CN105923654B - A kind of vanadium trioxide micro-nano particle and preparation method thereof - Google Patents
A kind of vanadium trioxide micro-nano particle and preparation method thereof Download PDFInfo
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- CN105923654B CN105923654B CN201610268807.2A CN201610268807A CN105923654B CN 105923654 B CN105923654 B CN 105923654B CN 201610268807 A CN201610268807 A CN 201610268807A CN 105923654 B CN105923654 B CN 105923654B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/36—Spheres fragmented
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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
Abstract
The invention provides a kind of micro-nano particle, the micro-nano particle is vanadium trioxide micro-nano particle, is self-assembly of by nanometer sheet.Present invention also offers the preparation method of the micro-nano particle, it the described method comprises the following steps and 1) add vanadic anhydride in ethylene glycol, stirring is well mixed it, forms suspending liquid A；2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；3) suspension B is heated, cooling is stored at room temperature afterwards, the predecessor containing black precipitate is obtained；4) by step 3) mixed solution containing the predecessor that is formed centrifuges, washs and dry, obtain the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of；5) by step 4) obtained predecessor calcines in a nitrogen atmosphere, obtains the micro-nano particle.The barium oxide micro-nano particle of the present invention has very high specific surface area, and stronger structural stability contributes to it as the raising of electricity material and catalyst performance.
Description
Technical field
The present invention relates to field of nanometer technology, in particular to a kind of micro-nano particle and its preparation method and application.
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.It is well known that the property and application performance of nano material
Depend greatly on the pattern and size of its particle.And the pattern and size of particle often have with synthetic method and path
Close contact.The flower-shaped micro-nano particle that nanometer sheet is self-assembly of, because it has three-dimensional structure, using the teaching of the invention it is possible to provide more
Adsorption potential, so as to preferably be contacted with each other with gas, have outstanding performance in catalytic field.Flower on nanometer sheet self assembly
Shape micro-nano particle, there is some reports at present.Method is concentrated mainly on following two：(1) vanadyl acetylacetonate is dissolved in 20 milliliters
In ethanol, 30 milliliters of hydrogen peroxide are added afterwards.Liquid mixed above is placed in 150 DEG C of autoclaves and heated 24 hours.By what is obtained
Precipitation separation is calcined 2 hours after drying under 400 DEG C of nitrogen, can obtain the pattern vanadium trioxide particle.(2) by ammonium metavanadate
It is dissolved in 50 ml deionized waters, system pH is adjusted to 2 using nitric acid, and stirred at 50 DEG C until there is orange precipitation.
20 ml methanols are added into above solution, 24 hours are stood at room temperature.Precipitation becomes to be isolated washing during darkorange.The deep orange
Color precipitation is the vanadium oxide particles of floriform appearance.Afterwards, at a certain temperature (such as 600 DEG C) under reducing atmosphere
(such as hydrogen) calcines the particle, can obtain three vanadium oxides of similar pattern.The pattern and above-mentioned three of other method synthesis
V 2 O particle has obvious difference, such as sea urchin shape vanadium trioxide micron particles.
Above method cost of material is higher, and method is complicated, and product has spent acid generation, and inadequate environmental protection is not suitable for big rule
Mould is produced, and huge inconvenience is brought to follow-up use.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of micro-nano particle, and the micro-nano particle has lamella nanostructured simultaneously
With flower-shaped spherical flower-shaped micrometer structure.
The second object of the present invention is to provide a kind of preparation method of the micro-nano particle, this method is simple to operate, into
This cheap, safety and environmental protection, can be with large-scale application in actual production.
The third object of the present invention is the application for providing the micro-nano particle, and the micro-nano particle has a wide range of application
It is general, it is adaptable in new energy, catalysis and food and medical domain.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
One aspect of the invention is related to a kind of micro-nano particle, and the micro-nano particle is vanadium trioxide micro-nano particle, by receiving
Rice piece is self-assembly of.
The micro-nano particle formed is assembled by nanometer sheet has micron-sized macro-size, meanwhile, its surface area ratio is common
Micro-nano particle is much larger, therefore its adsorption area is very big.
Preferably, the micro-nano particle is flower-shaped micro-nano particle.
Flower-shaped micro-nano particle has good catalysis and electric property, and it has good in terms of lithium battery and catalysis
Potential application.
Another aspect of the present invention is related to the preparation method of described micro-nano particle, the described method comprises the following steps：
1) vanadic anhydride is added in ethylene glycol, stirring is well mixed it, forms suspending liquid A；
2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；
Adding sodium carbonate liquor can promote in subsequent reactions, and the oxyvanadium compound of sheet is flower-shaped by being self-assembly of
Micro-nano particle.
3) suspension B is heated, cooling is stood at room temperature afterwards, obtains the predecessor containing black precipitate；
Heat suspension so that vanadic anhydride is dissolved in ethylene glycol, and chemically reacts therewith, generate sheet output.
4) by step 3) mixed solution containing the presoma that is formed centrifuges, washs and dry, received
The flower-shaped vanadium oxide predecessor that rice piece is self-assembly of.
5) by step 4) obtained predecessor calcines under inert gas atmosphere, obtains the micro-nano particle.
Calcined in inert gas, barium oxide can be avoided to be contacted with the oxygen in air so as to be oxidized, while before
The high price vanadium ion in particle can be reduced by driving the reducibility gas discharged in thing in heating, so that it is micro- to obtain vanadium trioxide
Receive particle.
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.
Preferably, the step 1) in stirring carried out in 50-70 DEG C of water-bath, five oxygen described in the suspending liquid A
It is 0.075-0.3mM to change two vanadium relative to the molar concentration of ethylene glycol.
The excessive concentration of vanadic anhydride can cause the micro-nano particle formed in subsequent reactions excessive, and its concentration it is too low when
Then it can lead to not to form particle.
Preferably, the molar concentration of the sodium bicarbonate solution is 1-1.5M.
Preferably, the step 2) in sodium bicarbonate solution addition be 1-10ml/16mL suspension.
Sodium acid carbonate concentration is 1-1.5M, when addition is 1-10ml, and it promotes the ability of flower-shaped micro-nano particle generation most
By force.
Preferably, the step 3) in, the suspension B is heated to 180-260 DEG C, and the heat time is 12-36 hours.
Heating is preferably carried out under elevated pressure conditions, therefore suspension B can be heated to 180-260 DEG C, be added with the temperature
Hot suspension can cause vanadic anhydride to be dissolved in ethylene glycol, and concurrent biochemical reaction, the sheet of generation barium oxide is sunk
Form sediment.
Preferably, the step 4) in, washed using ethanol and deionized water, the drying is under conditions of 50-80 DEG C
Carry out.
Preferably, the temperature of the calcining is 500-700 DEG C, and calcination time is 2-6 hours.
The calcining heat of 500-700 DEG C of selection, can cause presoma to be sintered into vanadium trioxide completely, while not breaking
The flower-shaped configuration of surface of bad generated micro-nano particle.
Another aspect of the present invention is related to application of the micro-nano particle in new energy, catalysis, food and medical domain.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention synthesizes the flower-shaped micro-nano particle forerunner that nanoscale twins are self-assembly of in ethylene glycol solution first
Thing.
(2) the barium oxide micro-nano particle after being formed has very high specific surface area, and stronger structural stability.This meeting
Contribute to it as the raising of battery material and catalyst performance.
(3) the flower-shaped barium oxide particle that nanometer sheet is self-assembly of is provided simultaneously with lamella nanostructured and flower-shaped class
Spherical micrometer structure.Lamella nanostructured plays a leading role to application function, and flower-shaped spherical micrometer structure contributes to device figure
The assembling of layer.
(4) preparation method for the flower-shaped micro-nano particle that nanometer sheet provided by the present invention is self-assembly of it is simple to operate, into
Sheet is cheap, possess the possibility largely produced, has in new energy (lithium battery), catalysis and food and medical domain and widely should
Use prospect.
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 flower-shaped vanadium oxide micro-nano predecessor scanning that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
Electromicroscopic photograph.
Fig. 3 is the flower-shaped vanadium trioxide micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of.
Fig. 4 is the X-ray for the flower-shaped predecessor micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
Diffracting spectrum.
Fig. 5 is the X for the flower-shaped vanadium trioxide micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
X ray diffraction collection of illustrative plates.
The flower-shaped vanadium trioxide that nanometer sheets of the Fig. 6 prepared by the embodiment of the present invention 1 is self-assembly of is as an oxidation
The CO conversion of the catalyst of carbon hydrogenation reaction with reaction temperature relation.
Specific 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
Micro-nano 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, makes it in being bathed in 50 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.075mM；
1.2) 1mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.5M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 180 DEG C, and the heat time is 12 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting 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 at 50 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
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 DEG C, and calcination time is 6 hours.
Embodiment 2
Micro-nano 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, makes it in being bathed in 70 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.3mM；
1.2) 10mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 260 DEG C, and the heat time is 36 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting 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 at 70 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
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 DEG C, and calcination time is 2 hours.
Embodiment 3
Micro-nano 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, makes it in being bathed in 60 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.15mM；
1.2) 5mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.25M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 220 DEG C, and the heat time is 24 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting 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 at 60 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
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 DEG C, and calcination time is 4 hours.
Embodiment 4
Micro-nano 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, makes it in being bathed in 60 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.2mM；
1.2) 7mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.3M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 200 DEG C, and the heat time is 24 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting 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 at 60 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
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 650 DEG C, and calcination time is 4 hours.
Experimental example
The flower-shaped micro-nano particle of vanadium trioxide for evaluating synthesis by the use of carbon monoxide (CO) hydrogenation reaction is used as catalyst
Catalytic performance, contrasted therewith using sea urchin shape vanadium trioxide micro-nano particle.The Hydrogenation Experiment of carbon monoxide is in tubular type
Carried out in flow reactor, pressure is 1 atmospheric pressure, carbon monoxide and hydrogen mol ratio are 1:3, flow velocity is 3.0 cubic centimetres
Every gram of catalyst is per minute.Product analysis utilizes gas-chromatography (Shimadzu GC-8A) on-line analysis with thermal conductivity detector (TCD).Chromatogram
Column length is 2 meters, and helium is as carrier gas, and flow velocity is 30 cubic centimetres per minutes.Fig. 6 show both the above catalyst (it is flower-shaped and
Sea urchin shape vanadium trioxide) carried out under different catalytic temperatures co hydrogenation experiment CO conversion.The figure
Shown, flower-shaped vanadium trioxide micro-nano particle is as the CO conversion of carbon monoxide hydrogenation agent than sea urchin shape three
V 2 O micro-nano particle is high, shows that the flower-shaped vanadium trioxide catalytic performance of this patent synthesis is than sea urchin shape three to the reaction
V 2 O is high.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (9)
1. a kind of vanadium trioxide micro-nano particle, it is characterised in that the micro-nano particle is that flake nano structure is self-assembly of
Flower-shaped particle, the particle diameter of the micro-nano particle is 4-5 micron, and specific surface area is 56.4 square metres every gram, the micro-nano particle
The lamellar structure thickness of the middle flower-shaped particle of composition is 10 nanometers, and purity is 99.5%, and essential element is trivalent vanadium and divalent oxygen element；
The micro-nano particle is prepared by the following method：
1) vanadic anhydride is added in ethylene glycol, stirring is well mixed it, forms suspending liquid A；
2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；
3) heat suspension B, after be stored at room temperature cooling, obtain the predecessor containing black precipitate；
4) by step 3) mixed solution containing the predecessor that is formed centrifuges, washs and dry, obtain nanometer sheet
The flower-shaped vanadium oxide predecessor being self-assembly of；
5) by step 4) obtained predecessor calcines under inert gas atmosphere, obtains the micro-nano particle.
2. the preparation method of the micro-nano particle described in claim 1, it is characterised in that the described method comprises the following steps：
1) vanadic anhydride is added in ethylene glycol, stirring is well mixed it, forms suspending liquid A；
2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；
3) heat suspension B, after be stored at room temperature cooling, obtain the predecessor containing black precipitate；
4) by step 3) mixed solution containing the predecessor that is formed centrifuges, washs and dry, obtain nanometer sheet
The flower-shaped vanadium oxide predecessor being self-assembly of；
5) by step 4) obtained predecessor calcines under inert gas atmosphere, obtains the micro-nano particle.
3. method according to claim 2, it is characterised in that the step 1) in stirring in 50-70 DEG C of water-bath
Carry out, vanadic anhydride described in the suspending liquid A is 0.075-0.3mM relative to the molar concentration of ethylene glycol.
4. method according to claim 2, it is characterised in that the molar concentration of the sodium bicarbonate solution is 1-1.5M.
5. method according to claim 2, it is characterised in that the step 2) in the addition of sodium bicarbonate solution be 1-
10mL/16ml suspension.
6. method according to claim 2, it is characterised in that the step 3) in, the suspension B is heated to 180-
260 DEG C, the heat time is 12-36 hours.
7. method according to claim 2, it is characterised in that the step 4) in, washed using ethanol and deionized water,
The drying is carried out under conditions of 50-80 DEG C.
8. method according to claim 2, it is characterised in that the temperature of the calcining is 500-700 DEG C, calcination time is
2-6 hours.
9. method according to claim 2, it is characterised in that the inert gas is nitrogen or argon gas.
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