CN108543531A - Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application - Google Patents
Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application Download PDFInfo
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- CN108543531A CN108543531A CN201810417288.0A CN201810417288A CN108543531A CN 108543531 A CN108543531 A CN 108543531A CN 201810417288 A CN201810417288 A CN 201810417288A CN 108543531 A CN108543531 A CN 108543531A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000002077 nanosphere Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004098 Tetracycline Substances 0.000 claims abstract description 9
- 229960002180 tetracycline Drugs 0.000 claims abstract description 9
- 229930101283 tetracycline Natural products 0.000 claims abstract description 9
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 9
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 9
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 230000008520 organization Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 3
- 230000001699 photocatalysis Effects 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000010865 sewage Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 238000007605 air drying Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 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 abstract 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000000280 vitalizing effect Effects 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
- 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
- B01J23/30—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
- 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
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- C02F2101/34—Organic compounds containing oxygen
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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
The invention belongs to the preparations of photochemical catalyst, especially three-dimensional meso-hole Bi2WO6Nanosphere, the flower-like structure of three-dimensional spherical shape is assembled by nanometer sheet, and has mesoporous hierarchical organization.Preparation method is to be dissolved in bismuth nitrate in the mixed solution of ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol；Sodium tungstate is added, template is added under strong stirring and stirs to get mixed liquor；It is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, 180 DEG C of isothermal reactions are for 24 hours；White precipitate will be obtained, will be washed 23 times with deionized water and absolute ethyl alcohol respectively, obtained product natural air drying be can be prepared by into object.Synthetic method craft of the present invention is simple, of low cost, reaction is mild, and product pattern is good, photocatalytic degradation efficiency is high and is easily recycled；The Bi of preparation2WO6Photochemical catalyst is by assemble three-dimensional flower-shaped of nanometer sheet and to have mesoporous hierarchical organization, to tetracycline with higher catalytic activity.
Description
Technical field
The invention belongs to the preparations of photochemical catalyst, especially three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application.
Background technology
In recent years, as various organic pollutions are increasing, photocatalysis utilizes light as a kind of high-level oxidation technology
The energy of son carrys out the electronics of vitalizing semiconductor catalyst to cause a series of photochemical reaction, so remove atmospheric environment and
The pollutant of water environment is to achieve the purpose that environmental pollution reparation.But material is mostly only available under the conditions of ultraviolet, for
There are significant limitations for application in reality.Therefore, preparing under visible light has the catalyst of better effects just to become
It is necessary to.
Bi2WO6As one of simplest member in aurivillius oxides race, because it is non-toxic, Strong oxdiative ability,
Cheap, suitable band-gap energy absorbing wavelength is considered a kind of excellent less than the ultraviolet light of 450nm and certain visible light
Different photochemical catalyst.Three-dimensional meso-hole structure provides more photocatalysis because possessing larger specific surface area, big specific surface area
Reactivity site, the contact which increase photochemical catalyst with organic pollution；Meanwhile meso-hole structure imparts three-dimensional photocatalysis
The high-adsorption-capacity of agent.Larger specific surface area and high-adsorption-capacity improves the catalytic performance of catalyst, is conducive to improve
Its photocatalysis performance has prodigious potentiality in terms of research.
Invention content
Present invention aims at there are problems for above-mentioned, a kind of three-dimensional meso-hole Bi is provided2WO6Nanosphere and its preparation side
Method, the synthetic method craft is simple, of low cost, and the catalyst of preparation has higher catalytic activity, performance steady in tetracycline
Determine and is easily recycled.
The design scheme of the present invention：
A kind of three-dimensional meso-hole Bi2WO6Nanosphere is assembled into the flower-like structure of three-dimensional spherical shape by nanometer sheet, and with mesoporous
Hierarchical organization.
Three-dimensional meso-hole Bi2WO6The preparation method of nanosphere, includes the following steps：
(1) by Bi (NO3)3It is dissolved in the mixed solution of ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol and in magnetic agitation
It is stirred under device to being completely dissolved；Ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol volume ratio 1:1.5:1；
(2) by Na2WO4It is added in above-mentioned mixed solution and is stirred continuously；
(3) template is added under strong stirring, stirs 30min, obtains mixed liquor；
(4) above-mentioned mixed liquor is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, constant temperature is anti-under 180 DEG C of hydrothermal conditions
It should for 24 hours；
(5) white precipitate is obtained after reaction, is washed 2-3 times with deionized water and absolute ethyl alcohol respectively, the production that will be obtained
Object natural air drying, you can object Bi is made2WO6Photochemical catalyst.
Preferably, Na in the mixed liquor2WO4With Bi (NO3)3Dosage by W and Bi element ratio be 1:2.
Further, the template is cetyl trimethylammonium bromide (CTAB).
Three-dimensional meso-hole Bi2WO6Nanosphere, as photochemical catalyst for the tetracycline in treated sewage
It is an advantage of the invention that：Synthetic method craft is simple, of low cost, reaction process is mild, obtained product pattern
Well, photocatalytic degradation efficiency is high and is easily recycled；The Bi of preparation2WO6Photochemical catalyst is the three-dimensional flower-shaped and tool assembled by nanometer sheet
There is mesoporous hierarchical organization, there is higher catalytic activity to tetracycline.
Description of the drawings
Fig. 1 is Bi prepared by embodiment 12WO6The XRD spectrum of photochemical catalyst；
Fig. 2 a are Bi prepared by embodiment 12WO6One of SEM spectrum of photochemical catalyst；
Fig. 2 b are Bi prepared by embodiment 12WO6The two of the SEM spectrum of photochemical catalyst；
Fig. 2 c are Bi prepared by embodiment 12WO6The three of the SEM spectrum of photochemical catalyst；
Fig. 3 is Bi prepared by embodiment 12WO6Photochemical catalyst is under the simulated solar irradiation of 500W xenon lamps to the degradation of tetracycline
Curve；
Fig. 4 is the Bi that embodiment 1 obtains2WO6The N2 adsorption of photochemical catalyst-parsing thermoisopleth and corresponding pore-size distribution
Curve.
Specific implementation mode
It is described in conjunction with the embodiments the specific technical solution of the present invention.
A kind of three-dimensional meso-hole Bi2WO6The hydrothermal synthesis method of nanosphere, steps are as follows：
(1) by the Bi (NO of 0.97g3)3It is dissolved in the mixed solution of ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol and in magnetic
It is stirred under power blender to being completely dissolved；Ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol volume ratio 1:1.5:1；
(2) by the Na of 0.33g2WO4It is added in above-mentioned solution and is stirred continuously；
(3) it is vigorously stirred down, the CTAB of 0.8g is then added, is vigorously stirred 30min, obtains mixed liquor；
(4) mixed liquor is transferred in the reaction kettle of 50ml polytetrafluoroethylliner liners, isothermal reaction under 180 DEG C of hydrothermal conditions
24h；
(5) white precipitate obtained after reaction is centrifuged, is washed 2-3 times with deionized water and absolute ethyl alcohol, certainly
It is air-dried under the conditions of so, it is object Bi to obtain pale yellow powder2WO6Photochemical catalyst.
Fig. 1 is Bi prepared by embodiment 12WO6The XRD spectrum of photochemical catalyst, it can be seen that：The Bi of preparation2WO6Sample
Diffraction maximum is relatively sharp and impurity wave crest does not occur, shows that sample made from embodiment 1 is the very high pure phase structure of crystallinity.
Fig. 2 a to Fig. 2 c are Bi prepared by embodiment 12WO6The SEM spectrum of photochemical catalyst different amplification is shown in figure：
Sample topography prepared by embodiment 1 is the chondritic of three-dimensional and pattern is uniform.
Detection to tetracycline degradation rate：
The accurate tetracycline 50ml for measuring 15ppm, is placed in the reaction vessel of 60ml, while 0.05g implementations are added
Photochemical catalyst prepared by example 1, under magnetic stirring, dark absorption 30min,.It is irradiated with the xenon lamp (simulated solar irradiation) of 500W, often
It is sampled every 30min.Obtained sample centrifugation takes supernatant liquor, with spectrophotometric determination absorbance at 350nm, judges
Photocatalysis efficiency.
Fig. 3 is Bi prepared by embodiment 12WO6Photochemical catalyst is under the simulated solar irradiation of 500W xenon lamps to the degradation of tetracycline
Curve, it can be seen that：The Bi after the irradiation 240min of 500W xenon lamps2WO6Photocatalyst for degrading can reach 83%.
Fig. 4 is the Bi that embodiment 1 obtains2WO6The N2 adsorption of photochemical catalyst-parsing thermoisopleth and corresponding pore-size distribution
Curve, it can be seen that：Thermoisopleth belongs to typical IV types curve, shows the mesoporous property of material.Find out from graph of pore diameter distribution, material
There is the aperture of 3.8nm or so, this Bi with nano-pore structure in material2WO6Material has unique catalytic activity.
Claims (6)
1. a kind of three-dimensional meso-hole Bi2WO6Nanosphere, which is characterized in that the flower-like structure of three-dimensional spherical shape is assembled by nanometer sheet, and
And there is mesoporous hierarchical organization.
2. a kind of three-dimensional meso-hole Bi according to claim 12WO6The preparation method of nanosphere, which is characterized in that including with
Lower step：
(1) by Bi (NO3)3It is dissolved in the mixed solution of ethylene glycol, polyethylene glycol 400 and absolute ethyl alcohol and under magnetic stirring apparatus
Stirring is to being completely dissolved；
(2) by Na2WO4It is added in above-mentioned mixed solution and is stirred continuously；
(3) template is added under strong stirring, stirs 30min, obtains mixed liquor；
(4) above-mentioned mixed liquor is transferred in the reaction kettle that polytetrafluoroethylene (PTFE) is liner, isothermal reaction under 180 DEG C of hydrothermal conditions
24h；
(5) white precipitate is obtained after reaction, is washed 2-3 times with deionized water and absolute ethyl alcohol respectively, certainly by obtained product
It so air-dries, you can object Bi is made2WO6Photochemical catalyst.
3. a kind of three-dimensional meso-hole Bi according to claim 12WO6The preparation method of nanosphere, which is characterized in that ethylene glycol,
Polyethylene glycol 400 and absolute ethyl alcohol volume ratio 1:1.5:1.
4. a kind of three-dimensional meso-hole Bi according to claim 12WO6The preparation method of nanosphere, which is characterized in that described mixed
Close Na in liquid2WO4With Bi (NO3)3Dosage by W and Bi element ratio be 1:2.
5. a kind of three-dimensional meso-hole Bi according to claim 12WO6The preparation method of nanosphere, which is characterized in that the mould
Plate agent is cetyl trimethylammonium bromide.
6. a kind of three-dimensional meso-hole Bi according to claim 12WO6The purposes of nanosphere, which is characterized in that as photocatalysis
Agent is used for the tetracycline in treated sewage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810417288.0A CN108543531A (en) | 2018-05-04 | 2018-05-04 | Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810417288.0A CN108543531A (en) | 2018-05-04 | 2018-05-04 | Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application |
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| CN108543531A true CN108543531A (en) | 2018-09-18 |
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| CN201810417288.0A Withdrawn CN108543531A (en) | 2018-05-04 | 2018-05-04 | Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101757908A (en) * | 2009-12-29 | 2010-06-30 | 南开大学 | Method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting pH |
| CN101785995A (en) * | 2010-02-05 | 2010-07-28 | 华中科技大学 | Solvothermal preparation method for visible-light photocatalyst Bi2WO6 nano structure |
| CN103191723A (en) * | 2013-03-22 | 2013-07-10 | 南开大学 | Hydro-thermal synthesis method of visible light photocatalyst mesoporous Bi2WO6 |
-
2018
- 2018-05-04 CN CN201810417288.0A patent/CN108543531A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101757908A (en) * | 2009-12-29 | 2010-06-30 | 南开大学 | Method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting pH |
| CN101785995A (en) * | 2010-02-05 | 2010-07-28 | 华中科技大学 | Solvothermal preparation method for visible-light photocatalyst Bi2WO6 nano structure |
| CN103191723A (en) * | 2013-03-22 | 2013-07-10 | 南开大学 | Hydro-thermal synthesis method of visible light photocatalyst mesoporous Bi2WO6 |
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Application publication date: 20180918 |
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