CN107188226A - Vanadium trioxide particle of gold load and preparation method thereof - Google Patents
Vanadium trioxide particle of gold load and preparation method thereof Download PDFInfo
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- CN107188226A CN107188226A CN201710407114.1A CN201710407114A CN107188226A CN 107188226 A CN107188226 A CN 107188226A CN 201710407114 A CN201710407114 A CN 201710407114A CN 107188226 A CN107188226 A CN 107188226A
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- 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
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2006/80—Compositional purity
Abstract
The present invention provides a kind of vanadium trioxide particle of gold load and preparation method thereof, and method includes：1) vanadium trioxide particle is calcined under inert gas atmosphere, the vanadium trioxide particle activated；2) the activation vanadium trioxide particle after cooling is added to the water, forms suspending liquid A；3) by gold chloride formation chlorauric acid solution B soluble in water；4) chlorauric acid solution B formation suspension C is added to suspending liquid A；5) stood after ultrasound suspending liquid C, generation has black flocculent deposit in suspension C；6) the suspension C that generation has black flocculent deposit is centrifuged, obtains sediment；7) sediment is dried, the flower-shaped particle of gold-nanoparticle-supported vanadium trioxide is obtained.The particle diameter of the flower-shaped particle of vanadium trioxide of gold load prepared by the above method is 45 microns, the nanometer sheet thickness of the flower-shaped particle of composition is about 10 nanometers, and the particle diameter of the gold grain of load is about 10 20 nanometers, and synthetic method is simple, with low cost, can large-scale use.
Description
Technical field
The invention belongs to vanadium trioxide particle and its preparation side of field of nanometer technology, more particularly to a kind of gold load
Method.
Background technology
Vanadium oxide nano particle is due to its unique lamellar structure, the property such as outstanding light, electricity, magnetic, in lithium battery, gas
Sensing and catalytic field have very outstanding performance, receive the extensive concern of people.Vanadium oxide mainly includes three kinds of oxygen
Compound：Vanadic anhydride, vanadium dioxide and vanadium trioxide.Different vanadium oxides are according to property different application in different fields.
This patent is only sketched due to relating only to vanadium trioxide to it.Vanadium trioxide is used as traditional catalyst quilt
Known to people.In this year, as the research to its nanostructured is gradually goed deep into, it is in traditional catalysis and new lithium ion
The premium properties produced in terms of battery is by people's extensive concern.Vanadium trioxide is a kind of with the mutual transformational of conductor insulation
The material of matter.At a certain temperature, its electric conductivity has qualitative leap to material with this property, i.e., be converted to from conductor
Insulator is converted to conductor from insulator, and this process is reversible.
In addition, research show noble metal load (especially golden load) can be different degrees of raising its functional character
(such as catalytic property).But the method for load often focuses on physical method, and granule-morphology is often the membrane structure of lamella.
Such as someone makes catalyst film using physical method (the physical vapor deposition method under such as UHV condition), such as in three oxygen
Change (0001) face gold-supported of two vanadium.But this higher complex operation of method cost, is unfavorable for large-scale production.
The content of the invention
In consideration of it, the application proposes three gold-nanoparticle-supported oxidations two that are a kind of simple and can be mass-produced
The method of the flower-shaped particle of vanadium simultaneously proposes a kind of vanadium trioxide particle of gold load prepared by this method.With physical method phase
Than, the method for invention is simple to operate, flexible, is not limited to membrane structure, can any pattern vanadium trioxide
(such as spherical, flower-shaped) load gold nano grain on grain, technical process environmental protection is with low cost.
The first object of the present invention is to provide a kind of vanadium trioxide particle of gold load, with flower-shaped grain structure.
The vanadium trioxide grain structure of gold load is self-assembly of for vanadium trioxide nanometer sheet in the embodiment of the present invention
Flower-shaped micron particles；
The particle diameter of flower-shaped micron particles is 4-5 microns, and the nanometer sheet thickness of composition flower-like structure is 8-12 nanometers；
Gold nano grain is dispersed in vanadium trioxide nanometer sheet surface.
In addition, vanadium trioxide nanometer sheet thickness is about 10 nanometers, the gold nano grain of load is a diameter of 10-20 nanometers,
Gold nano grain is evenly distributed on the nanometer sheet surface of vanadium trioxide.
The second object of the present invention is to provide a kind of preparation method of the vanadium trioxide particle of gold load, this method behaviour
Make simple, with low cost, safety and environmental protection, can be with large-scale application in actual production.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of method for the vanadium trioxide particle for preparing gold load, including：
1) pure substance of vanadium trioxide particle is calcined under inert gas atmosphere, makes the activation of vanadium trioxide particle simultaneously
Cooled down in inert gas, the vanadium trioxide particle activated；
2) the activation vanadium trioxide particle after cooling is added in deionized water, stirred, form suspending liquid A；
3) gold chloride is dissolved in deionized water, stirred, form chlorauric acid solution B；
4) chlorauric acid solution B is added to suspending liquid A, forms suspension C；
5) stood after ultrasound suspending liquid C, generation has black flocculent deposit in suspension C；
6) the suspension C that generation has black flocculent deposit is centrifuged, obtains sediment；
7) sediment is dried, the vanadium trioxide particle of gold load is obtained.
Alternatively, the step 1) in vanadium trioxide particle be flower-like structure particle, purity is 99.0-
99.6%.
Alternatively, the step 1) in calcining heat be 300 DEG C -400 DEG C, calcination time is 2-6h；
Inert gas is nitrogen or argon gas.
Alternatively, chlorauric acid solution B molar concentrations are 0.01-0.1mol/L.
Alternatively, step 4) at 15-30 DEG C, to suspending liquid A add chlorauric acid solution B, formed gold and vanadium mole
Than the suspension C between 1%-5%.
Alternatively, step 5) in ultrasonic time be 30min-60min, time of repose 30-60min.
Alternatively, step 6) centrifugation condition be 2000-3000rpm, centrifuge 15-30min,
In step 6) in centrifuge after, it is colourless to straight supernatant respectively using ethanol and deionized water washing sediment
It is transparent, the precipitation after being separated.
Alternatively, step 7) middle 50-80 DEG C of the temperature dried, 1-3h of drying time.
Beneficial effects of the present invention are：
Preparation method provided by the present invention is simple to operate, with low cost, possess the possibility largely produced.With physical method
Compare, the method for invention is simple to operate, flexible, is not limited to membrane structure, can any pattern vanadium trioxide
(such as spherical, flower-shaped, wire, bar-shaped) load gold nano grain on particle, technical process environmental protection is with low cost.Prepare
Gold-nanoparticle-supported vanadium trioxide particle have extensively in new energy (lithium battery), catalysis and food and medical domain
General application prospect.
The present invention method in, the used equal safety and environmental protection of reagent, and source be easy to get, it is with low cost, the present invention is used
Method mild condition.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is preparation manipulation scheme sketch of the invention；
Fig. 2 is the X ray diffracting spectrum of the vanadium trioxide of the gold load prepared by Example 1 and Example 2 of the present invention；
Fig. 3 is sweeping for the flower-shaped micron particles of gold-nanoparticle-supported vanadium trioxide prepared by the embodiment of the present invention 2
Retouch electromicroscopic photograph schematic diagram；
Fig. 4 is the height of the gold-nanoparticle-supported vanadium trioxide flower-like nanometer particle prepared by the embodiment of the present invention 2
The ESEM back scattering photo schematic diagram of resolution ratio；
Fig. 5 is the gold load flower-shaped micron particles of vanadium trioxide and the flower-shaped micron particles conduct of unsupported vanadium trioxide
The schematic diagram of the CO conversion of catalyst at different temperatures；
Fig. 6 is the stereoscan photograph of the flower-like structure of the vanadium trioxide particle prepared by the embodiment of the present invention 3；
Fig. 7 is the X ray diffracting spectrum signal of the flower-like structure of the vanadium trioxide particle prepared by the embodiment of the present invention 3
Figure.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
The present embodiment provides a kind of preparation method of gold-nanoparticle-supported vanadium trioxide particle, this method include with
Lower step：
01) pure substance of vanadium trioxide particle is calcined under inert gas atmosphere, activates vanadium trioxide particle
And cooled down in inert gas, the vanadium trioxide particle after the activation cooled down.
Vanadium trioxide particle in the step preferably uses the particle of flower-like structure, and purity is 99.0-99.6%.Should
Calcining heat is 300 DEG C -400 DEG C in step, and calcination time is 2-6h；
Inert gas is preferably nitrogen or argon gas.Calcine, can be avoided in barium oxide and air in inert gas
Oxygen contact is so as to oxidized.
In other embodiments, the step 01) in the particle of vanadium trioxide can also be what market was commercially available
The particle of any pattern, the present embodiment is not limited thereof.To prepare the flower-shaped particle of vanadium trioxide of gold load, preferably make
With step 01) in vanadium trioxide flower-shaped particle.
02) the vanadium trioxide particle after natural cooling in an inert atmosphere is added in deionized water, stirred,
Form suspending liquid A；
03) gold chloride is dissolved in deionized water, stirred, form chlorauric acid solution B；B moles of chlorauric acid solution is dense
Spend for 0.01-0.1mol/L；
04) chlorauric acid solution B is added to suspending liquid A, forms suspension C；
05) stood after ultrasound suspending liquid C, generation has black flocculent deposit in suspension C；
Ultrasonic time is about 30min-60min in the step, and time of repose is about 30-60min.
06) the suspension C that generation has black flocculent deposit is centrifuged, obtains sediment；
07) sediment is dried, gold-nanoparticle-supported vanadium trioxide particle, X-ray diffraction as shown in Figure 2 is obtained
Collection of illustrative plates, can will be apparent that the diffraction maximum of deposit really and vanadium trioxide.
The vanadium trioxide grain structure of gold load in the present embodiment can be self-assembly of for vanadium trioxide nanometer sheet
Flower-shaped micron particles；The particle diameter of flower-shaped micron particles is 4-5 microns, and the nanometer sheet thickness for constituting flower-shaped particle is received for 8-12
Rice；Gold nano grain is dispersed in the flower-shaped particle surface of vanadium trioxide.
Especially, vanadium trioxide nanometer sheet thickness is about 10 nanometers, and a diameter of 10-20 of gold nano grain of load receives
Rice, gold nano grain is evenly distributed on the nanometer sheet surface of vanadium trioxide.
For example, step 06) in, ethanol and deionized water washing sediment are used respectively for the sediment of separation,
To straight supernatant water white transparency, the precipitation after being separated.
Step 07) middle 50-80 DEG C of the temperature dried, dry 1-3h.
The preparation method of the present embodiment is simple to operate, with low cost, possess the possibility largely produced.With physical method phase
Than, the above method is simple to operate, flexible, is not limited to the membrane structure prepared in the prior art, can any pattern three oxygen
Change on two vanadium particles (such as spherical, flower-shaped) load gold nano grain, technical process environmental protection is with low cost.
The gold-nanoparticle-supported vanadium trioxide particle prepared by the above method is in new energy
(lithium battery), catalysis and food and medical domain have a wide range of applications.
Embodiment 2
The present embodiment provides a kind of preparation method of gold-nanoparticle-supported vanadium trioxide particle, as shown in figure 1, should
Method comprises the following steps：
11) purity of flower-like structure is calcined into 2-4h under inert gas atmosphere for 99.5% vanadium trioxide particle,
350-380 DEG C of calcining heat, activates vanadium trioxide particle, and is cooled down in inert gas, three for being activated and being cooled down
V 2 O particle；
Inert gas in the step can be nitrogen or argon gas.
12) pure substance of the vanadium trioxide particle for the 0.03g for activating and cooling down is added in deionized water, stirring is equal
It is even, form suspending liquid A；
13) gold chloride of certain mass is dissolved in deionized water, stirred, form chlorauric acid solution B；The present embodiment
Middle chlorauric acid solution B concentration is 0.01mol/L or 0.03,0.05mol/L；
14) chlorauric acid solution B at room temperature, is added to suspending liquid A, suspension C is formed；Gold rubs with vanadium in suspension C
You are maintained between 1-5% ratio, and such as mol ratio is 3%；
15) generation in 1.5h, suspension C is stood after the general 40min of ultrasound suspending liquid C black flocculent deposit；
16) the suspension C that generation has black flocculent deposit is centrifuged under the conditions of 2000-3000rpm, separated
General 25min, and the sediment separated respectively using ethanol and deionized water washing, to straight supernatant water white transparency,
Precipitation after being separated.
17) sediment is directed to, 2-3h is dried at 50-80 DEG C, obtains gold-nanoparticle-supported vanadium trioxide particle.
The low resolution stereoscan photograph of the flower-shaped micron particles of gold-nanoparticle-supported vanadium trioxide as shown in Figure 3.Fig. 4 shows
The high-resolution ESEM back scattering for having gone out the gold-nanoparticle-supported vanadium trioxide flower-like nanometer particle prepared is shone
Piece, wherein clear portions are gold nano grain.
Because the size of gold is smaller, gold grain not shown in Fig. 3.
The gold-nanoparticle-supported vanadium trioxide grain structure prepared by the method for the present embodiment is flower-shaped micron
Particle, particle diameter is 4-5 microns.Nanometer sheet thickness is about 10 in the flower-shaped micron particles that vanadium trioxide nanometer sheet is self-assembly of
Nanometer, generally in 8-12 nanometer ranges.The particle of load in the present embodiment is gold nano grain, about 10-20 nanometers of diameter.
Above-mentioned gold-nanoparticle-supported vanadium trioxide particle is widely used, it is adaptable to new energy, catalysis and food
Product and medical domain.Flower-shaped micro-nano particle has good catalysis and electric property, has very in terms of lithium battery and catalysis
Good potential application.
It is that the purity of flower-like structure is 99.5% vanadium trioxide particle due to what is preferably used in the embodiment of the present invention,
Therefore, spy is 99.5% by example 3 below and the purity that explanation prepares flower-like structure respectively of embodiment 4,5 in the present invention
The method of vanadium trioxide particle.
Embodiment 3
The flower-shaped particle of vanadium trioxide is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours in being bathed in 50 DEG C waters,
It is well mixed, suspension 0A is formed；The molar concentration of the suspension 0A is 0.075mM；
1.2) 1mL sodium bicarbonate solutions are added into suspension 0A, the color of suspension is changed into light yellow from brown color,
Suspension 0B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.5mol/L；
1.3) suspension 0B is put into autoclave and heated, heating-up temperature is 180 degrees Celsius, the heat time is 12 hours,
The predecessor containing black precipitate can be arrived after being stored at room temperature cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, dried at 50 c.Obtain the flower-shaped oxidation that nanometer sheet is self-assembly of
Vanadium predecessor.
2) preparation for the flower-shaped vanadium trioxide micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in a nitrogen atmosphere
Shape vanadium trioxide micro-nano particle.Calcining heat is 500 degrees Celsius, and calcination time is 6 hours, obtains flower-shaped vanadium trioxide micro-
Receive particle, as shown in Figure 6 and Figure 7.
Embodiment 4
The flower-like structure of vanadium trioxide particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours in being bathed in 70 DEG C waters,
It is well mixed, suspension 0A is formed；The molar concentration of the suspension 0A is 0.3mmol/L；
1.2) 10mL sodium bicarbonate solutions are added into suspension 0A, the color of suspension is changed into pale yellow from brown color
Color, forms suspension 0B, wherein, the molar concentration of the sodium bicarbonate solution is 1mol/L；
1.3) suspension 0B is put into autoclave and heated, heating-up temperature is 260 degrees Celsius, the heat time is 36 hours,
The predecessor containing black precipitate can be arrived after being stored at room temperature cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, is dried under 70 degrees Celsius.Obtain the flower-shaped oxidation that nanometer sheet is self-assembly of
Vanadium predecessor.
2) preparation for the flower-shaped vanadium trioxide micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in a nitrogen atmosphere
Shape vanadium trioxide micro-nano particle.Calcining heat is 700 degrees Celsius, and calcination time is 2 hours, obtains flower-shaped vanadium trioxide micro-
Receive particle.
Embodiment 5
The flower-like structure of vanadium trioxide particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours in being bathed in 60 DEG C waters,
It is well mixed, suspension 0A is formed；The molar concentration of the suspension 0A is 0.15mmol/L；
1.2) 5mL sodium bicarbonate solutions are added into suspension 0A, the color of suspension is changed into light yellow from brown color,
Suspension 0B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.25mol/L；
1.3) suspension 0B is put into autoclave and heated, heating-up temperature is 220 degrees Celsius, the heat time is 24 hours,
The predecessor containing black precipitate can be arrived after being stored at room temperature cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, dried at 60 c.Obtain the flower-shaped oxidation that nanometer sheet is self-assembly of
Vanadium predecessor.
2) preparation for the flower-shaped vanadium trioxide micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in a nitrogen atmosphere
Shape vanadium trioxide micro-nano particle.Calcining heat is 600 degrees Celsius, and calcination time is 4 hours, obtains flower-shaped vanadium trioxide micro-
Receive particle.
Experimental example
The gold-nanoparticle-supported vanadium trioxide that synthesis is evaluated using carbon monoxide (CO) hydrogenation reaction is flower-shaped micro-
Receive catalytic performance of the particle as catalyst, contrasted therewith using the unsupported flower-shaped micro-nano particle of vanadium trioxide.One
The Hydrogenation Experiment of carbonoxide is carried out in tubular flow reactor, and pressure is 1 atmospheric pressure, and carbon monoxide and hydrogen mol ratio are
1:3, flow velocity is every gram of catalyst of 3.0 cubic centimetres per minute.Product analysis utilizes the gas-chromatography (island with thermal conductivity detector (TCD)
Tianjin GC-8A) on-line analysis.Chromatogram column length is 2 meters, and helium is as carrier gas, and flow velocity is 30 cubic centimetres per minutes.Fig. 5 is shown
The oxidation that both the above catalyst (golden load and unsupported flower-shaped vanadium trioxide) is carried out under different catalytic temperatures
The CO conversion of carbon Hydrogenation Experiment.Shown in the Fig. 5, the flower-shaped vanadium trioxide micro-nano particle of gold load is used as an oxygen
Changing carbon hydrogenation catalyst, not only CO conversion is higher than unsupported vanadium trioxide micro-nano particle, and the catalysis of optimization
Temperature has obvious reduction (being reduced to 180 DEG C from 210 DEG C).Show to the reaction, flower-shaped the three of the gold load of this patent synthesis
V 2 O catalytic performance is higher than unsupported vanadium trioxide.
The technical principle of the present invention is described above in association with specific embodiment, these descriptions are intended merely to explain the present invention's
Principle, it is impossible to be construed to limiting the scope of the invention in any way.Based on explaining herein, those skilled in the art
Would not require any inventive effort can associate other embodiments of the present invention, and these modes fall within this hair
Within bright protection domain.
Claims (10)
1. a kind of vanadium trioxide particle of gold load, it is characterised in that
The vanadium trioxide grain structure of gold load is the flower-shaped micron particles that vanadium trioxide nanometer sheet is self-assembly of；
The particle diameter of flower-shaped micron particles is 4-5 microns, and the thickness for constituting flower-shaped particle nanometer sheet is 8-12 nanometers；
Gold nano grain is dispersed in the flower-shaped particle surface of vanadium trioxide.
2. vanadium trioxide particle according to claim 1, it is characterised in that
The flower-shaped particle of vanadium trioxide is made up of thickness for 10 nanometers of nanometer sheet self assembly, and the gold nano grain of load is a diameter of
10-20 nanometers, gold nano grain is evenly distributed on the flower-shaped particle surface of vanadium trioxide.
3. a kind of method of the vanadium trioxide particle of the gold load prepared described in claim 1 or 2, it is characterised in that including：
1) pure substance of vanadium trioxide particle is calcined under inert gas atmosphere, vanadium trioxide particle is activated and cold
But, the vanadium trioxide particle activated；
2) the activation vanadium trioxide particle after cooling is added in deionized water, stirred, form suspending liquid A；
3) gold chloride is dissolved in deionized water, stirred, form chlorauric acid solution B；
4) chlorauric acid solution B is added to suspending liquid A, forms suspension C；
5) stood after ultrasound suspending liquid C, generation has black flocculent deposit in suspension C；
6) the suspension C that generation has black flocculent deposit is centrifuged, obtains sediment；
7) sediment is dried, the vanadium trioxide particle of gold load is obtained.
4. method according to claim 3, it is characterised in that the step 1) in vanadium trioxide particle be flower-shaped knot
The particle of structure, purity is 99.0-99.6%.
5. method according to claim 3, it is characterised in that the step 1) in calcining heat be 300 DEG C -400 DEG C,
Calcination time is 2-6h；
Inert gas is nitrogen or argon gas.
6. method according to claim 3, it is characterised in that chlorauric acid solution B molar concentrations are 0.01-0.1mol/L.
7. method according to claim 3, it is characterised in that step 4) at 15-30 DEG C, add chlorine to suspending liquid A
Auric acid solution B, forms suspension C of the mol ratio of golden and vanadium between 1%-5%.
8. method according to claim 3, it is characterised in that step 5) in ultrasonic time be 30min-60min, during standing
Between 30-60min.
9. method according to claim 3, it is characterised in that step 6) centrifugation condition be 2000-3000rpm,
Centrifuge 15-30min,
In step 6) in centrifuge after, respectively using ethanol and deionized water washing sediment, to straight supernatant water white transparency,
Remove supernatant, the precipitation after being separated.
10. method according to claim 3, it is characterised in that step 7) middle 50-80 DEG C of the temperature dried, drying time
1-3h。
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