CN104445420A - Preparation method of bismuth tungstate photo-catalyst with vehicle wheel shaped three-dimensional hierarchical structure - Google Patents
Preparation method of bismuth tungstate photo-catalyst with vehicle wheel shaped three-dimensional hierarchical structure Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 53
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 50
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 50
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 150000001621 bismuth Chemical class 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 150000003657 tungsten Chemical class 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-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
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 230000009286 beneficial effect Effects 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 40
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 10
- 239000007864 aqueous solution Substances 0.000 abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [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 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a bismuth tungstate photo-catalyst with a vehicle wheel shaped three-dimensional hierarchical structure, belonging to the field of photo-catalysis. The preparation method is mainly characterized by comprising the following step: by adopting bismuth salt, tungsten salt and sulfate as main raw materials, preparing the bismuth tungstate photo-catalyst with the vehicle wheel shaped three-dimensional hierarchical structure by virtue of a simple hydrothermal process. The prepared catalyst has effective visible light photo-catalytic activity. The preparation method comprises the following preparation steps: (1) firstly dissolving bismuth salt into a nitric acid solution with a certain concentration, then mixing with a tungsten salt aqueous solution with a stoichiometric ratio, and uniformly stirring; and (2) preparing a sulfate aqueous solution with a certain concentration, slowly adding into the solution obtained in the step (1), fully stirring, then charging into a reaction kettle to perform hydrothermal reaction, and washing, centrifuging and drying an obtained product to obtain a vehicle wheel shaped bismuth tungstate photo-catalyst. The method disclosed by the invention is simple in process and low in cost; and the prepared bismuth tungstate photo-catalyst with the vehicle wheel shaped three-dimensional hierarchical structure has very high visible light photo-catalytic activity.
Description
Technical field
The invention belongs to photocatalysis field, relate to and adopt hydrothermal method to prepare wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst material, by the regulation and control of raw material type and add-on, can realize the successful preparation of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst material, and gained wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst has efficient visible light catalysis activity.
Background technology
The control of environmental pollution is face of mankind nowadays and the focal issue needing solution badly, and the environmental problem that particularly poisonous, Persistent organic pollutants (as halides, agricultural chemicals, dyestuff etc.) cause has become affects human survival and healthy significant problem.The purification of photocatalysis technology to organic pollutant has the advantages such as energy consumption is low, purification condition is gentle, non-secondary pollution and extremely payes attention to, and is a kind of green environment Treatment process with broad prospect of application.The key of photocatalysis technology is photocatalyst, with TiO
2for traditional photocatalyst material greater band gap of representative, can only by ultraviolet excitation, and also photo-generate electron-hole is to easy compound, causes photocatalysis efficiency lower.In order to make photocatalysis technology move towards practical further, give full play to its advantage in environmental pollution improvement, development is efficient, high stability photocatalyst material system is inexorable trend.Bismuth system photocatalyst material excites wide spread interest because having the energy gap of special laminate structure and suitable size.The bismuth series photocatalyst reported at present mainly comprises bismuth oxide, BiOX, the oxysalt of bismuth and compound bismuth catalyst etc.
As the one of novel photocatalyst bismuth series photocatalyst, bismuth tungstate (Bi
2wO
6) be a kind of multi-element compounds with laminate structure, by WO
6octahedra corner-sharing forms flaggy, and interlayer is dispersed with one deck [Bi
2o
2]
2+.Bi
2wO
6be typical bismuth series photocatalyst, it all shows excellent visible light catalysis activity in environmental pollution improvement and solar energy converting.Bi
2wO
6catalytic activity is under visible light illumination higher, can produce O by splitting water
2and degradation of organic substances (CHCl
3and CH
3cHO).But these utilize high temperature solid-state method to prepare Bi
2wO
6the method of material, not only need to consume a large amount of energy, and the product specific surface area obtained is less, and size is comparatively large, is unfavorable for the raising of photocatalysis property.For improving the defect of Solid phase synthesis, being recently reported and preparing Bi with soft chemical method
2wO
6nano material, but in the photocatalytic process of reality, there is size little Yi and reunite, be unfavorable for repeating the shortcomings such as recycling in photocatalyst nano-powder.But the photocatalyst of three-dimensional hierarchical structure effectively avoids the unfavourable condition of nano-powder, its overall dimensions is larger, but composition primitive still keeps nanoscale, both the efficient catalytic efficiency that nanoscale brings had been kept, be conducive to again the recycling of catalyzer, therefore, it is significant for constructing the bismuth tungstate photocatalyst with three-dimensional hierarchical structure.This patent utilizes simple hydrothermal method one step to realize the preparation of wheel shape three-dimensional hierarchical structure bismuth tungstate, and is studied its efficient photocatalysis performance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst, the method technique is simple, with low cost, and the bismuth tungstate photocatalyst of synthesis has efficient photocatalysis performance, and is beneficial to recycling.
A kind of preparation method of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst, it is characterized in that: with bismuth salt, tungsten salt, sodium sulfate for main raw material, wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst is obtained by simple hydrothermal method, the photocatalyst of preparation has efficient visible light catalysis activity, be beneficial to recycling, concrete preparation process is:
(1) be dissolved in the 2M dilute acid solution of 1 ~ 10mL by 1mmol bismuth salt, form clear solution A, be dissolved in 20mL deionized water by the tungsten salt of metering ratio, and it slowly added in solution A, stir 0.5 ~ 1h, the solution of formation is denoted as B solution;
(2) a certain amount of vitriol is dissolved in 10mL deionized water, slowly add in B solution, continue stirring 0.5 ~ 1h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 150 ~ 200 DEG C of reaction 10 ~ 30h, products therefrom centrifugation is washed, and 50 ~ 100 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
The bismuth salt mentioned in the preparation method of the wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst described in the present invention is the one in Bismuth trinitrate, bismuth chloride, and tungsten salt is the one in sodium wolframate, ammonium tungstate, and diluted acid is the one in dust technology, dilute hydrochloric acid.
The diluted acid mentioned in the preparation method of the wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst described in the present invention determines according to the selection of bismuth salt, if Bismuth trinitrate selected by bismuth salt, diluted acid selects dust technology, if bismuth salt selective chlorination bismuth, diluted acid selects dilute hydrochloric acid.
The vitriol mentioned in the preparation method of the wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst described in the present invention is the one in sodium sulfate, potassium sulfate, ammonium sulfate, and vitriol add-on is 0.2 ~ 2g.
The present invention compared with prior art, has remarkable advantage:
(1) the present invention adopts simple hydrothermal method, and with bismuth salt simple and easy to get and tungsten salt for raw material, add the successful preparation that can realize wheel shape three-dimensional hierarchical structure bismuth tungstate by vitriol, the method technique is simple, easy to operate, with low cost.
(2) bismuth tungstate photocatalyst of the wheel shape three-dimensional hierarchical structure prepared by the present invention has efficient photocatalysis performance, and the three-dimensional hierarchical structure of its large-size is beneficial to recycling.
Accompanying drawing explanation
The scanning electron photomicrograph of Fig. 1 wheel shape three-dimensional hierarchical structure bismuth tungstate sample
The X-ray diffraction style of Fig. 2 wheel shape three-dimensional hierarchical structure bismuth tungstate sample
The photocatalysis performance test of Fig. 3 wheel shape three-dimensional hierarchical structure bismuth tungstate sample
Embodiment
The preparation method of a kind of wheel shape of the present invention three-dimensional hierarchical structure bismuth tungstate photocatalyst, it is characterized in that: with bismuth salt, tungsten salt, sodium sulfate for main raw material, wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst is obtained by simple hydrothermal method, the photocatalyst of preparation has efficient visible light catalysis activity, be beneficial to recycling, concrete preparation process is:
(1) be dissolved in the 2M dilute acid solution of 1 ~ 10mL by 1mmol bismuth salt, form clear solution A, be dissolved in 20mL deionized water by the tungsten salt of metering ratio, and it slowly added in solution A, stir 0.5 ~ 1h, the solution of formation is denoted as B solution;
(2) a certain amount of vitriol is dissolved in 10mL deionized water, slowly add in B solution, continue stirring 0.5 ~ 1h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 150 ~ 200 DEG C of reaction 10 ~ 30h, products therefrom centrifugation is washed, and 50 ~ 100 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with example, but the example that content of the present invention is given below being not limited to.
The side's of enforcement example 1: the preparation method of a kind of wheel shape of the present invention three-dimensional hierarchical structure bismuth tungstate photocatalyst, concrete preparation process is:
(1) be dissolved in the 2M diluted nitric acid aqueous solution of 5mL by 1mmol Bismuth trinitrate, form clear solution A, be dissolved in 20mL deionized water by the sodium wolframate of metering ratio, and it slowly added in solution A, stir 0.5h, the solution of formation is denoted as B solution;
(2) 0.5g sodium sulfate is dissolved in 10mL deionized water, slowly add in B solution, continue to stir 0.5h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 180 DEG C of reaction 15h, products therefrom centrifugation is washed, and 60 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
Characterize through the pattern of scanning electronic microscope to prepared bismuth tungstate sample, as shown in Figure 1, the wheel shape three-dimensional hierarchical structure of the sample obtained all for being formed by flake-assembly mode, overall size is between 1.5 ~ 3 microns, sample is only deposited comparatively large, is beneficial to the recycling to photocatalyst.Characterize mutually the thing of prepared wheel shape three-dimensional hierarchical structure sample, as shown in Figure 2, all diffraction peaks can index be all orthorhombic phase bismuth tungstate (JCPDS No.73-1126).The photocatalysis performance of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst is rhodamine B degradation (Rhodamine B under the radiation of visible light provided by 300W xenon lamp, RhB) solution is weighed, and concrete experimentation is as follows: taking 50mg photocatalyst, to add concentration be 10
-5in the 100mLRhB solution of M, the solution prepared is placed in dark place dispersed with stirring and makes it reach adsorption equilibrium in 2 hours.Then solution is carried out light-catalyzed reaction, get the solution of about 5mL at regular intervals, catalyzer is fallen in centrifuging, colour contrast is carried out to its supernatant liquor, as shown in Figure 3, photocatalyst in 70 minutes by degradable for RhB be colourless, the wheel shape three-dimensional hierarchical structure bismuth tungstate prepared by explanation has higher visible light catalytic performance.
Embodiment 2: the preparation method of a kind of wheel shape of the present invention three-dimensional hierarchical structure bismuth tungstate photocatalyst, concrete preparation process is:
(1) be dissolved in the 2M diluted hydrochloric acid aqueous solution of 5mL by 1mmol bismuth chloride, form clear solution A, be dissolved in 20mL deionized water by the sodium wolframate of metering ratio, and it slowly added in solution A, stir 0.5h, the solution of formation is denoted as B solution;
(2) 1g sodium sulfate is dissolved in 10mL deionized water, slowly add in B solution, continue to stir 0.5h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 180 DEG C of reaction 15h, products therefrom centrifugation is washed, and 50 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure sodium wolframate photocatalyst.
Embodiment 3: the preparation method of a kind of wheel shape of the present invention three-dimensional hierarchical structure bismuth tungstate photocatalyst, concrete preparation process is:
(1) be dissolved in the 2M diluted nitric acid aqueous solution of 5mL by 1mmol Bismuth trinitrate, form clear solution A, be dissolved in 20mL deionized water by the ammonium tungstate of metering ratio, and it slowly added in solution A, stir 0.5h, the solution of formation is denoted as B solution;
(2) 2g ammonium sulfate is dissolved in 10mL deionized water, slowly add in B solution, continue to stir 0.5h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 180 DEG C of reaction 16h, products therefrom centrifugation is washed, and 50 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
Embodiment 4: the preparation method of a kind of wheel shape of the present invention three-dimensional hierarchical structure bismuth tungstate photocatalyst, concrete preparation process is:
(1) be dissolved in the 2M diluted nitric acid aqueous solution of 5mL by 1mmol Bismuth trinitrate, form clear solution A, be dissolved in 20mL deionized water by the sodium wolframate of metering ratio, and it slowly added in solution A, stir 0.5h, the solution of formation is denoted as B solution;
(2) 1.5g sodium sulfate is dissolved in 10mL deionized water, slowly add in B solution, continue to stir 0.5h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 160 DEG C of reaction 20h, products therefrom centrifugation is washed, and 50 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
Claims (4)
1. the preparation method of a wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst, it is characterized in that: with bismuth salt, tungsten salt, sodium sulfate for main raw material, wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst is obtained by simple hydrothermal method, the photocatalyst of preparation has efficient visible light catalysis activity, be beneficial to recycling, concrete preparation process is:
(1) be dissolved in the 2M dilute acid solution of 1 ~ 10mL by 1mmol bismuth salt, form clear solution A, be dissolved in 20mL deionized water by the tungsten salt of metering ratio, and it slowly added in solution A, stir 0.5 ~ 1h, the solution of formation is denoted as B solution;
(2) a certain amount of vitriol is dissolved in 10mL deionized water, slowly add in B solution, continue stirring 0.5 ~ 1h, then 50mL is proceeded to containing in teflon-lined stainless steel autoclave, 150 ~ 200 DEG C of reaction 10 ~ 30h, products therefrom centrifugation is washed, and 50 ~ 100 DEG C of vacuum-dryings, obtains wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst.
2. the preparation method of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst according to claim 1, it is characterized in that the bismuth salt mentioned in step (1) is the one in Bismuth trinitrate, bismuth chloride, tungsten salt is the one in sodium wolframate, ammonium tungstate.
3. the preparation method of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst according to claim 1, it is characterized in that the diluted acid mentioned in step (1) determines according to the selection of bismuth salt, if Bismuth trinitrate selected by bismuth salt, diluted acid selects dust technology, if bismuth salt selective chlorination bismuth, diluted acid selects dilute hydrochloric acid.
4. the preparation method of wheel shape three-dimensional hierarchical structure bismuth tungstate photocatalyst according to claim 1, it is characterized in that the vitriol mentioned in step (2) is the one in sodium sulfate, potassium sulfate, ammonium sulfate, vitriol add-on is 0.2 ~ 2g.
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| 段芳: "新型复合氧化物纳米结构的制备及其在可见光催化和吸附", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 段芳等: "铋系半导体光催化剂的光催化性能调控", 《化学进展》 * |
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