CN109879315A - A kind of porous hexagon nano-titanium dioxide of two-dimensional layer and its preparation method and application - Google Patents
A kind of porous hexagon nano-titanium dioxide of two-dimensional layer and its preparation method and application Download PDFInfo
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- CN109879315A CN109879315A CN201910280202.9A CN201910280202A CN109879315A CN 109879315 A CN109879315 A CN 109879315A CN 201910280202 A CN201910280202 A CN 201910280202A CN 109879315 A CN109879315 A CN 109879315A
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Abstract
The invention discloses porous hexagon nano-titanium dioxides of a kind of two-dimensional layer and its preparation method and application, prepare layered porous hexagon TiO using simple step heating2, with two-dimensional nano sheet TiSe2Powder is raw material, using Muffle furnace or warm table as heating equipment, by simply heating the hexagon TiO that can be obtained pure two-dimensional layer and have porous nanometer structure2.Compared with traditional P25 nano-powder, under identical light application time, P25 degrades 51.3%, and prepared TiO282.9% is degraded, therefore there is more excellent catalytic degradation ability.Equipment of this method without complexity, thus it is easy, efficient, repeated high, and it is not related to harmful reagent, and it is safe to the human body, it is harmless, particularly suitable for industrialized mass production.
Description
Technical field
The invention belongs to field of nano material preparation, while being related to Application of micron in photocatalysis field, and in particular to
A kind of porous hexagon nano-titanium dioxide of two-dimensional layer and its preparation method and application.
Background technique
Nano-TiO2It is a kind of very important semiconductor material.It has chemical stabilization, very strong anti-oxidant-reduction
Property, it is anticorrosive, it is nontoxic the advantages that, have become functional material important in development of modern industry.It is in battery, gas sensor,
Photocatalysis, electronic component, the fields such as high-end cosmetics all have especially important status.Especially in photocatalysis field,
It can will be degraded into nontoxic substance to human body and the harmful industrial wastewater of environment and dyestuff under the irradiation of sunlight.
So gradually becoming a typical representative species in photocatalysis field titanium dioxide.The titanium dioxide of nanosizing has higher
Specific surface area can effectively improve light-catalysed performance.The production technology of nano-titanium dioxide has especially important thus
Economic value, for example the P25 nano particle of Germany's production is to use a kind of nanometer of more oxide/titanium dioxide currently on the market.Mirror
In the learning value and economic value of nano-titanium dioxide, countries in the world carry out extensive and deep grind for nano-titanium dioxide
Study carefully.
Up to the present various nano-titanium dioxide preparation methods are had been developed that.It mainly include sol-gel
Method, flame hydrolysis, water-in-oil microemulsion method, chemical vapour deposition technique, solvent-thermal method and hydro-thermal method etc..Prepared pattern packet
Include graininess, rodlike, sheet, threadiness, tubulose, hollow ball-shape.Every kind of method has respective advantage and disadvantage, but regrettably,
It yet there are no the related porous hexagon nano-TiO of two-dimensional layer2Relevant report.The porous hexagon nano-TiO of two-dimensional layer2It is excellent
It puts and is to provide a kind of flake porous nanostructure being cross-linked with each other, both prevented the reunion of three-dimensional between particle, also favorably
It is efficiently separated in photo-generate electron-hole pairs, to improve its photocatalysis performance.So developing and a kind of preparing two-dimensional layer
The porous hexagon nano-TiO of shape2Process seem particularly important, also can for research prepare novel sun optical drive TiO2
Photochemical catalyst and its efficient light degradation property provide a kind of material base.
Summary of the invention
The purpose of the present invention is to provide porous hexagon nano-titanium dioxide of a kind of two-dimensional layer and preparation method thereof, with
Overcome defect of the existing technology, the present invention obtains two dimension by a kind of technique of the porous hexagon self-template of two-dimensional layer
The nano-TiO of layered porous hexagon2Special appearance and structure, the porous hexagon of the two-dimensional layer of this nanosizing can have
Improve TiO in effect ground2Catalytic degradation performance under visible light illumination.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer, by forerunner's body plate shape TiSe2It is placed on and adds
In hot equipment, under the conditions of being passed through the mixed gas of air and inert gas, presoma is subjected to heating reaction, reaction terminates
Afterwards, it is down to room temperature and obtains white powder, i.e. two-dimensional layer nanoporous shape hexagon TiO2。
Further, the heating equipment is Muffle furnace or warm table.
Further, the inert gas is nitrogen or argon gas.
Further, the gas flow for being passed through air is 10-100mL/min.
Further, the gas flow for being passed through inert gas is 10-200mL/min.
Further, heating reaction specifically: presoma is heated to 300-500 DEG C, is then kept the temperature, soaking time 1-
5h。
A kind of porous hexagon nano-titanium dioxide of two-dimensional layer, is received using a kind of above-mentioned porous hexagon of two-dimensional layer
The preparation method of rice titanium dioxide is made.
A kind of application of the porous hexagon nano-titanium dioxide of two-dimensional layer in photocatalysis.
Further, specially degradation of the porous hexagon nano-titanium dioxide of two-dimensional layer to rhodamine B.
Compared with prior art, the invention has the following beneficial technical effects:
With existing preparation TiO2Method compare, presoma need to be only put into heating by the high-temperature heating method that the present invention uses
It is heated in instrument, the porous hexagon nano-TiO of two-dimensional layer can be obtained by the heating of one-step method2.With other
The method of report compares, and this method is especially easy, efficient, safe, is also particularly well-suited for industrialized mass production, prepares
The mixed gas of air and inert gas is used in the process, on the other hand oxygen atom needed on the one hand providing product provides one
The environment of kind relative inertness, is unlikely to so that reaction is too fast, a very big advantage of the invention is prepared TiO2It can
Perfection retains the profile of presoma, forms vesicular texture, and this method operability, and repeatability is good, of the invention
The TiO arrived2It can be in battery, gas sensor, photocatalysis, electronic component device for the cellular lamellar structure with hexagonal shape
Part, the fields such as high-end cosmetics all have potential application.
With it is existing it has been reported that various preparation methods compare, process of the present invention is not a simple heat erosion
Journey, but it is related to the chemical reaction on surface.Using two selenizing titanium compounds in the case where increasing temperature, selenium atom is easy to move
The surface of nano-sheet is moved on to, oxygen fully replaces selenium atom, to complete from two selenizing titaniums to titanium oxide
The transformation of crystal structure.What is particularly worth mentioning is that the two selenizing titanium of nanometer of sheet not only mentions in entire chemical reaction process
Exchange with oxygen atom for selenium atom, a kind of template in situ is also provided.As silkworm eats mulberry leaf, receiving for part is left
Metre hole hole remains the profile of two selenizing titanium template two-dimensional layers.
Obtained TiO of the invention2For the cellular lamellar structure with hexagonal shape and there is single-phase crystal knot
Structure, photocatalysis performance is better than used P25 on the market.
Detailed description of the invention
Fig. 1 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 1 obtains2XRD spectrum；
Fig. 2 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 1 obtains2SEM photograph；
Fig. 3 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 1 obtains2Visible absorption picture；
Fig. 4 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 1 obtains2To the degradation rate picture of rhodamine B；
Fig. 5 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 2 obtains2XRD spectrum；
Fig. 6 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 2 obtains2SEM photograph；
Fig. 7 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 3 obtains2XRD spectrum；
Fig. 8 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 3 obtains2SEM photograph；
Fig. 9 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 4 obtains2XRD spectrum；
Figure 10 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 4 obtains2SEM photograph；
Figure 11 is the porous hexagon nano-TiO of two-dimensional layer that embodiment 5 obtains2XRD spectrum.
Specific embodiment
Embodiments of the present invention are described in further detail below:
The TiO of the cellular lamellar structure of hexagonal shape of the invention2Synthesis is related to following procedure:
Firstly, by powder TiSe2Presoma is placed in Muffle furnace or warm table, in the mixed gas of air and inert gas
In heated, inert gas includes nitrogen or argon gas, and when being passed through mixed gas, the flow of inert gas is 10-200mL/
Min, air gas flow 10-100mL/min；Then setting heating temperature is 300-500 DEG C, soaking time 1-5h；Reaction knot
Shu Hou cools to room temperature with the furnace, and the TiO of the cellular lamellar structure with hexagonal shape can be obtained2。
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
Firstly, pouring into TiSe in silica crucible2Powder places it on warm table；Then, it is passed through nitrogen flow
80mL/min, air mass flow 20mL/min, setting heating temperature is 500 DEG C, soaking time 2h, after reaction, cold with furnace
But to room temperature, white powder is target product TiO2。
Fig. 1 is the TiO grown according to embodiment 12The X-ray diffraction spectrum of nanometer sheet, free from admixture peak occur, illustrate to produce
Object is for pure TiO2。
Fig. 2 is the TiO grown according to embodiment 12SEM pattern photo, it can be seen that TiO2With apparent six
Side shape profile, surface are Nanoparticulate.
Fig. 3 is the visible absorption picture of embodiment 1, with the increase of visible light application time, hence it is evident that sees that absorption peak exists
It decreases, shows that Rh B is constantly being degraded.
Fig. 4 is the absorptivity picture of embodiment 1, is calculated it is found that in 40min, under visible light, with TiO2For catalyst
Degradation rate to rhodamine B is 82.9%, and commercialized P25 only degrades 51.3%, illustrates prepared TiO2Have excellent
Catalytic degradation ability.
Embodiment 2
TiSe is poured into silica crucible2Powder places it on warm table；Being passed through argon flow is 30mL/min；It is empty
Throughput 10mL/min, setting heating temperature are 300 DEG C, soaking time 1h, after reaction, cool to room temperature with the furnace, white
Toner body is target product TiO2。
Fig. 5 is the TiO grown by embodiment 22X-ray diffraction spectrum, free from admixture peak occur, it is pure for illustrating that product is
TiO2。
Fig. 6 is the corresponding TiO of embodiment 22SEM pattern photo, it can be seen that stratiform superposition hexagon TiO2On have
Apparent particle and hole.
Embodiment 3
TiSe is poured into silica crucible2Powder places it on warm table；Being passed through nitrogen flow is 10mL/min；It is empty
Throughput 100mL/min, setting heating temperature are 450 DEG C, soaking time 5h, after reaction, cool to room temperature with the furnace, white
Toner body is target product TiO2。
Fig. 7 is the TiO grown by embodiment 32X-ray diffraction spectrum, free from admixture peak occur, it is pure for illustrating that product is
TiO2, and crystallinity is good.
Fig. 8 is the TiO grown by embodiment 32The SEM pattern photo of nanometer sheet.
Embodiment 4
TiSe is poured into silica crucible2Powder places it in Muffle furnace；The gas flow for being passed through argon gas is 200mL/
min；Air mass flow 70mL/min, setting heating temperature are 350 DEG C, and heating rate is 10 DEG C/min, soaking time 2h；Reaction
After, cool to room temperature with the furnace, white powder is target product TiO2。
Fig. 9 is the XRD diagram of 4 gained sample of embodiment.
Figure 10 is that the SEM of 4 gained sample of embodiment schemes, TiO2Hexagonal sheet.
Embodiment 5
TiSe is poured into silica crucible2Powder places it in Muffle furnace；The gas flow for being passed through nitrogen is 150mL/
min；Air mass flow 50mL/min, setting heating temperature are 300 DEG C, and heating rate is 10 DEG C/min, soaking time 3.5h；Instead
After answering, room temperature is cooled to the furnace, white powder is target product TiO2。
Figure 11 is the TiO grown according to embodiment 52X-ray diffraction spectrum, free from admixture peak occur, illustrate that product is
For pure TiO2。
Claims (9)
1. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer, which is characterized in that by forerunner's body plate shape
TiSe2It is placed in heating equipment, under the conditions of being passed through the mixed gas of air and inert gas, presoma heat anti-
It answers, after reaction, is down to room temperature and obtains white powder, i.e. two-dimensional layer nanoporous shape hexagon TiO2。
2. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 1, feature
It is, the heating equipment is Muffle furnace or warm table.
3. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 1, feature
It is, the inert gas is nitrogen or argon gas.
4. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 1, feature
It is, the gas flow for being passed through air is 10-100mL/min.
5. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 1, feature
It is, the gas flow for being passed through inert gas is 10-200mL/min.
6. a kind of preparation method of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 1, feature
It is, heating reaction specifically: presoma is heated to 300-500 DEG C, is then kept the temperature, soaking time 1-5h.
7. a kind of porous hexagon nano-titanium dioxide of two-dimensional layer, which is characterized in that using described in any one of claim 1-6
A kind of porous hexagon nano-titanium dioxide of two-dimensional layer preparation method be made.
8. a kind of application of porous hexagon nano-titanium dioxide of two-dimensional layer as claimed in claim 7 in photocatalysis.
9. application of the porous hexagon nano-titanium dioxide of two-dimensional layer according to claim 8 in photocatalysis, special
Sign is, degradation of the porous hexagon nano-titanium dioxide of two-dimensional layer to rhodamine B.
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| CN1868582A (en) * | 2006-06-02 | 2006-11-29 | 安徽大学 | Nanometer titanium dioxide/selenium dioxide composition and its prepn. method |
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| CN104085920A (en) * | 2014-07-09 | 2014-10-08 | 河海大学 | Preparation method for two-dimensional sheet-shaped titanium dioxide nanosheet material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN105642262A (en) * | 2016-02-04 | 2016-06-08 | 梁书齐 | Two-dimensional-layered titanium-dioxide nanometer photocatalytic material and preparing method |
| CN108439353A (en) * | 2018-05-10 | 2018-08-24 | 陕西科技大学 | Single-phase two selenizings titanium nanometer sheet and its method and purposes prepared by a kind of solwution method |
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- 2019-04-09 CN CN201910280202.9A patent/CN109879315B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1868582A (en) * | 2006-06-02 | 2006-11-29 | 安徽大学 | Nanometer titanium dioxide/selenium dioxide composition and its prepn. method |
| CN103489651A (en) * | 2013-09-03 | 2014-01-01 | 上海师范大学 | Preparing method for embellish titanium dioxide nanotube array electrode material embellished by cadmium selenide nano-particles |
| CN104085920A (en) * | 2014-07-09 | 2014-10-08 | 河海大学 | Preparation method for two-dimensional sheet-shaped titanium dioxide nanosheet material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN105642262A (en) * | 2016-02-04 | 2016-06-08 | 梁书齐 | Two-dimensional-layered titanium-dioxide nanometer photocatalytic material and preparing method |
| CN108439353A (en) * | 2018-05-10 | 2018-08-24 | 陕西科技大学 | Single-phase two selenizings titanium nanometer sheet and its method and purposes prepared by a kind of solwution method |
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