CN106390991A - Preparation method and application of ultra-fine WO3 nanowire - Google Patents
Preparation method and application of ultra-fine WO3 nanowire Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000006259 organic additive Substances 0.000 claims abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 9
- 238000012869 ethanol precipitation Methods 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 abstract 2
- 229910020341 Na2WO4.2H2O Inorganic materials 0.000 abstract 2
- 235000011130 ammonium sulphate Nutrition 0.000 abstract 2
- 239000000839 emulsion Substances 0.000 abstract 2
- WPZFLQRLSGVIAA-UHFFFAOYSA-N sodium tungstate dihydrate Chemical compound O.O.[Na+].[Na+].[O-][W]([O-])(=O)=O WPZFLQRLSGVIAA-UHFFFAOYSA-N 0.000 abstract 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 26
- 239000000463 material Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910008940 W(CO)6 Inorganic materials 0.000 description 1
- 229910003091 WCl6 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention provides a preparation method of an ultra-fine WO3 nanowire. The ultra-fine WO3 nanowire is prepared by virtue of a modified solvothermal method. The method comprises the following steps: weighing 0.05-0.2g of Na2WO4.2H2O and 0.1-0.4g of (NH4)2SO4, dissolving Na2WO4.2H2O and (NH4)2SO4 in 6mL deionized water, adding 2mL of 0.1-0.3mol/L hydrochloric acid solution, and stirring and mixing all ingredients uniformly, thereby obtaining a solution A; taking 5mL of cyclohexane and 0.4g of an organic additive, uniformly mixing cyclohexane with the organic additive so as to obtain a solution B; mixing solution B with the solution A to obtain an emulsion mixture, performing reaction on the emulsion mixture in a high-pressure reaction kettle at a temperature of 150-200 DEG C for 24 hours, and performing extraction, washing and drying, thereby obtaining the ultra-fine WO3 nanowire. The preparation method is low in cost, simple and convenient to operate, realizable based on one step and high in productivity; the prepared ultra-fine WO3 nanowire has relatively high photocatalysis activity and can be used for photocatalytic degradation of organic pollutants.
Description
Technical field
The invention belongs to photocatalysis, Optical Electro-Chemistry field of material technology, particularly to a kind of ultra-fine WO3The preparation of nano wire
Method and its application.
Background technology
Nano tungsten trioxide (WO3) due to there is unique design feature and excellent photoelectricity and photocatalysis performance etc. too
Sun can have boundless application prospect in the field such as battery, semiconductor photoelectric device, photocatalytic degradation material, sensor material,
Extensive concern by home and abroad many researchers.Compared with traditional semi-conducting material, nano tungsten trioxide forbidden band width
Spend narrower (2.5-3.0eV), under visible light conditions, there is good photoelectric response performance, and cheap, stable performance,
Harmless, nontoxic, efficiently can save as photochemical catalyst, using the waste gas of the organic pollution in sunshine degradation water and in the air
Can, cleaning, pollution-free.
Superfine nanowire is the one-dimensional nano structure that a kind of diameter is less than 5nm, because it has superhigh specific surface area, directly
Electro transfer path and larger quantum confinement effect, can improve further one dimension semiconductor material photocatalysis live
Property, efficient degradation organic pollution, for environmental improvement, effectively improve sun light utilization efficiency and energy saving has important meaning
Justice.At present, the preparation of tungstic acid superfine nanowire mainly adopts bottom-to-top method, such as utilizes WCl6、[W(CO)6] etc. before
Drive body and carry out alcoholysis, these presomas are typically relatively expensive, if the cheap presoma such as sodium tungstate to be adopted, synthetic route
Complicated.For solving these problems, the present invention proposes a kind of process is simple, lower-cost solvent-thermal method preparation ultrafine tungsten trioxide
Nano wire, its prominent performance can have the application of reality, effectively solving present social environmental pollution problem in photocatalysis field.
Content of the invention
It is an object of the invention to provide a kind of one-dimensional ultra-fine WO3The preparation method of nano wire and being prepared by the method
Ultra-fine WO3The application of nano wire.The inventive method is simple to operate, and cost is relatively low, and yield is higher, prepared ultra-fine WO3Nanometer
Line has higher photocatalysis performance.
The present invention comprises the following steps that：
(1) weigh 0.05～0.2gNa2WO4·2H2O and 0.1～0.4g (NH4)2SO4, it is dissolved in 6mL deionized water, add
The hydrochloric acid solution of 2mL 0.1～0.3mol/L, is uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g organic additive, transparent for gained mixed liquor is poured into step (1)
In resulting solution, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave,
150～200 DEG C are reacted 8～24 hours, naturally cool to room temperature；
(3) add hexamethylene to be extracted to step (2) to be cooled in the reactor of room temperature, that is, stand after being sufficiently stirred for
Layering, takes upper strata blue supernatant, and adding ethanol makes product precipitate, and is then centrifuged under 10000 revs/min of rotating speed with centrifuge
15 minutes, remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, the product after centrifugation is existed
50 DEG C of dryings 12 hours, obtain blue ultra-fine WO3Nano wire；
Described Na2WO4·2H2O、(NH4)2SO4, hydrochloric acid, hexamethylene and purity of alcohol be the pure above purity of chemistry；
Described organic additive is one of oleyl amine, octadecylamine or oleic acid.
The ultra-fine WO of present invention synthesis3Nano wire, diameter is only 1.5 ± 1nm, has obvious quantum confined effect and relatively
Big specific surface area, being capable of efficient degradating organic dye；Ultra-fine WO3Nano wire contains Lacking oxygen, in visible-near-infrared area
There is stronger absorption, so that photocatalysis performance is improved further.Therefore, ultra-fine WO3Nano wire as a kind of visible light-responded material,
In environmental pollution such as degradation of dye, photocatalysis treatment sewage, the aspect such as solar cell has very big application potential.
Brief description
Fig. 1 is the ultra-fine WO of the embodiment of the present invention 1 preparation3The transmission electron microscope picture of nano wire.
Fig. 2 is the ultra-fine WO of the embodiment of the present invention 1 preparation3The XRD spectrum of nano wire.
Fig. 3 is the ultra-fine WO of the embodiment of the present invention 1 preparation3The x-ray photoelectron energy spectrum diagram (XPS) of nano wire.Fig. 3 a is
Ultra-fine WO3The full spectrogram of XPS of nano wire, Fig. 3 b is the high-resolution XPS spectrum figure of W4f.
Fig. 4 is the ultra-fine WO of the embodiment of the present invention 1 preparation3Ultraviolet-visible light (UV-Vis) diffusing reflection spectrum of nano wire
Figure.
Fig. 5 is the ultra-fine WO of the embodiment of the present invention 1 preparation3Nano wire and the photocatalysis performance test chart of block.
Specific embodiment
Embodiment 1：
(1) weigh 0.1gNa2WO4·2H2O and 0.2g (NH4)2SO4, it is dissolved in 6mL deionized water, add 2mL0.3mol/L
Hydrochloric acid solution, be uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g oleyl amine, transparent for gained mixed liquor is poured into step (1) gained molten
In liquid, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave, 200 DEG C
Reaction 8 hours, naturally cools to room temperature；
(3) have cooled to step (2) in the reactor of room temperature add hexamethylene to be extracted, standing point after being sufficiently stirred for
Layer, takes upper strata blue supernatant, and adding ethanol makes product precipitate, and is then centrifuged 15 under 10000 revs/min of rotating speed with centrifuge
Minute, remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, by the product after being centrifuged 50
DEG C drying 12 hours, obtains blue ultra-fine WO3Nano wire.
The ultra-fine WO of embodiment 1 preparation3The transmission electron microscope picture of nano wire and XRD spectrum refer to Fig. 1 and Fig. 2.Fig. 1 shows
Show WO3The diameter of nano wire is 1～2nm, and Fig. 2 shows that this nano wire is hexagonal phase structure.Fig. 3 is the ultra-fine of embodiment 1 preparation
WO3The x-ray photoelectron energy spectrum diagram (XPS) of nano wire.Wherein, Fig. 3 a is ultra-fine WO3The full spectrogram of XPS of nano wire, Fig. 3 b is
The high-resolution XPS spectrum figure of W4f.The WO that Fig. 3 explanation obtains3W is contained in nano wire5+And W6+, it is a kind of containing oxygen defect
WO3.Fig. 4 is the ultra-fine WO of embodiment 1 preparation3The ultraviolet-visible light (UV-Vis) of nano wire diffuses spectrogram it is seen that sample
There is stronger absorption in visible region, be conducive to strengthening photocatalysis performance.Prepared WO3Superfine nanowire is as photochemical catalyst
For Visible Light Induced Photocatalytic methyl orange, the photochemical catalyst prepared by 50mg embodiment 1 is taken to be the methyl orange of 20mg/L with 50mL concentration
Solution mixes, and stirring in the dark makes catalyst reach adsorption equilibrium in 30 minutes, is then turned on 450W Metal halogen lamp, by filtering
Piece filters the ultraviolet light of below 420nm, samples at set intervals, centrifuging and taking supernatant, is surveyed with ultraviolet-visible spectrophotometer
Determine absorbance, according to methyl orange solution working curve, the concentration of methyl orange in solution after acquisition photocatalytic degradation.Fig. 5 is real
Apply the ultra-fine WO of example 1 preparation3Nano wire and the photocatalysis performance test chart of block.As can be seen from Figure 5, WO3The light of superfine nanowire
Catalysis activity is far above business WO3Block, is highly suitable for photocatalysis degradation organic contaminant.
Embodiment 2：
(1) weigh 0.05gNa2WO4·2H2O and 0.1g (NH4)2SO4, it is dissolved in 6mL deionized water, add 2mL 0.1mol/
The hydrochloric acid solution of L, is uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g oleic acid, transparent for gained mixed liquor is poured into step (1) gained molten
In liquid, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave, 150 DEG C
Reaction 24 hours, naturally cools to room temperature；
(3) add hexamethylene to be extracted in the reactor cooling down to step (2), that is, be sufficiently stirred for rear stratification, take
Upper strata blue supernatant, adding ethanol makes product precipitate, and is then centrifuged 15 minutes under 10000 revs/min of rotating speed with centrifuge,
Remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, by the product after centrifugation in 50 DEG C of dryings
12 hours, obtain blue WO3Nano wire.
Embodiment 3：
(1) weigh 0.2gNa2WO4·2H2O and 0.4g (NH4)2SO4, it is dissolved in 6mL deionized water, add 2mL0.2mol/L
Hydrochloric acid solution, be uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g octadecylamine, transparent for gained mixed liquor is poured into step (1) gained
In solution, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave, 180
DEG C reaction 12 hours, naturally cool to room temperature；
(3) have cooled to step (2) in the reactor of room temperature add hexamethylene to be extracted, that is, stand after being sufficiently stirred for
Layering, takes upper strata blue supernatant, and adding ethanol makes product precipitate, and is then centrifuged under 10000 revs/min of rotating speed with centrifuge
15 minutes, remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, the product after centrifugation is existed
50 DEG C of dryings 12 hours, obtain blue WO3Nano wire.
Embodiment 4：
(1) weigh 0.1gNa2WO4·2H2O and 0.2g (NH4)2SO4, it is dissolved in 6mL deionized water, add 2mL 0.1mol/L
Hydrochloric acid solution, be uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g oleyl amine, transparent for gained mixed liquor is poured into step (1) gained molten
In liquid, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave, 200 DEG C
Reaction 12 hours, naturally cools to room temperature；
(3) have cooled to step (2) in the reactor of room temperature add hexamethylene to be extracted, standing point after being sufficiently stirred for
Layer, takes upper strata blue supernatant, and adding ethanol makes product precipitate, and is then centrifuged 15 under 10000 revs/min of rotating speed with centrifuge
Minute, remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, by the product after being centrifuged 50
DEG C drying 12 hours, obtains blue WO3Nano wire.
Na in embodiments above2WO4·2H2O、(NH4)2SO4, hydrochloric acid, hexamethylene and purity of alcohol be chemistry
Pure above purity.
Claims (2)
1. a kind of ultra-fine WO3The preparation method of nano wire is it is characterised in that concretely comprise the following steps：
(1) weigh 0.05～0.2g Na2WO4·2H2O and 0.1～0.4g (NH4)2SO4, it is dissolved in 6mL deionized water, add 2mL
The hydrochloric acid solution of 0.1～0.3mol/L, is uniformly mixed；
(2) measure 5mL hexamethylene to mix with 0.4g organic additive, transparent for gained mixed liquor is poured into step (1) gained
In solution, stir 5 minutes, obtain white " milky " mixture, this mixture is poured in 25mL ptfe autoclave, 150
～200 DEG C are reacted 8～24 hours, naturally cool to room temperature；
(3) have cooled to step (2) in the reactor of room temperature add hexamethylene to be extracted, that is, standing point after being sufficiently stirred for
Layer, takes upper strata blue supernatant, and adding ethanol makes product precipitate, and is then centrifuged 15 under 10000 revs/min of rotating speed with centrifuge
Minute, remove supernatant, repeat to process 3 times with hexamethylene extraction, ethanol precipitation, centrifugation, by the product after being centrifuged 50
DEG C drying 12 hours, obtains blue ultra-fine WO3Nano wire；
Described Na2WO4·2H2O、(NH4)2SO4, hydrochloric acid, hexamethylene and purity of alcohol be the pure above purity of chemistry；
Described organic additive is one of oleyl amine, octadecylamine or oleic acid.
2. the ultra-fine WO that preparation method as claimed in claim 1 obtains3Nano wire has for photocatalytic degradation as photochemical catalyst
Organic pollutants.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046321A (en) * | 2018-07-10 | 2018-12-21 | 北京工业大学 | A kind of nanometer tungsten oxide and its preparation method and application |
| CN109908891A (en) * | 2019-04-16 | 2019-06-21 | 齐鲁工业大学 | A kind of efficient oxygen vacancy tungsten trioxide nano fiber catalysis material and preparation method thereof |
| CN111994957A (en) * | 2020-08-20 | 2020-11-27 | 临沂大学 | WO (WO)3Gas-sensitive material and preparation method and application thereof |
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| JP2005075654A (en) * | 2003-08-28 | 2005-03-24 | National Institute For Materials Science | Single crystal tungsten oxide nanotube, single crystal tungsten oxide nanowire, and method for manufacturing them |
| CN101318703A (en) * | 2008-07-08 | 2008-12-10 | 清华大学 | Tungstic oxide nano-wire and method for preparing tungstic oxide nano-wire ammonia sensitive sensor |
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