CN109759041A - A kind of hollow laminated structure titania nanotube catalysis material and preparation method thereof - Google Patents
A kind of hollow laminated structure titania nanotube catalysis material and preparation method thereof Download PDFInfo
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- CN109759041A CN109759041A CN201910166429.0A CN201910166429A CN109759041A CN 109759041 A CN109759041 A CN 109759041A CN 201910166429 A CN201910166429 A CN 201910166429A CN 109759041 A CN109759041 A CN 109759041A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention provides a kind of hollow laminated structure titania nanotube catalysis materials and preparation method thereof.The diameter of the titania nanotube is 2~3 μm, and the titania nanotube is accumulated by nanometer sheet, and nanometer sheet thickness is 10~15nm, and nanometer sheet size is 20~30nm, forms meso-hole structure between nanometer sheet.This method is with ethyl alcohol, and glycerine, ether mixed liquor is solvent, using titanyl sulfate as titanium source, passes through solvent thermal reaction and sintering forms hollow laminated structure titania nanotube catalysis material.Advantage of the invention is that preparation method is quick and easy, it is easy to produce in enormous quantities, it is repeated high, and the titania nanotube of this method preparation is accumulated by nanometer sheet, and there is high specific surface area and cellular structure abundant, photocatalytic water H2-producing capacity is excellent, and hydrogen-producing speed is 2.35 times of business P25, and catalyst is reusable.
Description
Technical field
The invention belongs to catalysis material synthesis technical fields, and in particular to a kind of hollow laminated structure nano titania
Pipe catalysis material and preparation method thereof.
Background technique
TiO2As most widely used conductor photocatalysis material, due to stable physicochemical properties, to life
The advantages that object is non-toxic, abundance, low in cost has very big excellent in terms of the photocatalytic degradation of organic and inorganic pollutant
Gesture is the environment pollution treatment material of a kind of great potential and application future.Although TiO2Have in terms of photocatalysis performance all
More advantages, and faster development has been arrived in recent years, but up to the present can't reach due to some bottlenecks of its own
The degree applied to industry, application industrially are restricted, and are even in theoretical research and experimental stage.Titanium dioxide
It is very low that problem encountered essentially consists in quantum yield.
Studies have shown that TiO2Photocatalysis performance be highly dependent on its structure.Lesser partial size and some specific shapes
State can effectively shorten electrons spread distance, photocatalytic activity can be improved.Several forms have been widely studied, have been wrapped
Include nanotube, nano wire, hollow sphere, core-shell structure etc..In particular, complicated one-dimensional hollow pipe nanostructure can be mentioned effectively
The photocatalysis performance of high material.This structure generally includes one-dimensional skeleton and hollow porous shell, due to its biggish specific surface area
And light scattering ability, there is excellent light capture ability.So the TiO with other forms2It compares, TiO2Nanotube has bigger
Specific surface area and stronger adsorption capacity, be very beneficial for improve TiO2Photocatalysis performance.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of simple process, what can be synthesized on a large scale has high catalysis
Active hollow laminated structure titania nanotube catalysis material and preparation method thereof.
The technical solution taken by the invention to solve the above technical problem are as follows:
A kind of hollow laminated structure titania nanotube catalysis material, the diameter of the titania nanotube are 2
~3 μm, the titania nanotube is accumulated by nanometer sheet, and nanometer sheet thickness is 10~15nm, and nanometer sheet size is 20
~30nm forms meso-hole structure between nanometer sheet.
The preparation method of the hollow laminated structure titania nanotube catalysis material, it the following steps are included:
(1) ethyl alcohol, glycerine and ether is taken to be added to the container, at the uniform velocity stirring 30-60min；
(2) titanium source, uniform stirring 3-4h is added into step (1) obtained solution；
(3) step (2) resulting reaction solution being transferred in reaction kettle and is reacted, reaction temperature is 100 DEG C -120 DEG C,
Insulation reaction 40-50h；
(4) it takes out reaction kettle and cooling, product is washed and dried；
(5) product after drying is calcined in Muffle furnace to get the hollow laminated structure nano titania is arrived
Pipe catalysis material.
In above scheme, the titanium source is titanyl sulfate.
In above scheme, step (5) sintering time is 2h, and sintering temperature is 600-700 DEG C.
In above scheme, it is dried after being washed repeatedly in step (4) with dehydrated alcohol at 40-60 DEG C.
In above scheme, the molar ratio of ethyl alcohol, glycerine and ether three and titanium source is 3.4~3.6:1.2 in step 1)
~1.4:0.9~1.0:0.013~0.015.
The beneficial effects of the present invention are: synthetic method is simple, at low cost, can largely synthesize, and is suitable for industrial production.
This titania nanotube material is hollow structure, specific surface area with higher and cellular structure abundant, these structures
Conducive to the transmitting of substance, so there is preferable photocatalysis performance.The hydrogen-producing speed highest of 600 DEG C of resulting samples of sintering is
70.88mmol g-1h-1, it is 2.35 times of business P25 hydrogen-producing speed.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, the attached drawing to embodiment is simply situated between below
It continues.
Fig. 1 (a) is the low resolution SEM figure of hollow laminated structure titania nanotube materials Example 1；It (b) is hollow
The high-resolution SEM of laminated structure titania nanotube materials Example 1 schemes；It (c) is hollow laminated structure nano titania
The low resolution SEM of tube material embodiment 2 schemes；(d) be hollow laminated structure titania nanotube materials Example 2 high-resolution
SEM figure；(e) be hollow laminated structure titania nanotube material comparative example 1 low resolution SEM figure；It (f) is hollow sheet knot
The high-resolution SEM of structure titania nanotube material comparative example 1 schemes；It (g) is hollow laminated structure titania nanotube material
The low resolution SEM of comparative example 2 schemes；(h) be hollow laminated structure titania nanotube material reality comparative example 2 high-resolution SEM
Figure；(i) be hollow laminated structure titania nanotube material comparative example 3 low resolution SEM figure；It (j) is hollow laminated structure
The high-resolution SEM of titania nanotube material comparative example 3 schemes.
Fig. 2 is the XRD diagram of hollow laminated structure titania nanotube material；
Fig. 3 (a) is nitrogen adsorption-desorption curve figure of hollow laminated structure titania nanotube material；It (b) is hollow
The graph of pore diameter distribution of laminated structure titania nanotube material.
Fig. 4 is the photodissociation of different sintering temperatures and business P25 before hollow laminated structure titania nanotube material sintering
Aquatic products hydrogen rate diagram.
Specific embodiment
For a better understanding of the present invention, the content that the present invention is furture elucidated with reference to the accompanying drawings and examples, but this
The content of invention is not limited solely to the following examples.
Embodiment 1
(1) 161.2g ethyl alcohol, 119.73g glycerine are taken, 66.7g ether is added in beaker.At the uniform velocity stir 30min.
(2) 2.08g titanyl sulfate, uniform stirring 3h are added into (1) obtained solution.
(3) after the completion of stirring, reaction solution is transferred in reaction kettle, and reaction temperature is 110 DEG C, insulation reaction 48h.
(4) reaction kettle is taken out from air dry oven, 60 DEG C of dryings are to be processed after product is washed three times with dehydrated alcohol.
(5) product after drying is placed in 600 DEG C of Muffle furnaces and calcines 2h to get the hollow laminated structure dioxy is arrived
Change titanium nano pipe photochemical catalyst material.
Embodiment 2
(1) 161.2g ethyl alcohol, 119.73g glycerine are taken, 66.7g ether is added in beaker.At the uniform velocity stir 30min.
(2) after 30min, 2.08g titanyl sulfate, uniform stirring 3h are added into (1) obtained solution.
(3) after the completion of stirring, reaction solution is transferred in reaction kettle, and reaction temperature is 110 DEG C, insulation reaction 48h.
(4) reaction kettle is taken out from air dry oven, 60 DEG C of dryings are to be processed after product is washed three times with dehydrated alcohol.
(5) product after drying is placed in 700 DEG C of Muffle furnaces and calcines 2h to get the hollow laminated structure dioxy is arrived
Change titanium nano pipe photochemical catalyst material.
Comparative example 1
(1) 161.2g ethyl alcohol, 119.73g glycerine are taken, 66.7g ether is added in beaker.At the uniform velocity stir 30min.
(2) after 30min, 2.08g titanyl sulfate, uniform stirring 3h are added into (1) obtained solution.
(3) after the completion of stirring, reaction solution is transferred in reaction kettle, and reaction temperature is 110 DEG C, insulation reaction 48h.
(4) reaction kettle is taken out from air dry oven, 60 DEG C of dryings are to be processed after product is washed three times with dehydrated alcohol.
(5) product after drying is placed in 400 DEG C of Muffle furnaces and calcines 2h to get the hollow laminated structure dioxy is arrived
Change titanium nano pipe photochemical catalyst material.
Comparative example 2
(1) 161.2g ethyl alcohol, 119.73g glycerine are taken, 66.7g ether is added in beaker.At the uniform velocity stir 30min.
(2) after 30min, 2.08g titanyl sulfate, uniform stirring 3h are added into (1) obtained solution.
(3) after the completion of stirring, reaction solution is transferred in reaction kettle, and reaction temperature is 110 DEG C, insulation reaction 48h.
(4) reaction kettle is taken out from air dry oven, 60 DEG C of dryings are to be processed after product is washed three times with dehydrated alcohol.
(5) product after drying is placed in 500 DEG C of Muffle furnaces and calcines 2h to get the hollow laminated structure dioxy is arrived
Change titanium nano pipe photochemical catalyst material.
Comparative example 3
(1) 161.2g ethyl alcohol, 119.73g glycerine are taken, 66.7g ether is added in beaker.At the uniform velocity stir 30min.
(2) after 30min, 2.08g titanyl sulfate, uniform stirring 3h are added into (1) obtained solution.
(3) after the completion of stirring, reaction solution is transferred in reaction kettle, and reaction temperature is 110 DEG C, insulation reaction 48h.
(4) reaction kettle is taken out from air dry oven, 60 DEG C of dryings are to be processed after product is washed three times with dehydrated alcohol.
(5) product after drying is placed in 800 DEG C of Muffle furnaces and calcines 2h to get the hollow laminated structure dioxy is arrived
Change titanium nano pipe photochemical catalyst material.
In order to study the photocatalysis performance of hollow laminated structure titanic oxide nano pipe light catalyst prepared by the present invention,
By embodiment 1 with to embodiment 2, comparative example 1, comparative example 2, hollow laminated structure nano titania prepared by comparative example 3
Pipe photochemical catalyst carries out the experiment of photodissociation aquatic products hydrogen respectively.Specific step is as follows: by embodiment 1-2, prepared by comparative example 1-3 in
Empty laminated structure titanic oxide nano pipe light catalyst 20mg is added separately to 50ml methanol and the mixing of 50ml deionized water is molten
It is added in a closed glass reactor and stirs in liquid, then after instilling 51 μ l chloroplatinic acid (10mM) ultrasonic disperses, be placed in
Under 300W xenon lamp (PLS-SXE300C, Bo Fei Lay Science and Technology Ltd.).The gas of generation passes through Agilent 7890B gas-chromatography
Instrument analysis, it is 19A that source current is arranged when turning on light, and every mistake takes a point for 1 hour, takes 5 points altogether.
Fig. 1 is the electron-microscope scanning figure for the hollow laminated structure titania nanotube material prepared, can from Fig. 1 (a)
To find out, TiO prepared by embodiment 12The diameter of nanotube is hollow structure at 2 μm or so, and titania nanotube is
It is accumulated by the nanometer sheet that thickness is about 10nm, nanometer sheet size is than more uniform, as shown in Fig. 1 (b).With sintering temperature
It is continuously improved, smooth nanometer is gradually converted into the nano particle that diameter is about 10nm, as shown in Fig. 1 (f).Fig. 2 is XRD diagram,
It can be seen from the figure that TiO prepared by embodiment 12Nanotube is pure Anatase.TiO prepared by embodiment 22Nanotube
Middle a small amount of Rutile Type occur, titanium ore type Titanium Dioxide activity is higher than brilliant red stone.When sintering temperature is 400 DEG C, gained
Titanium dioxide is unformed phase, i.e. comparative example 1, and unformed titanium dioxide is almost without catalytic activity.Sintering temperature is 500 DEG C
When, crystallinity is not high, and there are part amorphous phases, i.e. comparative example 2.When sintering temperature is 800 DEG C, gained nano titania
Pipe is anatase and rutile compound phase.Fig. 3 is the nitrogen adsorption curve graph of hollow laminated structure titania nanotube material
And graph of pore diameter distribution, it is wherein adsorption desorption curve in left figure, right figure is graph of pore diameter distribution.1 institute of embodiment known to test result
The specific surface area of catalyst obtained is 68.29m2·g-1, average pore size 26.08nm, it was demonstrated that a process for preparing tools
There is the hollow laminated structure titania nanotube material of high specific surface area.Fig. 4 is hollow laminated structure nano titania
The photocatalytic water H2-producing capacity figure of tube material, as can be seen from the figure the hydrogen-producing speed highest of the resulting catalyst of embodiment 1 are
70.88mmol g-1h-1, rate is 2.35 times of business P25.Catalyst hydrogen-producing speed prepared by embodiment 2 is
47.56mmol g-1h-1, equally it is higher than (the 0.63mmol g of comparative example 1-1h-1), (the 10.87mmol g of comparative example 2-1h-1), comparison
(the 30.77mmol g of example 3-1h-1) prepared by catalyst and business P25 (30.16).This is because when sintering temperature is from 400 liters
When to 600 DEG C, material crystalline degree is continuously improved, therefore photolysis water hydrogen performance is continuously improved.But when sintering temperature is higher than 600 DEG C,
Making the photolysis water hydrogen performance of sample can decline instead.This, which is that sintering temperature is excessively high, causes a nanometer chip architecture to start (such as Fig. 1 that collapses
(d) shown in), specific surface area is substantially reduced, and material surface active site is reduced, and nanometer sheet structure collapses, also will affect object
The transmission of matter, so causing the hydrogen-producing speed of catalyst reduces.Table 1 is the ratio of hollow laminated structure titania nanotube material
Surface area and pore size.
Table 1
| Sintering temperature (DEG C) | Specific surface area (m2·g-1) | Pore size (nm) |
| Embodiment 1 | 68.29 | 26.08 |
| Embodiment 2 | 45.15 | 36.12 |
| Comparative example 1 | 84.14 | 23.58 |
| Comparative example 2 | 72.85 | 24.44 |
| Comparative example 3 | 29.92 | 31.91 |
It should be noted that those skilled in the art should understand that, technical solution of the present invention can be carried out
Modification or equivalent replacement should all cover and want in right of the invention without departing from the objective and range of technical solution of the present invention
It asks in range.
Claims (6)
1. a kind of hollow laminated structure titania nanotube catalysis material, which is characterized in that the titania nanotube
Diameter be 2~3 μm, the titania nanotube is accumulated by nanometer sheet, nanometer sheet thickness be 10~15nm, nanometer sheet
Size is 20~30nm, forms meso-hole structure between nanometer sheet.
2. the preparation method of hollow laminated structure titania nanotube catalysis material as described in claim 1, feature
Be, it the following steps are included:
(1) ethyl alcohol, glycerine and ether is taken to be added to the container, at the uniform velocity stirring 30-60min；
(2) titanium source, uniform stirring 3-4h is added into step (1) obtained solution；
(3) step (2) resulting reaction solution is transferred in reaction kettle and is reacted, reaction temperature is 100 DEG C -120 DEG C, heat preservation
React 40-50h；
(4) it takes out reaction kettle and cooling, product is washed and dried；
(5) product after drying is calcined in Muffle furnace to get the hollow laminated structure titania nanotube light is arrived
Catalysis material.
3. preparation method as claimed in claim 2, it is characterised in that: the titanium source is titanyl sulfate.
4. preparation method as claimed in claim 2, it is characterised in that: step (5) sintering time is 2h, and sintering temperature is
600-700℃。
5. preparation method as claimed in claim 2, it is characterised in that: in 40- after being washed repeatedly in step (4) with dehydrated alcohol
60 DEG C of drying process.
6. preparation method as claimed in claim 2, it is characterised in that: ethyl alcohol, glycerine and ether three and titanium in step 1)
The molar ratio in source is 3.4~3.6:1.2~1.4:0.9~1.0:0.013~0.015.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111675429A (en) * | 2020-06-10 | 2020-09-18 | 哈尔滨工业大学 | Chromium-containing tannery wastewater treatment method based on photocatalytic advanced reduction |
| CN112588283A (en) * | 2020-11-25 | 2021-04-02 | 内江师范学院 | Carbon quantum dot/mesoporous layered titanium dioxide and preparation method and application thereof |
| CN113171778A (en) * | 2021-04-21 | 2021-07-27 | 太原煤炭气化(集团)有限责任公司 | Deep purification desulfurizer for coke oven gas and preparation method and application thereof |
| CN113559833A (en) * | 2021-07-07 | 2021-10-29 | 武汉工程大学 | Hollow structure Na4TiO4Base nanosheet assembly, nanosheet derivative, and preparation method and application thereof |
| CN114560498A (en) * | 2022-03-10 | 2022-05-31 | 北京建筑材料检验研究院有限公司 | Method for preparing titanium dioxide with hollow rod-like structure |
| CN117886353A (en) * | 2024-03-15 | 2024-04-16 | 陕西燃气集团富平能源科技有限公司 | Method for preparing defective TiO by biological template method 2 Method for manufacturing micro-tube and defective TiO 2 Micro-tube and application thereof |
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| CN111675429A (en) * | 2020-06-10 | 2020-09-18 | 哈尔滨工业大学 | Chromium-containing tannery wastewater treatment method based on photocatalytic advanced reduction |
| CN112588283A (en) * | 2020-11-25 | 2021-04-02 | 内江师范学院 | Carbon quantum dot/mesoporous layered titanium dioxide and preparation method and application thereof |
| CN112588283B (en) * | 2020-11-25 | 2023-05-23 | 内江师范学院 | Carbon quantum dot/mesoporous Kong Cengzhuang titanium dioxide and preparation method and application thereof |
| CN113171778A (en) * | 2021-04-21 | 2021-07-27 | 太原煤炭气化(集团)有限责任公司 | Deep purification desulfurizer for coke oven gas and preparation method and application thereof |
| CN113171778B (en) * | 2021-04-21 | 2023-02-17 | 太原煤炭气化(集团)有限责任公司 | Deep purification desulfurizer for coke oven gas and preparation method and application thereof |
| CN113559833A (en) * | 2021-07-07 | 2021-10-29 | 武汉工程大学 | Hollow structure Na4TiO4Base nanosheet assembly, nanosheet derivative, and preparation method and application thereof |
| CN114560498A (en) * | 2022-03-10 | 2022-05-31 | 北京建筑材料检验研究院有限公司 | Method for preparing titanium dioxide with hollow rod-like structure |
| CN117886353A (en) * | 2024-03-15 | 2024-04-16 | 陕西燃气集团富平能源科技有限公司 | Method for preparing defective TiO by biological template method 2 Method for manufacturing micro-tube and defective TiO 2 Micro-tube and application thereof |
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