CN107952455A - It is a kind of with the three-dimensional sheet BiOI catalysis materials of macroscopic frame and its preparation and application - Google Patents
It is a kind of with the three-dimensional sheet BiOI catalysis materials of macroscopic frame and its preparation and application Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- UOZDOLIXBYLRAC-UHFFFAOYSA-L [2-hydroxy-3-(trimethylazaniumyl)propyl]-trimethylazanium;diiodide Chemical compound [I-].[I-].C[N+](C)(C)CC(O)C[N+](C)(C)C UOZDOLIXBYLRAC-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 11
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 239000000975 dye Substances 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 5
- 239000012265 solid product Substances 0.000 claims abstract description 5
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 8
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 2
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 2
- 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 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- LGPJVNLAZILZGQ-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;iodide Chemical compound [I-].CCCCCCCCCCCCCCCC[N+](C)(C)C LGPJVNLAZILZGQ-UHFFFAOYSA-M 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 claims 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims 1
- 230000006872 improvement Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 10
- 238000011068 loading method Methods 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 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 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003760 hair shine Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000258 photobiological effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J27/08—Halides
-
- 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—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
Mainly include with the three-dimensional sheet BiOI catalysis materials of macroscopic frame and its preparation and application, preparation the present invention relates to a kind of（1）Under conditions of 26 ~ 28 DEG C, structure directing agent polyvinylpyrrolidone and bismuth source are dissolved in organic solvent；Propiodal is added with vigorous stirring, continues 10 ~ 60 min of stirring；（2）By step（1）Gained settled solution is transferred in stainless steel autoclave, and organic solvent adjustment amount of fill is 60% ~ 80%, 140 ~ 180 DEG C, carries out 9 ~ 24 h of crystallization；（3）It is cooled to room temperature, filters to obtain solid product, fully washing is carried out to product after 50 ~ 90 DEG C, dry 8 ~ 24 h.The three-dimensional sheet BiOI catalysis materials with macroscopic frame being prepared can form the catalysis material of heterojunction structure as the photochemical catalyst and catalyst carrier of the degraded of organic dyestuff, carried noble metal etc..The micron-sized three-dimensional sheet structure BiOI with good crystallinity of the present invention, it is conducive to the improvement of activity and the raising of mass transfer rate with larger surface area and porosity.
Description
Technical field
The present invention relates to nano-photocatalyst material preparation, more particularly to a kind of three-dimensional sheet BiOI light with macroscopic frame
Catalysis material and its preparation and application.
Background technology
BiOI indirect band-gap semiconductors, have unique internal electric field and suitable energy gap（1.7-1.92 eV）,
There is good response to the light of 690 nm, be a kind of emerging visible-light photocatalysis material.Research shows particle diameter, the shape of BiOI
Looks and structure have its photocatalysis performance significant impact, therefore the preparation method and application research of BiOI causes domestic foreign object
The great interest of reason, chemistry and material science worker.
[Zhai C, Hu J, Sun M, et al. Two dimensional visible-light-active Pt-
BiOI photoelectrocatalyst for efficient ethanol oxidation reaction in
Alkaline media [J] Applied Surface Science, 2017.] report a kind of two-dimensional nano piece BiOI
（nanoplates）Preparation method, and have studied its photocatalytic activity.
[Wang Y, Lin L, Li F, et al. Enhanced photocatalytic bacteriostatic
activity towards Escherichia coli using 3D hierarchical microsphere BiOI/
BiOBr under visible light irradiation[J]. Photochemical & Photobiological
Sciences, 2016, 15(5):666-672.] a kind of synthetic method of three-dimensional multistage structure microspheres is reported, synthesis
Multilevel hierarchy microballoon shows excellent bacteriostasis under visible light.
At present, prepared in BiOI materials is with " bottleneck " problem run into practical application：The two-dimensional nano piece of synthesis
Shape BiOI easily accumulates, and causes exposed external surface area small, has seriously affected its catalytic performance, be unfavorable for practical application.Cause
This, is integrated into the functional form catalysis material with macroscopic frame with important scientific meaning and practical valency by BiOI nanometer sheets
Value.
The content of the invention
For problems of the prior art, it is an object of the invention to provide a kind of three-dimensional plate with macroscopic frame
Shape BiOI catalysis materials and its preparation and application.
A kind of preparation method of the three-dimensional sheet BiOI catalysis materials with macroscopic frame, mainly includes the following steps that：
（1）Under conditions of 26 ~ 28 DEG C, structure directing agent polyvinylpyrrolidone and bismuth source are dissolved in organic solvent；
Lower addition propiodal is vigorously stirred, continues 10 ~ 60 min of stirring；
（2）By step（1）Gained settled solution is transferred in stainless steel autoclave, organic solvent adjustment amount of fill for 60% ~
80%, 140 ~ 180 DEG C, carry out 9 ~ 24 h of crystallization；
（3）It is cooled to room temperature, filters to obtain solid product, fully washing is carried out to product after 50 ~ 90 DEG C, dry 8 ~ 24 h.
The organic solvent of the present invention in addition to as solvent, since the large viscosity of organic solvent, polarity are small, may be used also in the reaction
Effectively to reduce the diffusion velocity of reaction species, regulate and control the growth of crystal, so as to regulate and control appearance structure.The present invention has by control
Solvent additive amount regulates and controls pressure in kettle to change loadings, influences the degree of super saturation of mother liquor.Solution loading is different in kettle,
It is bound to cause the change of top gaseous phase volume.In high reaction temperatures, the partial pressure of gas reactor, gas phase composition will be with first
The difference of beginning loading and change, so as to cause the change of mother liquor constituents ratio, its result can produce crystal growing process
Raw serious influence, causes the crystal of synthesis to have different structure and pattern.In general, in the solvent less than critical-temperature
In thermal response, identical initial concentration, different initial compactednesses correspond to different vapor-liquid equilibrium lines, thus loading it is identical,
Reaction kettle capacity is different；Reaction kettle capacity is identical, and loading is different, and the pattern, structure to the material of synthesis can produce directly
Influence.
The structure directing agent of the present invention is polyvinylpyrrolidone PVP（K-30）, it is a kind of there is amphipathic nonionic
Polymer, can be stably dispersed in the nano-particle of polar solvent as surfactant, can also be used as capping reagent control synthesis
The size and shape of nano-particle.In the present invention, PVP is optionally adsorbed on some faces of BiOI, it is suppressed that these faces
Growth, can regulate and control sample pattern, control nanometer sheet thickness and spacing.
Formation of the selection of temperature and time equally to structure produces large effect in the present invention.
Further, the bismuth source, the molar ratio of propiodal are 1：0.5~2.
Further, the stainless steel autoclave liner is polytetrafluoroethylene (PTFE), capacity 250mL；Described has
Total dosage of solvent is 150 ~ 200 mL.
Further, the bismuth source includes the one or more in five nitric hydrate bismuths, bismuthyl carbonate, bismuth sulfate；
The organic reagent includes the one or more in ethylene glycol, glycol monoethyl ether, glycerine；The propiodal includes iodine
Change the one or more in potassium, sodium iodide, cetyl trimethyl ammonium iodide.
Further, step（1）The mixing speed is 350 ~ 600 r/min.
Further, step（3）The washing is first to be washed for several times with absolute ethyl alcohol, then number is washed with deionized
It is secondary.
Three-dimensional sheet BiOI catalysis materials with macroscopic frame prepared by above-mentioned preparation method.
The application of the above-mentioned three-dimensional sheet BiOI catalysis materials with macroscopic frame, the light as the degraded of organic dyestuff
Catalyst.Show good organic dyestuff the disposal efficiency.The light degradation for mainly acting on the organic dyestuff such as rhodamine B is anti-
Should.Can also catalyst carrier, carried noble metal etc. formed heterojunction structure catalysis material.
Compared with prior art, the present invention uses simple solvent-thermal method, by controlling organic solvent additive amount to change
Pressure in loadings regulation and control kettle, influences the degree of super saturation of mother liquor, and the selection of integrated structure directed agents and its reaction temperature and
The reasonable control of time, prepares a kind of micron-sized three-dimensional sheet structure BiOI with good crystallinity, it is with larger
Surface area and porosity, be conducive to activity improvement and mass transfer rate raising.The material is in the organic dyestuff light such as rhodamine B
Good performance is shown in degraded, while the light that can be also used as catalyst carrier, carried noble metal etc. to form heterojunction structure is urged
Change material.In addition preparation method synthetic route of the invention is convenient, simple efficient, will not introduce the thing polluted to environment
Matter, it is environmentally protective.
Brief description of the drawings
Fig. 1 is that the x-ray powder of the three-dimensional sheet BiOI catalysis materials with macroscopic frame prepared by embodiment 1 spreads out
Penetrate figure；
Fig. 2 is the scanning electron microscope (SEM) photograph of the three-dimensional sheet BiOI catalysis materials with macroscopic frame prepared by embodiment 1；
Fig. 3 is the photocatalytic degradation of the three-dimensional sheet BiOI catalysis materials with macroscopic frame prepared by embodiment 1；
Fig. 4 is the X-ray powder diffraction figure of spherical BiOI prepared by embodiment 4；
Fig. 5 is the scanning electron microscope (SEM) photograph of spherical BiOI prepared by embodiment 4；
Fig. 6 is the X-ray powder diffraction figure of the spherical BiOI of groove prepared by embodiment 5；
Fig. 7 is the scanning electron microscope (SEM) photograph of the spherical BiOI of groove prepared by embodiment 5.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
It is described in detail on step ground.
Embodiment 1
Under room temperature, magnetic agitation（350~600 r/s）, by 3.395 g, five nitric hydrate bismuths（Bi(NO3)2·5H2O）With 0.375
G polyvinylpyrrolidones（K-30）It is dissolved in 150 mL ethylene glycol.Add 1.162 g potassium iodide（KI）, persistently stir 30 min.
Above-mentioned solution is transferred in the autoclave of 250 mL, adding 50 mL ethylene glycol makes loadings reach 80%, is put into 160 DEG C
12 h are kept in baking oven.Natural cooling, filtering, is washed three times, obtained solid sample is 70 respectively with ethanol, deionized water successively
DEG C, dry 12 h.
The XRD spectras of the three-dimensional sheet BiOI catalysis materials for the macroscopic frame being prepared as shown in Figure 1,10.34 °,
29.4 °, 31.4 °, 45.1 °, and 55.0 ° of (001) for not corresponding to BiOI crystal, (102), (110), (104), (212) crystal face, spreads out
Penetrate that peak is sharp and intensity is high, represent that the particle diameter of synthesized BiOI crystal is big, crystallinity is higher.From the three-dimensional sheet of macroscopic frame
SEM photograph Fig. 2 of BiOI catalysis materials can be seen that the micron order three-dimensional sheet of macroscopic frame is presented in the BiOI materials of synthesis,
8-10 μm, rough surface and there is larger specific surface area and porosity.
The light degradation of rhodamine B solution is reacted, and eight magnetic stirring apparatus is used in camera bellows, with full quartz glass reaction test tube
As reaction vessel, 500 W xenon lamp simulated visible light illumination of the heart in the reactor, install quartzy cold-trap, band additional outside lamp source
Heat is walked, protection light source ensures the uniformity of experiment at the same time.In evaluation, 10 mg catalyst are scattered in 50 mL, 10 mg/L's
In rhodamine B solution, lucifuge reacts 2 h, and lamp source is opened after dark reaction and carries out light degradation.In reaction process, at interval of one
The section time takes out 1 mL liquid with syringe, and solution absorbance is measured after filtering and calculates degradation rate.Fig. 3 is through 6 h illumination
Rhodamine B degraded situation, degradation rate reach 66.8%, and micron order three-dimensional sheet structure BiOI is to the degradation rate of rhodamine B in 3 h
It inside can reach 65%.
Embodiment 2
A kind of preparation method of the three-dimensional sheet BiOI catalysis materials with macroscopic frame, mainly includes the following steps that：
（1）Under conditions of 26 DEG C, structure directing agent polyvinylpyrrolidone and bismuth source are dissolved in organic solvent；Violent
Stirring is lower to add propiodal, continues to stir 60min；Wherein bismuth source, the molar ratio of propiodal are 1：0.5；The weight of polyvinylpyrrolidone
It is 600 r/min to measure as 0.375 g, mixing speed；
（2）By step（1）It is polytetrafluoroethylene (PTFE) that gained settled solution, which is transferred to liner, and capacity is the stainless steel reaction under high pressure of 250mL
In kettle, organic solvent adjustment amount of fill is 60%, 140 DEG C, carries out 24 h of crystallization；
（3）It is cooled to room temperature, filters to obtain solid product, product first washed for several times with absolute ethyl alcohol, then use deionized water
For several times, fully washing is after 50 DEG C, dry 24 h for washing.
The XRD spectra of the three-dimensional sheet BiOI catalysis materials of the obtained macroscopic frame prepared is similar to Fig. 1, and SEM shines
Piece is similar to Fig. 2.Micron order three-dimensional sheet, rough surface and has larger specific surface area and porosity.Photocatalytic degradation
It is similar to Fig. 3.
Embodiment 3
A kind of preparation method of the three-dimensional sheet BiOI catalysis materials with macroscopic frame, mainly includes the following steps that：
（1）Under conditions of 28 DEG C, structure directing agent polyvinylpyrrolidone and bismuth source are dissolved in organic solvent；Violent
Stirring is lower to add propiodal, continues to stir 10 min；Bismuth source, the molar ratio of propiodal are 1： 2；The weight of polyvinylpyrrolidone is
0.375 g, mixing speed are 600 r/min；
（2）By step（1）It is polytetrafluoroethylene (PTFE) that gained settled solution, which is transferred to liner, and capacity is the stainless steel reaction under high pressure of 250mL
In kettle, organic solvent adjustment amount of fill is 80%, 180 DEG C, carries out 9 h of crystallization；
（3）It is cooled to room temperature, filters to obtain solid product, product first washed for several times with absolute ethyl alcohol, then use deionized water
For several times, fully washing is after 90 DEG C, dry 8 h for washing.
The XRD spectra of the three-dimensional sheet BiOI catalysis materials of the obtained macroscopic frame prepared is similar to Fig. 1, and SEM shines
Piece is similar to Fig. 2.Micron order three-dimensional sheet, rough surface and has larger specific surface area and porosity.Photocatalytic degradation
It is similar to Fig. 3.
Embodiment 4
The preparation of spherical BiOI：Under room temperature, magnetic agitation（480 r/s）, by 1.358 g, five nitric hydrate bismuth Bi (NO3)2·
5H2O and 0.15 g polyvinylpyrrolidones（K-30）It is dissolved in 50 mL ethylene glycol.0.485 g potassium iodide KI are added, are persistently stirred
Mix 30 min.Above-mentioned solution is transferred in the autoclave of 100 mL, adding 30 mL ethylene glycol makes loadings reach 80%, puts
Enter in 160 DEG C of baking ovens and keep 12 h.Natural cooling, filtering, is washed three times, obtained solid respectively with ethanol, deionized water successively
Sample is at 70 DEG C, dry 12 h.As can be seen from Figure 4 synthesized material is BiOI and crystallinity is good.Fig. 5 can be seen
The BiOI for going out synthesis is the spheroidal material that sheet is self-assembly of.
Embodiment 5
The preparation of the spherical BiOI of groove：Under room temperature, magnetic agitation（480 r/s）, by 3.395 g, five nitric hydrate bismuths（Bi
(NO3)2·5H2O）With 0.375 g PVP（K-30）It is dissolved in 150 mL ethylene glycol.Add 1.162 g potassium iodide（KI）, continue
Stir 30 min.Above-mentioned solution is transferred in the autoclave of 250 mL, is put into 160 DEG C of baking ovens and keeps 12 h.Naturally it is cold
But, filter, washed respectively three times with ethanol, deionized water successively, obtained solid sample is at 70 DEG C, dry 12 h.From Fig. 6
It can be seen that synthesized material is BiOI and crystallinity is good.Fig. 7 can be seen that the BiOI of synthesis is reeded spherical material
Material.
From embodiment 1,4 and 5 test result indicates that, following two kinds of conditions can produce the pattern of the material of synthesis, structure
It is raw directly to influence：1）Loading is identical, reaction kettle capacity is different；2）Reaction kettle capacity is identical, and loading is different.
Although above the present invention is made to retouch in detail with general explanation, embodiment and experiment
State, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Scope.
Claims (9)
1. a kind of preparation method of the three-dimensional sheet BiOI catalysis materials with macroscopic frame, it is characterised in that mainly include
Following steps：
（1）Under conditions of 26 ~ 28 DEG C, structure directing agent polyvinylpyrrolidone and bismuth source are dissolved in organic solvent；
Lower addition propiodal is vigorously stirred, continues 10 ~ 60 min of stirring；
（2）By step（1）Gained settled solution is transferred in stainless steel autoclave, organic solvent adjustment amount of fill for 60% ~
80%, 140 ~ 180 DEG C, carry out 9 ~ 24 h of crystallization；
（3）It is cooled to room temperature, filters to obtain solid product, fully washing is carried out to product after 50 ~ 90 DEG C, dry 8 ~ 24 h.
2. preparation method according to claim 1, it is characterised in that the bismuth source, the molar ratio of propiodal are 1：0.5~
2。
3. preparation method according to claim 1, it is characterised in that the stainless steel autoclave liner is poly-
Tetrafluoroethene, capacity 250mL；Total dosage of the organic solvent is 150 ~ 200 mL.
4. preparation method according to claim 2, it is characterised in that the bismuth source includes five nitric hydrate bismuths, carbonic acid
One or more in oxygen bismuth, bismuth sulfate；The organic reagent is included in ethylene glycol, glycol monoethyl ether, glycerine
It is one or more kinds of；The propiodal includes a kind of or more in potassium iodide, sodium iodide, cetyl trimethyl ammonium iodide
Kind.
5. preparation method according to claim 1, it is characterised in that step（1）The mixing speed is 350 ~ 600
r/min。
6. preparation method according to claim 1, it is characterised in that step（3）The washing is first to use absolute ethyl alcohol
Washing for several times, then is washed with deionized for several times.
7. urged according to the three-dimensional sheet BiOI light with macroscopic frame prepared by claim 1-6 any one of them preparation method
Change material.
8. the application of the three-dimensional sheet BiOI catalysis materials according to claim 7 with macroscopic frame, its feature exist
In the photochemical catalyst as the degraded of organic dyestuff.
9. the application of the three-dimensional sheet BiOI catalysis materials according to claim 7 with macroscopic frame, its feature exist
In as catalyst carrier, carried noble metal forms the catalysis material of heterojunction structure.
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| CN108816254A (en) * | 2018-06-19 | 2018-11-16 | 东北大学 | A kind of BiOI catalysis material and its preparation method and application |
| CN108940325A (en) * | 2018-07-23 | 2018-12-07 | 汕头大学 | A kind of binary composite semiconductor light-catalyst materials A g2CrO4/ BiOI and its preparation and application |
| CN109046400A (en) * | 2018-07-23 | 2018-12-21 | 汕头大学 | A kind of BiOI photochemical catalyst and its preparation and application that precious metals pt is modified |
| CN109134228A (en) * | 2018-06-22 | 2019-01-04 | 杭州电子科技大学 | A kind of method that room temperature catalytic phenylmethanol generates benzaldehyde |
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| CN112023955A (en) * | 2020-08-31 | 2020-12-04 | 上海电力大学 | Preparation method of three-dimensional spherical bismuth oxybromide-bismuth oxyiodate heterojunction with visible light broad-spectrum response |
| CN113735167A (en) * | 2021-09-18 | 2021-12-03 | 淮阴师范学院 | Iodine deficient BiO1.2I0.6Method for preparing microspheres |
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| CN108940325A (en) * | 2018-07-23 | 2018-12-07 | 汕头大学 | A kind of binary composite semiconductor light-catalyst materials A g2CrO4/ BiOI and its preparation and application |
| CN109046400A (en) * | 2018-07-23 | 2018-12-21 | 汕头大学 | A kind of BiOI photochemical catalyst and its preparation and application that precious metals pt is modified |
| CN108940325B (en) * | 2018-07-23 | 2021-05-25 | 汕头大学 | Binary composite semiconductor photocatalyst material Ag2CrO4/BiOI and preparation and application thereof |
| CN109550512A (en) * | 2018-11-02 | 2019-04-02 | 河南师范大学 | A kind of preparation method of the flower-shaped ball tungsten sulfide/bismuthino composite material of micron |
| CN110565188A (en) * | 2019-09-08 | 2019-12-13 | 中山市蝶安芬内衣有限公司 | Preparation method and application of powder for fiber with warm-keeping and bacteriostatic functions |
| CN110565188B (en) * | 2019-09-08 | 2021-12-10 | 中山市蝶安芬内衣有限公司 | Preparation method and application of powder for fiber with warm-keeping and bacteriostatic functions |
| CN111632615A (en) * | 2020-05-11 | 2020-09-08 | 湖北臻润环境科技股份有限公司 | 2D/2DBiOI/Ti3C2Composite photocatalyst and preparation method and application thereof |
| CN112023955A (en) * | 2020-08-31 | 2020-12-04 | 上海电力大学 | Preparation method of three-dimensional spherical bismuth oxybromide-bismuth oxyiodate heterojunction with visible light broad-spectrum response |
| CN113735167A (en) * | 2021-09-18 | 2021-12-03 | 淮阴师范学院 | Iodine deficient BiO1.2I0.6Method for preparing microspheres |
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