CN105236491B - A kind of thread W18O49The preparation method of material - Google Patents
A kind of thread W18O49The preparation method of material Download PDFInfo
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- CN105236491B CN105236491B CN201510536148.1A CN201510536148A CN105236491B CN 105236491 B CN105236491 B CN 105236491B CN 201510536148 A CN201510536148 A CN 201510536148A CN 105236491 B CN105236491 B CN 105236491B
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- 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
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
A kind of thread W18O49The preparation method of material, by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.03～0.08mol/L；18-amine. is added in solution A, solution B is obtained；Solution B is stirred in confined conditions, solution C is obtained；Solution C is added in autoclave, is cooled down after then reacting at 140～180 DEG C in homogeneous reactor, is obtained thread W18O49Material.Reaction condition of the present invention is gentle, temperature required relatively low, and processing step is simple, and repeatability is high, and the thread W of present invention synthesis18O49Material, methylene blue is had by stronger absorption property, good photocatalysis performance is shown to methyl orange simultaneously, specifically there is certain absorption to methyl orange in cloudy, turbid phase product, degradeds of the 40min to methyl orange before photoreaction stage reaches 80%, and its aspect of performance prediction is worth with larger exploration.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of thread W18O49The preparation method of material.
Background technology
WO3It is made up of perovskite structure unit, its crystal structure is just made up of 1 tungsten atom and 6 oxygen atoms
Octahedral unit shares zenithal alignment and forms.WO3With various crystal formations, such as monocline (m-WO3), three oblique (tr-WO3), orthogonal (o-
WO3), four directions (te-WO3), six side (h-WO3) etc..Wherein monocline, three tiltedly, orthogonal, and hexagonal structure can stable existence at normal temperatures.
The structure of crystal is to WO3Performance necessarily affect, the tungsten oxide crystal structure of such as hexagonal structure has larger pore passage structure, energy
Enough accommodate cation ic-converted for tungsten blue, it is considered to be good electrochromic material.WO3It is easily formed non-stoichiometric
WOx.There is WO in the crystal structure of the type oxide6Construction unit shares the situation of rib dough-making powder.Wherein, W18O49With maximum
Oxygen defect, be known unique non-stoichiometric WO existed with pure formx.Since [ZHU Y Q, the HU W such as ZHU
B,HSU W K,TERRONES M,GROBERT N,HARE J P.Tungsten oxide tree-like structures
[J].Chemical Physics Letters,1999,309(5/6):327-334.] the broken micron dendrite of first passage obtains
W is arrived18O49Since nano wire, researchers have synthesized the W of different-shape using various methods such as heat treatment, vapor phase growths18O49
Nanostructured, and detailed sign has been carried out to its structure and performance.The material is except with good air-sensitive, becoming normal complexion catalysis
Outside performance, good absorption-heat-convertibility energy is shown to infrared light.
Japanese scholars leaf JINHUA is further discovered that the W of 1-dimention nano filament within 201218O49Material can be shone in visible ray
Penetrate lower catalysis reduction CO2Gas [G.Xi, S.Ouyang, P.Li, J.Ye, Q.Ma, N.Su, H.Bai, C.Wang, Ultrathin
W18O49Nanowires with Diameters below 1nm:Synthesis,Near-Infrared Absorption,
Photoluminescence,and Photochemical Reduction of Carbon Dioxide,Angewandte
Chemie International Edition, 51 (2012) 2395-2399.], catalytic reaction efficiency high and do not need noble metal
Load, the W of this explanation nanostructured18O49Material can not only make up WO3The deficiency of material activity in light-catalyzed reaction, also not
Noble-metal-supported is needed, the preparation cost of material can be effectively reduced, with good potential application foreground.Current W18O49Material
Shortcomings are gone back in research in synthesis with its photocatalysis performance field, need further to explore.
The existing W for preparing 1-dimention nano filament18O49The method of material is complicated, and obtained W18O49Chemistry
Purity is low, pattern heterogeneity.
The content of the invention
To overcome the problems of the prior art, it is an object of the invention to provide a kind of technical process is simple, reaction time
Short, gained powder body chemical composition is homogeneous, crystal morphology size uniformity, the thread W of morphology controllable18O49The preparation method of material.
For achieving the above object, the technical solution used in the present invention is as follows：
1) by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.03～0.08mol/L；
2) 18-amine. is added in solution A, obtain solution B；Wherein, WCl6Ratio with the amount of the material of 18-amine. is 1：
(0.8～2)；
3) solution B is stirred in confined conditions, obtains solution C；
4) solution C is added in autoclave, then in homogeneous reactor at 140～180 DEG C reaction 12～
Cool to room temperature after 28h with the furnace, Jing after centrifugation, washing, being dried, obtain thread W18O49Material.
The magnetic agitation that specifically first carry out that stirs, then carries out supersound process.
The power of the supersound process is 60～80Hz, and the time of supersound process is 20～40min.
The autoclave is with politef as liner.
The filling rate of the autoclave is 30～60%.
The washing is carried out using dehydrated alcohol.
The drying is in vacuum drying oven or freeze drying box is carried out.
The temperature of the drying is 40～60 DEG C, and the time is 3～12h.Compared with prior art, what the present invention had is beneficial
Effect：The present invention can be prepared with obvious oriented growth and crystallinity by adding the 18-amine. as surfactant
Of a relatively high pure phase W18O49Material, overcomes W in prior art18O49The relatively low situation of material crystalline；The present invention utilizes ten
Eight amine are surfactant, by controlling 18-amine. (CH3(CH2)16CH2NH2) consumption, can be very good thread length
Degree, realizes controlledly synthesis of the single filar length in nanometer with micrometer range.The present invention prepares the W with oxygen defect18O49Material
During material, the finely dispersed W of pure phase is prepared in not blanketing with inert gas at 140～180 DEG C18O49Material, the present invention are anti-
Mild condition is answered, it is temperature required relatively low, and processing step is simple, and repeatability is high, and the thread W of present invention synthesis18O49Material
Material, has stronger absorption property to methylene blue, while good photocatalysis performance is shown to methyl orange, specifically dark anti-
Stage product is answered to have certain absorption to methyl orange, degradeds of the 40min to methyl orange before photoreaction stage reaches 80%, its performance
Aspect prediction is worth with larger exploration.
Description of the drawings
Fig. 1 is the W that the present invention is prepared under the conditions of embodiment 118O49XRD spectrum.
Fig. 2 is the W that the present invention is prepared under the conditions of embodiment 118O49SEM photograph under 30k amplifications.
Fig. 3 is the W that the present invention is prepared under the conditions of embodiment 118O49SEM photograph under 10k amplifications.
Fig. 4 is W prepared by the embodiment of the present invention 118O49Degradation curve under 500W mercury lamps to methyl orange.
Specific embodiment
It is described in detail by specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1) by 0.7931g WCl6It is added in 40mL dehydrated alcohol, is configured to the solution A of 0.05mol/L；
2) in solution A 0.5390g is added to analyze Pure Octaamine (CH3(CH2)16CH2NH2), obtain solution B；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 20min, then ultrasonic (60Hz)
30min is processed, solution C is obtained；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
40%, after then seal autoclave, cool to room temperature, Jing with the furnace after 24h being reacted at 160 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 3 times, is dried 3h in 60 DEG C in vacuum drying oven, obtains thread W18O49Material.
As seen from Figure 1：The W of product pure phase prepared by the present invention18O49Material.As seen from Figure 2：Of the invention
The W for arriving18O49It is a kind of filament.As seen from Figure 3：The thread W that the present invention is obtained18O49Single length about 0.8～
1.5μm。
As can be seen from Figure 4 there is certain absorption to methyl orange in cloudy, turbid phase product, 40min before photoreaction stage
Degraded to methyl orange reaches 80%.
Embodiment 2
1) by 0.9914g WCl6It is added in 50mL dehydrated alcohol, is configured to the solution A of 0.06mol/L；
2) in solution A 0.6468g is added to analyze Pure Octaamine (CH3(CH2)16CH2NH2), obtain solution B；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 40min, then ultrasonic (60Hz)
20min is processed, solution C is obtained；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
40%, after then seal autoclave, cool to room temperature, Jing with the furnace after 18h being reacted at 150 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 3 times, is dried 3h in 60 DEG C in vacuum drying oven, obtains thread W18O49Material.
Thread W obtained by this example18O49About 1～1.5 μm of single length.
Embodiment 3
1) by 1.0259g WCl6It is added in 60mL dehydrated alcohol, is configured to the solution A of 0.08mol/L；
2) in solution A 2.5870g is added to analyze Pure Octaamine (CH3(CH2)16CH2NH2), obtain solution B；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 20min, then ultrasonic (60Hz)
30min is processed, solution C is obtained；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
60%, after then seal autoclave, cool to room temperature, Jing with the furnace after 18h being reacted at 170 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 3 times, is dried 3h in 60 DEG C in vacuum drying oven, obtains thread W18O49Material.
Thread W obtained by this example18O49About 1.3～1.8 μm of single length.
Embodiment 4
1) by 0.4758g WCl6It is added in 40mL dehydrated alcohol, is configured to the solution A of 0.03mol/L；
2) in solution A 0.3881g is added to analyze Pure Octaamine (CH3(CH2)16CH2NH2), obtain solution B；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 40min, then ultrasonic (60Hz)
10min is processed, solution C is obtained；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
60%, after then seal autoclave, cool to room temperature, Jing with the furnace after 24h being reacted at 160 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 3 times, is dried 3h in 60 DEG C in vacuum drying oven, obtains thread W18O49Material.
Thread W obtained by this example18O49About 0.8～1.2 μm of single length.
Embodiment 5
1) by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.04mol/L；
2) 18-amine. is added in solution A, obtain solution B；Wherein, WCl6Ratio with the amount of the material of 18-amine. is 1：
0.8；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 20min, at ultrasonic (80Hz)
Process and stir under 20min airtight conditions, obtain solution C；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
40%, after then seal autoclave, cool to room temperature with the furnace after 28h being reacted at 140 DEG C in homogeneous reactor,
Jing dehydrated alcohol is centrifuged, washs 4 times, is dried 12h in 40 DEG C in vacuum drying oven, obtains thread W18O49Material.
Embodiment 6
1) by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.07mol/L；
2) 18-amine. is added in solution A, obtain solution B；Wherein, WCl6Ratio with the amount of the material of 18-amine. is 1：2；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 20min, at ultrasonic (60Hz)
Process and stir under 40min airtight conditions, obtain solution C；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
50%, after then seal autoclave, cool to room temperature, Jing with the furnace after 12h being reacted at 180 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 4 times, is dried 8h in 50 DEG C in vacuum drying oven, obtain thread W18O49Material.
Embodiment 7
1) by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.05mol/L；
2) 18-amine. is added in solution A, obtain solution B；Wherein, WCl6Ratio with the amount of the material of 18-amine. is 1：
1.5；
3) by the fresh-keeping film phonograph seal of solution B, it is to avoid with air contact, first using magnetic agitation 20min, at ultrasonic (70Hz)
Process and stir under 30min airtight conditions, obtain solution C；
4) solution C is added in autoclaves of the 100mL with politef as liner, volume packing ratio is
55%, after then seal autoclave, cool to room temperature, Jing with the furnace after 20h being reacted at 140 DEG C in homogeneous reactor
Dehydrated alcohol is centrifuged, washs 4 times, is dried in freeze drying box, obtains thread W18O49Material.
Claims (6)
1. a kind of thread W18O49The preparation method of material, it is characterised in that comprise the following steps：
1) by WCl6It is added in dehydrated alcohol, is configured to the solution A of 0.03～0.08mol/L；
2) 18-amine. is added in solution A, obtain solution B；Wherein, WCl6Ratio with the amount of the material of 18-amine. is 1：(0.8～
2)；
3) solution B is stirred in confined conditions, obtains solution C；
4) solution C is added in autoclave, after then reacting 12～28h at 140～180 DEG C in homogeneous reactor
Cool to room temperature with the furnace, Jing after centrifugation, washing, being dried, obtain thread W18O49Material；
The magnetic agitation that specifically first carry out that stirs, then carries out supersound process；
The power of the supersound process is 60～80Hz, and the time of supersound process is 20～40min.
2. a kind of thread W according to claim 118O49The preparation method of material, it is characterised in that the autoclave
With politef as liner.
3. a kind of thread W according to claim 1 and 218O49The preparation method of material, it is characterised in that the high pressure is anti-
The filling rate for answering kettle is 30～60%.
4. a kind of thread W according to claim 118O49The preparation method of material, it is characterised in that the washing is to adopt
What dehydrated alcohol was carried out.
5. a kind of thread W according to claim 118O49The preparation method of material, it is characterised in that the drying is true
In empty drying baker or freeze drying box is carried out.
6. a kind of thread W according to claim 518O49The preparation method of material, it is characterised in that in vacuum drying oven
When being dried, dry temperature is 40～60 DEG C, and the time is 3～12h.
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Cited By (1)
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| CN107523988A (en) * | 2017-07-21 | 2017-12-29 | 西北大学 | A kind of W18O49Coat carbon fibre composite and preparation method thereof |
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| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
| CN103611170B (en) * | 2013-11-21 | 2015-08-26 | 南通南京大学材料工程技术研究院 | Have the W of photo-thermal therapy and CT contrast ability concurrently 18o 49the preparation method of nano-particle |
| CN103977789B (en) * | 2014-05-23 | 2016-06-01 | 福州大学 | A kind of W18O49Nanometer ball peroxidase and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107523988A (en) * | 2017-07-21 | 2017-12-29 | 西北大学 | A kind of W18O49Coat carbon fibre composite and preparation method thereof |
| CN107523988B (en) * | 2017-07-21 | 2020-05-05 | 西北大学 | W18O49Coated carbon fiber composite material and preparation method thereof |
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