methylimidazoles.
In step (2), in the solution B, the content of bromine is 0.01-0.6mol/L.
In step (3), the volume ratio of the solution A and solution B is 1:1.
In step (3), the time being stirred at room temperature is 5-120 minutes.
In step (4), the drying temperature is 50 DEG C, drying time 5-24h.
A kind of visible light-responded bismuth oxybromide ultrathin nanometer sheet material that the present invention obtains, is independent sheet, thickness
For 0.7-2nm.
The bismuth oxybromide ultrathin nanometer sheet material of gained of the invention has visible light-responded photocatalysis performance, big in wavelength
Under 400nm radiation of visible light, it is possible to achieve to the efficient degradation of all kinds of organic pollutions, for rhodamine B degradation, bis-phenol
A, Ciprofloxacin or tetracycline.
Beneficial effects of the present invention are：
(1) present invention is using response type ionic liquid as reaction source, the bismuth oxybromide ultrathin nanometer sheet material thickness of thin of synthesis,
It is pure
Degree is high, good dispersion.
(2) the bismuth oxybromide ultrathin nanometer sheet material that synthesis obtains has very high photocatalytic activity, can be to various rings
Border pollutant, especially Ciprofloxacin are efficiently degraded.
(3) whole building-up process is carried out at ambient temperature, it is not necessary to rear heat treatment, saves the energy, generated time is short, has
Beneficial to extensive synthesis.
Brief description of the drawings
X-ray diffraction (XRD) figure of Fig. 1 bismuth oxybromide ultrathin nanometer pieces.It will be seen from figure 1 that the spy of prepared sample
Levy peak it is consistent with standard card (JCPDS card NO.73-2061), 2 θ be 11.2 °, 21.8 °, 25.2 °, 31.8 °,
33.3 °, 39.5 °, 44.8 °, 46.4 °, 50.7 °, 53.4 °, 56.4 °, 57.2 °, 61.9 °, 69.6 °, 71.1 °, 74.4 ° and
78.9 ° correspond respectively to (001), (002), (011), (012), (110), (112), (004), (020), (014), (211)
(114), (212), (015), (006), (124), (032) and (116) crystal face.Gained sample is pure bismuth oxybromide material.
The atomic force microscopy diagram of Fig. 2 bismuth oxybromide ultrathin nanometer pieces.From figure 2 it can be seen that gained bismuth oxybromide surpasses
The thickness of thin nanometer sheet is about 1nm, and material thickness is homogeneous.
The scanning electron microscope (SEM) photograph of Fig. 3 bismuth oxybromide ultrathin nanometer pieces.From figure 3, it can be seen that gained bismuth oxybromide material is
Dimensional thinlayer structure, and pattern is homogeneous.
The transmission electron microscope picture of Fig. 4 bismuth oxybromide ultrathin nanometer pieces.Figure 4, it is seen that gained bismuth oxybromide material is
Thin layer nanometer sheet.
Embodiment：
Embodiment 1
The step of photochemical catalyst BiOBr ultrathin nanometer pieces are prepared as bromine source using 1-butyl-3-methylimidazolium bromide：
Bismuth nitrate is used as raw material, in 10mL water and acetic acid (volume ratio 9:1) in the mixed solvent is made into solution A,
Wherein the content of bismuth is 0.01-0.2mol/L, in another container, bromo ionic liquid is used as raw material, in 10mL ethanol
B solution is made into solvent, the wherein content of bromine is 0.01-0.6mol/L, solution A be in stirring under conditions of, by B solution by
It is added dropwise in solution A, gained mixed solution is continued 5-120 minutes are stirred at room temperature, product centrifuged, with deionized water and nothing
Water-ethanol is washed for several times, and 5-24h is dried at 50 DEG C and obtains solid powder.
Embodiment 2
Bismuth nitrate is used as raw material, in 10mL water and acetic acid (volume ratio 9:1) in the mixed solvent is made into solution A,
Wherein the content of bismuth is 0.01mol/L, in another container, bromo ionic liquid is used as raw material, in 10mL alcohol solvents
In be made into B solution, the wherein content of bromine is 0.05mol/L, solution A be in stirring under conditions of, B solution is added dropwise to dropwise
In solution A, gained mixed solution is continued to be stirred at room temperature 5 minutes, product is centrifuged, number is washed with deionized water and absolute ethyl alcohol
Secondary, dry 5h obtains solid powder at 50 DEG C.
Embodiment 3
Bismuth nitrate is used as raw material, in 10mL water and acetic acid (volume ratio 9:1) in the mixed solvent is made into solution A,
Wherein the content of bismuth is 0.1mol/L, in another container, bromo ionic liquid is used as raw material, in 10mL alcohol solvents
B solution is made into, the wherein content of bromine is 0.3mol/L, and under conditions of solution A is in stirring, it is molten that B solution is added dropwise to A dropwise
In liquid, gained mixed solution is continued to be stirred at room temperature 60 minutes, product is centrifuged, number is washed with deionized water and absolute ethyl alcohol
Secondary, dry 10h obtains solid powder at 50 DEG C.
Embodiment 4
Bismuth nitrate is used as raw material, in 10mL water and acetic acid (volume ratio 9:1) in the mixed solvent is made into solution A,
Wherein the content of bismuth is 0.2mol/L, in another container, bromo ionic liquid is used as raw material, in 10mL alcohol solvents
B solution is made into, the wherein content of bromine is 0.6mol/L, and under conditions of solution A is in stirring, it is molten that B solution is added dropwise to A dropwise
In liquid, gained mixed solution is continued to be stirred at room temperature 120 minutes, product is centrifuged, number is washed with deionized water and absolute ethyl alcohol
Secondary, dry 24h obtains solid powder at 50 DEG C.
Fig. 1 is X-ray diffraction (XRD) figure of bismuth oxybromide ultrathin nanometer piece, it will be seen from figure 1 that prepared sample
Characteristic peak is consistent with standard card (JCPDS card NO.73-2061), 2 θ be 11.2 °, 21.8 °, 25.2 °, 31.8 °,
33.3 °, 39.5 °, 44.8 °, 46.4 °, 50.7 °, 53.4 °, 56.4 °, 57.2 °, 61.9 °, 69.6 °, 71.1 °, 74.4 ° and
78.9 ° correspond respectively to (001), (002), (011), (012), (110), (112), (004), (020), (014), (211)
(114), (212), (015), (006), (124), (032) and (116) crystal face.Gained sample is pure bismuth oxybromide material.
Fig. 2 is the atomic force microscopy diagram of bismuth oxybromide ultrathin nanometer piece, from figure 2 it can be seen that gained bismuth oxybromide
The thickness of ultrathin nanometer piece is about 1nm, and material thickness is homogeneous.
Fig. 3 is the scanning electron microscope (SEM) photograph of bismuth oxybromide ultrathin nanometer piece, from figure 3, it can be seen that gained bismuth oxybromide material
For dimensional thinlayer structure, and pattern is homogeneous.
Fig. 4 is the transmission electron microscope picture of bismuth oxybromide ultrathin nanometer piece, figure 4, it is seen that gained bismuth oxybromide material
For thin layer nanometer sheet.
Claims (10)
1. the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst is synthesized under room temperature condition, it is characterised in that comprise the following steps：
(1) bismuth nitrate is used as raw material, in water and the in the mixed solvent wiring solution-forming A of acetic acid；
(2) in another container, bromo ionic liquid is used as raw material, the wiring solution-forming B in alcohol solvent；
(3) under conditions of the solution A obtained by step (1) is in stirring, step (2) resulting solution B is added dropwise to step dropwise
(1) in resulting solution A；Continue to be stirred at room temperature；
(4) after step (3) reaction terminates, product is centrifuged, is washed for several times with deionized water and absolute ethyl alcohol, is dried, obtain
Solid powder.
2. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (1), in the solution A, the content of bismuth is 0.01-0.2mol/L.
3. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (1), the in the mixed solvent of the water and acetic acid, the volume ratio of water and acetic acid is 9:1.
4. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (2), described bromo ionic liquid is 1-butyl-3-methylimidazolium bromide, bromination 1- octyl group -3- methyl
Imidazoles or bromination 1- cetyl -3- methylimidazoles.
5. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (2), in the solution B, the content of bromine is 0.01-0.6mol/L.
6. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (3), the volume ratio of the solution A and solution B is 1:1.
7. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (3), the time being stirred at room temperature is 5-120 minutes.
8. synthesizing the method for bismuth oxybromide ultrathin nanometer piece photochemical catalyst under room temperature condition according to claim 1, it is special
Sign is, in step (4), the drying temperature is 50 DEG C, drying time 5-24h.
9. a kind of bismuth oxybromide ultrathin nanometer piece photochemical catalyst, it is characterised in that be by synthesis side claim 1~8 described
It is independent sheet made from method, nanometer sheet thickness 0.7-2nm.
10. by the bismuth oxybromide ultrathin nanometer piece photochemical catalyst described in claim 9, for rhodamine B degradation, bis-phenol a, ring third
The purposes of husky star or tetracycline.
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