CN107497459A - A kind of Bi2Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst - Google Patents
A kind of Bi2Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 53
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 18
- 239000000839 emulsion Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 13
- 229910001868 water Inorganic materials 0.000 claims description 11
- 238000002604 ultrasonography Methods 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000011941 photocatalyst Substances 0.000 abstract 3
- 238000001354 calcination Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 230000001788 irregular Effects 0.000 abstract 1
- 239000002135 nanosheet Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 102
- -1 bismuthino Chemical group 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000011149 active material Substances 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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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
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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
- 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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of Bi2Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, the composite photo-catalyst include Bi2Sn2O7Nano particle and irregular nano-sheet Bi24O31Br10.By the present invention in that with hydro-thermal method and calcination method, that is, utilize Bi2Sn2O7With Bi24O31Br10Predecessor is mixed with Bi2Sn2O7/Bi24O31Br10Composite photo-catalyst.This composite photo-catalyst can not only increase Bi24O31Br10The avtive spot on surface, carrier can also be promoted in the separation rate of material interface.It is an advantage of the invention that：Method is simple, and stability is high, and repeatability is strong.
Description
Technical field
The present invention relates to the preparation method of composite visible light catalyst, more particularly to a kind of Bi2Sn2O7/Bi24O31Br10It is multiple
Close the preparation method of visible light catalyst.
Background technology
The behind of social development is the problem of environmental pollution of getting worse, and water pollution problems is especially serious, and it is dirty to solve water
Dye problem is very urgent.At present, the main reason for causing water pollution problems is the undying discharge of industrial wastewater and resisted
Abuse of raw element etc., and the pollutant in water is difficult to be biodegradable or occur chemical degradation.This can be degraded in order to find
The method of a little pollutants, researcher has carried out numerous studies, and the appearance of photochemical catalyst specifies to solve water pollution problems
New direction.At present, the principle of photochemical catalyst is semi-conducting material after by illumination, and electrons are energized into conduction band from ground state, and lead
Electronics in band and the hole in valence band can participate in the generation of active material, and the active material of generation can be by organic matter direct oxidation
Decompose.And the principal element for influenceing photocatalysis efficiency is the energy gap and electronics and the Compound Degree in hole of semi-conducting material.
Therefore, researcher has carried out a large amount of modifications, and develops a variety of photochemical catalysts.That most study is TiO at present2With
The wide band gap semiconducters such as ZnO, because the energy gap of material is larger, ultraviolet light can only be absorbed, therefore limit its practical application.
In recent years, bismuth-based oxide semiconductor receives research and learned as a kind of new, nontoxic, green photochemical catalyst
The favor of person.Although the special electronic structure of bismuthino material and relatively scattered valence band structure determine that most of bismuthino material all may be used
To absorb visible ray, but because the recombination rate of material internal light induced electron and hole pair is of a relatively high, it is therefore necessary to material
It is modified, and it is one of common method for improving photocatalysis efficiency to construct composite.
The content of the invention
It is an object of the invention to provide a kind of method is simple, stability is high, repeated strong Bi2Sn2O7/Bi24O31Br10
The preparation method of composite visible light catalyst.
In order to realize above-mentioned purpose, the present invention uses technical scheme as follows：
A kind of Bi2Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, this method include：
1）Bi2Sn2O7Preparation：
By 0.5~2 mmol Bi (NO3)310~30 mL volume ratios are dissolved in for 1:In 10 salpeter solution, ultrasonic 10min, stir
After mixing 20min, settled solution A is obtained；
By 0.5~2 mmol Na2Sn2O3It is dissolved in 20~50mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O solution is 9~12 to pH, is obtained mixed
Compound D；Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, with 50
~100mL deionized waters and 50~100mL absolute ethyl alcohols are respectively washed 3 times, and Bi is dried to obtain under 70~90 oC2Sn2O7Yellow powder
End；
2）Bi24O31Br10The preparation of precursor solution：
By 2~4 mmol Bi (NO3)3Ultrasound is dissolved in 20~80 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution
E；
2~4 mmol KBr is dissolved in 20~50mL ethylene glycol, 1h is stirred, obtains solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；Mixture G is heated into 4.5h in 70~90 oC water-bath
Afterwards, 0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation：
By 0.01~0.2g Bi2Sn2O750~100 mL volume ratios are scattered in for 10:In 1 ethanol-water solution, ultrasound
0.5h, obtain mixture H；Solution G is added drop-wise in mixture H, obtains mixture I, after centrifugation, with ultra-pure water and anhydrous second
Alcohol is respectively washed 3 times, and 2h is dried under 70~90 oC, obtains powder J；Powder J is transferred in Muffle furnace, with 5 oC/min liter
Warm speed is heated to 400~700 oC, keeps 2h, obtains Bi2Sn2O7/Bi24O31Br10Composite visible light catalyst.
Preferably, in Bi2Sn2O7Preparation in, drying temperature is 80 oC.
Preferably, in Bi24O31Br10In the preparation of precursor solution, the temperature of water-bath is 80 oC.
Preferably, in Bi2Sn2O7/Bi24O31Br10Preparation in, dry temperature is 80 oC.
The Bi of the present invention2Sn2O7/Bi24O31Br10Composite visible light catalyst is by Bi24O31Br10Precursor aqueous solution is added drop-wise to
It is dispersed with Bi2Sn2O7In the ethanol-water solution of nano particle, then by centrifuging, washing and annealing makes Bi2Sn2O7Nano particle
It is attached to sheet Bi24O31Br10On surface, so as to form composite, it is improved performance.
In light-catalyzed reaction system, factor result in the photocatalysis efficiency of single component material and compare the defects of material internal etc.
It is low, therefore the material that two kinds of energy bands match is configured to composite, the recombination rate of photo-generated carrier can be reduced, is current
Improve a kind of common method of photocatalysis efficiency.Although Bi2Sn2O7Visible ray can be absorbed, but material light excites what is formed
The recombination rate in electronics and hole pair is higher, therefore greatly influences photocatalysis efficiency.And Bi24O31Br10As a kind of two-dimentional material
Material, also has response to visible ray, and light excites the light induced electron to be formed and hole-recombination rate also higher.Therefore, can incite somebody to action
Nano particle and two-dimensional material progress are compound, and the photocatalysis efficiency of material is improved by constructing composite.The present invention is first
By Bi24O31Br10Precursor aqueous solution and Bi2Sn2O7Particle is mixed, in composite is caused using annealing method
Bi24O31Br10Mutually formed, ultimately form the Bi that band structure intersects dislocation type2Sn2O7/Bi24O31Br10Composite visible light is catalyzed
Agent.The Bi24O31Br10Precursor aqueous solution is Bi24O31Br10Predecessor separate out before settled solution.The intersection dislocation type
Band structure refer to Bi2Sn2O7Valence band and conduction band positions be above or less than Bi24O31Br10Conduction band and valence band location, i.e.,
The heterojunction structure of mutual dislocation formula.By by Bi2Sn2O7Particulate is dispersed in sheet Bi24O31Br10On surface, in two kinds of materials
Interface can form electrical potential difference, move photo-generated carrier, reach and efficiently separate, finally in the surface of two kinds of materials difference
Active material not of the same race is formed, these active materials directly can degrade water pollutant, ensure that two kinds of materials can be with
Absorb visible ray outside, moreover it is possible to make composite inner formed light induced electron and hole to efficiently separating.
The present invention prepares Bi using chemical method2Sn2O7/Bi24O31Br10Composite visible light catalyst, method is simple, surely
Qualitative height, repeatability are strong.
Brief description of the drawings
Fig. 1 is Bi prepared by the present invention2Sn2O7/Bi24O31Br10Scanning electron microscope (SEM) photograph.
Fig. 2 is Bi2Sn2O7/Bi24O31Br10The transmission plot of composite visible light catalyst.
Fig. 3 is Bi2Sn2O7-Bi24O31Br10The scanning electron microscope (SEM) photograph of mechanical blend.
Embodiment
Embodiment 1：
1）Bi2Sn2O7Preparation
By 1.5 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 1.5 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 0.03g Bi2Sn2O7It is scattered in 50 mL, v/v=10:In 1 ethanol-water solution, ultrasonic 0.5h, mixture H is obtained；Will
Solution G is added drop-wise in mixture H, obtains mixture I, and after centrifugation, 3 times are respectively washed with ultra-pure water and absolute ethyl alcohol, and 80
2h is dried under oC, obtains powder J；Powder J is transferred in Muffle furnace, 700 oC are heated to 5 oC/min heating rate, is protected
2h is held, obtains Bi2Sn2O7/Bi24O31Br10Composite.
Prepared Bi is can be seen that by Fig. 1 and Fig. 22Sn2O7/Bi24O31Br10Composite visible light catalyst is by Bi2Sn2O7Receive
Rice particulate is uniformly adhered to sheet Bi24O31Br10On surface.
Comparative example 1
1）Bi2Sn2O7Preparation
By 1.5 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 1.5 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G；Solution is added drop-wise to 50 mL, v/v=10:In 1 ethanol-water solution,
After centrifugation, it is respectively washed 3 times with ultra-pure water and absolute ethyl alcohol, 2h is dried under 80 oC, obtains powder H；Powder H is transferred to
In Muffle furnace, 700 oC are heated to 5 oC/min heating rate, 2h is kept, obtains Bi24O31Br10Powder；
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 1.0g Bi2Sn2O7With 1.0g Bi24O31Br10Powder is scattered in 20 mL absolute ethyl alcohols, ultrasonic 0.5h, stirring
Dry out solvent under 3h, 70 oC, obtains Bi2Sn2O7-Bi24O31Br10Mix photochemical catalyst.
It is that Fig. 3 carries out SEM pictures i.e. Fig. 1 and Fig. 2 contrasts with embodiment 1 by the SEM pictures of comparative example 1, it can be seen that machine
Obtained Bi is blended in tool2Sn2O7-Bi24O31Br10Mix Bi in photochemical catalyst24O31Br10By Bi2Sn2O7Cladding.
Embodiment 2：
1）Bi2Sn2O7Preparation
By 1.0 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 1.0 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 0.01g Bi2Sn2O7It is scattered in 50 mL, v/v=10:In 1 ethanol-water solution, ultrasonic 0.5h, mixture H is obtained；Will
Solution G is added drop-wise in mixture H, obtains mixture I, and after centrifugation, 3 times are respectively washed with ultra-pure water and absolute ethyl alcohol, and 80
2h is dried under oC, obtains powder J；Powder J is transferred in Muffle furnace, 700 oC are heated to 5 oC/min heating rate, is protected
2h is held, obtains Bi2Sn2O7/Bi24O31Br10Composite.
Embodiment 3：
1）Bi2Sn2O7Preparation
By 2.0 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 2.0 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 0.05g Bi2Sn2O7It is scattered in 50 mL, v/v=10:In 1 ethanol-water solution, ultrasonic 0.5h, mixture H is obtained；Will
Solution G is added drop-wise in mixture H, obtains mixture I, and after centrifugation, 3 times are respectively washed with ultra-pure water and absolute ethyl alcohol, and 80
2h is dried under oC, obtains powder J；Powder J is transferred in Muffle furnace, 700 oC are heated to 5 oC/min heating rate, is protected
2h is held, obtains Bi2Sn2O7/Bi24O31Br10Composite.
Embodiment 4：
1）Bi2Sn2O7Preparation
By 3.0 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 3.0 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 0.1g Bi2Sn2O7It is scattered in 50 mL, v/v=10:In 1 ethanol-water solution, ultrasonic 0.5h, mixture H is obtained；Will
Solution G is added drop-wise in mixture H, obtains mixture I, and after centrifugation, 3 times are respectively washed with ultra-pure water and absolute ethyl alcohol, and 80
2h is dried under oC, obtains powder J；Powder J is transferred in Muffle furnace, 700 oC are heated to 5 oC/min heating rate, is protected
2h is held, obtains Bi2Sn2O7/Bi24O31Br10Composite.
Embodiment 5：
1）Bi2Sn2O7Preparation
By 3.0 mmol Bi (NO3)3It is dissolved in 10 mL, v/v=1:In 10 salpeter solution, ultrasonic 10min, after stirring 20min,
Obtain settled solution A；
By 3.0 mmol Na2Sn2O3It is dissolved in 10 mL deionized water and obtains solution B；
Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O to pH is 12, obtains mixture D；
Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, uses deionized water
It is respectively washed three times with absolute ethyl alcohol, Bi is dried to obtain under 80 oC2Sn2O7Yellow powder；
2）Bi24O31Br10The preparation of precursor solution
By 3.8 mmol Bi (NO3)3Ultrasound is dissolved in 50 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；
3.8 mmol KBr is dissolved in 20 mL ethylene glycol, stirs 1h, obtain solution F；
Solution F is added in solution E, 1h is stirred, obtains mixture G；After mixture G is heated into 4.5 h in 80 oC water-bath,
0.5 h is stirred at room temperature to room temperature, obtains settled solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation
By 0.15g Bi2Sn2O7It is scattered in 50 mL, v/v=10:In 1 ethanol-water solution, ultrasonic 0.5h, mixture H is obtained；Will
Solution G is added drop-wise in mixture H, obtains mixture I, and after centrifugation, 3 times are respectively washed with ultra-pure water and absolute ethyl alcohol, and 80
2h is dried under oC, obtains powder J；Powder J is transferred in Muffle furnace, 700 oC are heated to 5 oC/min heating rate, is protected
2h is held, obtains Bi2Sn2O7/Bi24O31Br10Composite.
Claims (4)
- A kind of 1. Bi2Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, it is characterised in that this method includes：1）Bi2Sn2O7Preparation：By 0.5~2 mmol Bi (NO3)310~30 mL volume ratios are dissolved in for 1:In 10 salpeter solution, ultrasonic 10min, stir After mixing 20min, settled solution A is obtained；By 0.5~2 mmol Na2Sn2O3It is dissolved in 20~50mL deionized water and obtains solution B；Solution B is transferred in solution A, obtains emulsion C；NH is added dropwise into emulsion C3•H2O solution is 9~12 to pH, is obtained mixed Compound D；Mixture D is transferred in 50mL polytetrafluoroethylliner liner, 24h is kept under 180oC, after being cooled to room temperature, is spent Ionized water and absolute ethyl alcohol are respectively washed 3 times, and Bi is dried to obtain under 70~90 oC2Sn2O7Yellow powder；2）Bi24O31Br10The preparation of precursor solution：By 2~4 mmol Bi (NO3)3Ultrasound is dissolved in 20~80 mL ethylene glycol solution, stirs 1h at room temperature, obtains solution E；2~4 mmol KBr is dissolved in 20~50mL ethylene glycol, 1h is stirred, obtains solution F；Solution F is added in solution E, 1h is stirred, obtains mixture G；Mixture G is heated into 4.5h in 70~90 oC water-bath Afterwards, 0.5 h is stirred at room temperature to room temperature, obtains settled solution G.3）Bi2Sn2O7/Bi24O31Br10Preparation：By 0.01~0.2g Bi2Sn2O750~100 mL volume ratios are scattered in for 10:In 1 ethanol-water solution, ultrasound 0.5h, obtain mixture H；Solution G is added drop-wise in mixture H, obtains mixture I, after centrifugation, with ultra-pure water and anhydrous second Alcohol is respectively washed 3 times, and 2h is dried under 70~90 oC, obtains powder J；Powder J is transferred in Muffle furnace, with 5 oC/min liter Warm speed is heated to 400~700 oC, keeps 2h, obtains Bi2Sn2O7/Bi24O31Br10Composite visible light catalyst.
- A kind of 2. Bi according to claim 12Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, it is special Sign is, in Bi2Sn2O7Preparation in, drying temperature is 80 oC.
- A kind of 3. Bi according to claim 12Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, it is special Sign is, in Bi24O31Br10In the preparation of precursor solution, the temperature of water-bath is 80 oC.
- A kind of 4. Bi according to claim 12Sn2O7/Bi24O31Br10The preparation method of composite visible light catalyst, it is special Sign is, in Bi2Sn2O7/Bi24O31Br10Preparation in, dry temperature is 80 oC.
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| CN108568303A (en) * | 2018-04-10 | 2018-09-25 | 青岛农业大学 | A kind of TiO2/Bi24O31Br10The preparation method of/BiOBr composite photocatalyst materials |
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