CN106495223A - A kind of preparation method of monocline tungsten trioxide nano band - Google Patents
A kind of preparation method of monocline tungsten trioxide nano band Download PDFInfo
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- CN106495223A CN106495223A CN201610953437.6A CN201610953437A CN106495223A CN 106495223 A CN106495223 A CN 106495223A CN 201610953437 A CN201610953437 A CN 201610953437A CN 106495223 A CN106495223 A CN 106495223A
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- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- C01P2004/00—Particle morphology
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- 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
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
The invention discloses a kind of monocline Tungstic anhydride. (WO3) nano belt preparation method, including：Tungstates is dissolved in water, mix homogeneously, adds strong acid afterwards, and after continuing stirring, obtain uniform suspension, be incubated 24 72h at 150～220 DEG C, post-treated after obtain WO3Yellow powder；By WO3Yellow powder is mixed homogeneously with ethylenediamine, is incubated 6～48h at 150～220 DEG C afterwards, obtains product, will obtain banding intermediate product after cleaned clearly for product, drying；By banding intermediate product, 1～4h is incubated at 400～600 DEG C, obtains monocline WO3Nano belt.The present invention adopts the technique that hydro-thermal, solvent thermal and annealing combine, and carrys out the one-dimensional WO of synthesizing high specific surface area3Nano belt, the 1-dimention nano carrying material yield of synthesis are high, and repeatability is high, relative inexpensiveness, and specific surface area increases, and performance is improved.
Description
Technical field
The present invention relates to transition metal oxide technical field of function materials, and in particular to a kind of monocline Tungstic anhydride.
(WO3) nano belt preparation method.
Background technology
Transition metal oxide WO3There are monocline, six sides, multiple crystal structures such as orthogonal, energy gap 2.5～
Between 3.5eV, it is a kind of n-type semiconductor, is widely used in photocatalysis, electrochromism and sensor field.Material
The performance of material depends on its microstructure, including crystal structure, microstructure and dopant states etc..By changing technological parameter
Regulation and control WO3The microstructure of material, is to carry high performance effective ways.
Nano belt is typical monodimension nanometer material, with the performance not available for traditional material, for example skin effect and
Small-size effect etc..As nano belt has bigger serface, its physical property is very sensitive to surface adsorption and external environment,
It is with a wide range of applications at the aspect such as optically and electrically.
In sum, WO3Nano belt has important Research Prospects and using value.And according to document report, WO3Nanometer
The synthesis technique of band mainly has method of electrostatic spinning, solvent-thermal method, directed metal oxidation, and this is several.It is right that these methods are generally subject to
Instrument requirements are higher, the restriction of the not high aspect of obtained powder body degree of purity, can not obtain large-scale in actual production
Application.
In order to overcome these shortcomings, the method combined using solvent thermal and annealing receives the favor of people to the present invention,
Solvent-thermal method is easy to operate, can control crystal growth by factors such as the reaction temperatures and temperature retention time of adjusting solvent heat, and
Annealing can improve degree of crystallinity and stability again.
Content of the invention
The invention provides a kind of monocline Tungstic anhydride. (WO3) nano belt preparation method, using hydro-thermal, solvent thermal and move back
The technique that fire combines, carrys out the one-dimensional WO of synthesizing high specific surface area3Nano belt, the 1-dimention nano carrying material yield of synthesis are high, repeat
Property high, relative inexpensiveness, specific surface area increases, and performance is improved.
A kind of monocline WO3The preparation method of nano belt, comprises the following steps：
1) tungstates is dissolved in water, mix homogeneously, adds strong acid afterwards, and after continuing stirring, obtain uniformly suspended
Uniform suspension at 150～220 DEG C is incubated 24-72h, obtains yellow powder by liquid, will be post-treated for yellow powder after obtain
WO3Yellow powder；
2) by step 1) obtained in WO3Yellow powder is mixed homogeneously with ethylenediamine, afterwards 150～220 DEG C be incubated 6～
48h, obtains product, will obtain banding intermediate product after cleaned clearly for product, drying；
3) by step 2) the banding intermediate product for preparing, 1～4h is incubated at 400～600 DEG C, obtain monocline WO3Nanometer
Band (Lycoperdon polymorphum Vitt powder).
In the present invention, the technique that combined using hydro-thermal method, solvent thermal and annealing.Tungstates is firstly added, is blunged
Strong acid, Hydrothermal Synthesiss WO is added after dissolving3Yellow powder body；Then, by the WO of synthesis3Yellow powder body is added in ethylenediamine, and is passed through
Regulation and control reaction temperature and time, banding intermediate product is synthesized using solvent thermal process；Finally by obtained banding intermediate product
Heat treatment is carried out, the WO of monocline is prepared3Nanobelt material, gray is Lycoperdon polymorphum Vitt powder.
Step 1) in, described strong acid is nitric acid, and the mass percent of described nitric acid is 60%～70%, most preferably
65%.
The quality of described tungstates is 2.3～4.3g with the ratio of the volume of strong acid：5ml, more preferably 3.3g：
5ml.
Described post processing includes cleaning, dry and grinding, and cleaning is cleaned repeatedly using deionized water and dehydrated alcohol, is done
Dry employing is dried.
Uniform suspension is placed in reactor, and 24-72h is incubated at 150～220 DEG C.Described reactor is poly- four
Fluorothene inner bag, the closed reactor of rustless steel external member.
Uniform suspension is incubated 24h-72h, further preferably, by uniform suspension 200 at 180 DEG C～220 DEG C
24h-48h is incubated at DEG C.
Step 2) in, the volume of described ethylenediamine and step 1) in the mass ratio of tungstates be 35mL～45mL：
2.3～4.3g, more preferably 40mL：3.3g.
12h～48h is incubated at 180 DEG C～220 DEG C, further preferably, 12h～48h is incubated at 200 DEG C.
Step 3) in, 2～3h is incubated at 400～500 DEG C.
Compared with prior art, the invention has the advantages that：
Method of the present invention using from top to bottom (Top-Down), by block WO3Using ethylenediamine solvent-thermal method and annealing
Combine and carry out the one-dimensional WO of synthesizing high specific surface area3Nano belt.The 1-dimention nano carrying material yield of the method synthesis is high, repeatability
Height, relative inexpensiveness, specific surface area increase, and performance is improved.The preparation method is with low cost, it is easy to control, and product is produced
Rate is high.Compared with bulk material, the WO of preparation3Nano belt has one-dimensional pattern, and specific surface area is big, and photocatalytic activity has larger carrying
High.
The present invention prepares monocline WO by hydro-thermal, solvent thermal and annealing3Nano belt.The present invention is closed by hydro-thermal in the first step
Into block WO3Material, the synthesis for nano belt provide material source.On the other hand pass through during second step solvent thermal reaction
Ethylenediamine solvent is added, WO is effectively controlled3The morphology change of material, forms banding intermediate product.Finally push through annealing to close
Into WO3Nano belt.The preparation method is easily controllable, with low cost, and technique is relatively easy, it is possible to achieve large-scale production.
Description of the drawings
Fig. 1 is block WO prepared by the first step hydro-thermal in embodiment 13SEM photograph；
Fig. 2 is the SEM photograph of the second step solvent-thermal process banding intermediate product in embodiment 1；
Fig. 3 is the final product SEM photograph that the three-step annealing in embodiment 1 is formed.
Specific embodiment
The inventive method is further illustrated with reference to embodiments.In the present embodiment, described tungstates, strong acid, second two
It is pure that amine, dehydrated alcohol are chemistry.
Embodiment 1
1) tungstates (sodium tungstate) for weighing 3.3g is put into beaker, in water after stirring and dissolving, adds the nitric acid (matter of 5mL
Amount percent is for 65%), and continues to stir, and uniform suspension is moved into reactor inner bag afterwards, closed, is put into baking oven 200
48h, furnace cooling is incubated at DEG C；
2), after reactor cooling, the yellow powder deionized water of formation and dehydrated alcohol are cleaned repeatedly, is dried and is ground
Preserve after mill, obtain WO3Yellow powder；
3) by step 2) prepared by WO3Yellow powder, is put in the beaker of 50mL.The ethylenediamine for measuring 40mL pours beaker into
In, magnetic agitation makes the abundant disperse of yellow powder in ethylenediamine, obtains uniform suspension；
4) by step 3) the uniform suspension of gained is transferred in reactor inner bag, closed, and it is put in baking oven and protects at 200 DEG C
Warm 12h, furnace cooling to 25 DEG C of room temperature, obtains product；
5) by step 4) product of gained, deionized water and dehydrated alcohol clean repeatedly, are put into drying baker, are drying
Case inside holding is dried, and obtains banding intermediate product；
6) by step 5) the banding intermediate product of gained, it is put in Muffle furnace and heats, at 400 DEG C, is incubated 2h, gained
Lycoperdon polymorphum Vitt powder is final product, will test and analyze, and the Lycoperdon polymorphum Vitt powder for finally obtaining is monocline WO3Nano belt.
Fig. 1 is block WO prepared by the first step hydro-thermal in embodiment 13(i.e. WO3Yellow powder) SEM photograph；Fig. 2 is
The SEM photograph of the second step solvent-thermal process banding intermediate product in embodiment 1；Fig. 3 is the three-step annealing shape in embodiment 1
Into final product SEM photograph.The WO of preparation3Nano belt has one-dimensional pattern, and specific surface area is big, and photocatalytic activity has larger carrying
High.
Embodiment 2
1) tungstates (sodium tungstate) for weighing 3.3g is put into beaker, in water after stirring and dissolving, adds the nitric acid (matter of 5mL
Amount percent is for 65%), and continues to stir, and uniform suspension is moved into reactor inner bag afterwards, closed, is put into baking oven 200
24h, furnace cooling is incubated at DEG C；
2), after reactor cooling, the yellow powder deionized water of formation and dehydrated alcohol are cleaned repeatedly, is dried and is ground
Preserve after mill, obtain WO3Yellow powder；
3) by step 2) prepared by WO3Yellow powder, is put in the beaker of 50mL.The ethylenediamine for measuring 40mL pours beaker into
In, magnetic agitation makes the abundant disperse of yellow powder in ethylenediamine, obtains uniform suspension；
4) by step 3) the uniform suspension of gained is transferred in reactor inner bag, closed, and it is put in baking oven and protects at 200 DEG C
Warm 12h, furnace cooling to 25 DEG C of room temperature, obtains product；
5) by step 4) product of gained, deionized water and dehydrated alcohol clean repeatedly, are put into drying baker, are drying
Case inside holding is dried, and obtains banding intermediate product；
6) by step 5) product of gained, being put in Muffle furnace and heating, 3h, the Lycoperdon polymorphum Vitt of gained is incubated at 400 DEG C
Powder is final product, i.e. monocline WO3Nano belt.
Embodiment 3
1) tungstates (sodium tungstate) for weighing 3.3g is put into beaker, in water after stirring and dissolving, adds the nitric acid (matter of 5mL
Amount percent is for 65%), and continues to stir, and uniform suspension is moved into reactor inner bag afterwards, closed, is put into baking oven 200
48h, furnace cooling is incubated at DEG C；
2), after reactor cooling, the yellow powder deionized water of formation and dehydrated alcohol are cleaned repeatedly, is dried and is ground
Preserve after mill, obtain WO3Yellow powder；
3) by step 2) prepared by WO3Yellow powder, is put in the beaker of 50mL.The ethylenediamine for measuring 40mL pours beaker into
In, magnetic agitation makes the abundant disperse of yellow powder in ethylenediamine, obtains uniform suspension；
4) by step 3) the uniform suspension of gained is transferred in reactor inner bag, closed, and it is put in baking oven and protects at 200 DEG C
Warm 48h, furnace cooling to 25 DEG C of room temperature, obtains product；
5) by step 4) product of gained, deionized water and dehydrated alcohol clean repeatedly, are put into drying baker, are drying
Case inside holding is dried, and obtains banding intermediate product；
6) by step 5) product of gained, being put in Muffle furnace and heating, 2h, the Lycoperdon polymorphum Vitt of gained is incubated at 500 DEG C
Powder is final product, i.e. monocline WO3Nano belt.
Claims (9)
1. a kind of preparation method of monocline tungsten trioxide nano band, it is characterised in that comprise the following steps：
1) tungstates is dissolved in water, mix homogeneously, adds strong acid afterwards, and after continuing stirring, obtain uniform suspension, will
Uniform suspension is incubated 24-72h at 150～220 DEG C, obtains yellow powder, will be post-treated for yellow powder after obtain WO3Yellow
Color powder；
2) by step 1) obtained in WO3Yellow powder is mixed homogeneously with ethylenediamine, is incubated 6～48h at 150～220 DEG C afterwards, obtains
Product is arrived, banding intermediate product will be obtained after cleaned clearly for product, drying；
3) by step 2) the banding intermediate product for preparing, 1～4h is incubated at 400～600 DEG C, obtain monocline WO3Nano belt.
2. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 1) in, institute
The strong acid that states is nitric acid.
3. the preparation method of monocline tungsten trioxide nano band according to claim 2, it is characterised in that step 1) in, institute
The mass percent of the nitric acid that states is 60%～70%.
4. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 1) in, institute
The quality of the tungstates that states is 2.3～4.3g with the ratio of the volume of strong acid：5ml.
5. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 1) in, institute
The post processing that states includes cleaning, dry and grinding.
6. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 1) in, will
Uniform suspension is incubated 24h-72h at 180 DEG C～220 DEG C.
7. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 2) in, institute
The volume of the ethylenediamine that states and step 1) in the mass ratio of tungstates be 35mL～45mL：2.3～4.3g.
8. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 2) in,
180 DEG C～220 DEG C insulation 12h～48h.
9. the preparation method of monocline tungsten trioxide nano band according to claim 1, it is characterised in that step 3) in,
2～3h is incubated at 400～500 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381644A (en) * | 2017-08-22 | 2017-11-24 | 西安理工大学 | A kind of preparation method of one-dimensional tungsten trioxide nanowires |
| CN109364910A (en) * | 2018-12-14 | 2019-02-22 | 青岛大学 | A kind of isomerism tungsten trioxide nano band photochemical catalyst and the preparation method and application thereof |
| 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 |
| CN109987633A (en) * | 2017-12-29 | 2019-07-09 | 天津大学 | A kind of tungstic acid nano stick rich in Lacking oxygen, catalyst system and its preparation method and application |
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| CN102531063A (en) * | 2011-11-20 | 2012-07-04 | 湖南理工学院 | Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof |
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| CN102531063A (en) * | 2011-11-20 | 2012-07-04 | 湖南理工学院 | Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof |
| CN105923657A (en) * | 2016-07-20 | 2016-09-07 | 河南科技大学 | Preparation method of monoclinic tungsten trioxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381644A (en) * | 2017-08-22 | 2017-11-24 | 西安理工大学 | A kind of preparation method of one-dimensional tungsten trioxide nanowires |
| CN107381644B (en) * | 2017-08-22 | 2019-05-10 | 西安理工大学 | A kind of preparation method of one-dimensional tungsten trioxide nanowires |
| CN109987633A (en) * | 2017-12-29 | 2019-07-09 | 天津大学 | A kind of tungstic acid nano stick rich in Lacking oxygen, catalyst system and its preparation method and application |
| CN109987633B (en) * | 2017-12-29 | 2022-03-29 | 天津大学 | Oxygen vacancy-rich tungsten trioxide porous nanorod, catalytic system, preparation method and application thereof |
| CN109364910A (en) * | 2018-12-14 | 2019-02-22 | 青岛大学 | A kind of isomerism tungsten trioxide nano band photochemical catalyst and the preparation method and application thereof |
| CN109364910B (en) * | 2018-12-14 | 2021-05-25 | 青岛大学 | Homogeneous and heterogeneous tungsten trioxide nanobelt photocatalyst and preparation method and application thereof |
| 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 |
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Application publication date: 20170315 |