CN105148965B - A kind of TiO2/WO3/g-C3N4Full meso-porous nano fiber - Google Patents
A kind of TiO2/WO3/g-C3N4Full meso-porous nano fiber Download PDFInfo
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Abstract
The present invention relates to a kind of TiO2/WO3/g‑C3N4Full meso-porous nano fiber, TiO in the nanofiber2/WO3With TiO2/WO3Form of nanofibers exists, g-C3N4It is supported on TiO2/WO3On nanofiber, wherein TiO2/WO3Nanofiber has porous structure, and porous structure includes mesoporous.TiO of the present invention2/WO3/g‑C3N4Stable structure, the specific surface area of full meso-porous nano fiber are high.
Description
Technical field
The present invention relates to a kind of nanofiber more particularly to a kind of TiO2/WO3/g-C3N4Full meso-porous nano fiber.
The meaning of following expression formula in the present invention are as follows:
PVP: polyvinylpyrrolidone
WCl6: tungsten hexachloride
TBOT: butyl titanate
Background technique
With the fast development of modern industry, energy crisis and problem of environmental pollution increasingly sharpen, and develop and utilize cleaning
High efficient energy sources become the task of top priority of various countries.How effectively solar energy is inexhaustible as a kind of reproducible clean energy resource,
Become the hot spot studied at present using solar energy.
Photocatalysis technology has many advantages, such as that can directly absorb Driven by Solar Energy at room temperature reacts, and becomes that solar energy is direct
Or it is indirectly converted into the ideal production technology of mankind's available energy.The core of photocatalysis technology application is grinding for photochemical catalyst
System, in the development of the past few decades, it has been reported that hundreds of photochemical catalysts.But the photochemical catalyst reported at present is universal
There are photoresponse wavelength is narrow, the problems such as stability is poor, low efficiency, the large-scale use of photochemical catalyst seriously restrict.Therefore, high
The development of effect photochemical catalyst shoulders heavy responsibilities.
In order to solve the problems, such as that photochemical catalyst exists, researchers have done a large amount of explorations, are summed up mainly from material knot
Structure and constituent optimization etc. are set about.The optimization of material structure refers mainly to change the microscopic appearance feature of catalyst, with
High-specific surface area and stable geometrical construction improve the capture rate to light and the adsorption capacity to reactant.Research finds one-dimensional
Meso-hole structure such as meso-porous nano fiber is assigned its efficient and stable light and is urged due to its unique geometry and high-specific surface area
Change activity.Constituent optimization then passes through change band structure, reduces forbidden bandwidth, the service life for extending photo-generated carrier etc..Main packet
Include nonmetal doping, semiconductors coupling and noble-metal-supported etc..The wherein coupling of different semiconductor materials, especially ternary
System composite photo-catalyst can effectively block that photo-generated carrier is compound, enhance the utilization rate of solar energy.TiO2、WO3And g-C3N4
It is representative semiconductor light-catalyst material, having had document report, they are compound separately as either two of them
The research work of semiconductor light-catalyst, but the TiO of ternary system2/WO3/g-C3N4Photocatalyst material has not been reported.
In conjunction with the advantage of one-dimensional mesoporous structure, if it is possible to prepare TiO2/WO3/g-C3N4Meso-porous nano fiber will be from both direction simultaneously
Strengthen its photocatalysis performance, is expected to solve main problem present in traditional photochemical catalyst at present, especially for high efficiency photocatalyst
It is that visible-light photocatalyst establishes certain Research foundation and application value.
Summary of the invention
The purpose of the present invention is being directed to the above-mentioned problems in the prior art, a kind of stable structure, specific surface are proposed
The high TiO of product2/WO3/g-C3N4Full meso-porous nano fiber.
Object of the invention can be realized by the following technical scheme: a kind of TiO2/WO3/g-C3N4Full meso-porous nano is fine
Dimension, TiO2/WO3With TiO2/WO3Form of nanofibers exists, g-C3N4It is supported on TiO2/WO3On nanofiber, wherein TiO2/
WO3Nanofiber has porous structure, and porous structure includes mesoporous.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, TiO2/WO3Nanofiber is complete mesoporous knot
Structure.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, TiO2/WO3Jie of full meso-porous nano fiber
Hole aperture is 2-30nm.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, TiO2/WO3The ratio of full meso-porous nano fiber
Surface area is 10-50m2/g。
TiO of the present invention2/WO3/g-C3N4Full meso-porous nano fiber is by g-C3N4Load TiO2/WO3Full meso-porous nano fiber group
At there is high specific surface area and stable geometrical construction, can be improved pair when being used for photocatalysis hydrolytic hydrogen production as photochemical catalyst
The capture rate of light and adsorption capacity to reactant.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, the nanofiber the preparation method comprises the following steps: first
Prepare g-C3N4Nano flake and TiO2/WO3Full meso-porous nano fiber, the g-C that then will be prepared3N4Nano flake and
TiO2/WO3Full meso-porous nano fiber, which is scattered in solvent, forms solution, g-C3N4Nano flake deposits to TiO2/WO3It is complete mesoporous
Nanofiber is separated after nanofiber, re-dry anneals to obtain TiO2/WO3/g-C3N4Full meso-porous nano fiber.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, g-C3N4Nano flake by by urea into
It is made after row roasting, grinding.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, maturing temperature is 450-550 DEG C, when heat preservation
Between be 3-5h.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, maturing temperature is 500 DEG C, and soaking time is
4h。
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, TiO2/WO3The system of full meso-porous nano fiber
Preparation Method are as follows: by raw material PVP, TBOT, WCl6It is dissolved in solvent, and foaming agent is added, obtain spinning liquid as precursor；By forerunner
Body spinning solution obtains organic precursor fiber through electrostatic spinning and dries, and carries out at calcining after obtaining solid-state organic precursor fiber
TiO is made in reason2/WO3Full meso-porous nano fiber.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, raw material PVP, TBOT, WCl6Mass ratio
For (1-2): (1-5): 1.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, raw material PVP, TBOT, WCl6Mass ratio
For 1.4:3:1.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, solvent is the mixed solvent of pure and mild acid, alcohol
Volume ratio with acid is (2-5): 1.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, foaming agent DIPA.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, foaming agent and WCl6Mass ratio (1-5):
1。
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, foaming agent and WCl6Mass ratio 2:1.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, electrostatic spinning voltage is 10-20kV, cathode
The distance between anode is 15-25cm.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, electrostatic spinning voltage is 15kV, cathode with
The distance between anode is 20cm.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, calcination temperature is 450-550 DEG C, when heat preservation
Between be 1-5h.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, calcination temperature is 500 DEG C, and soaking time is
3h。
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, g-C3N4Nano flake and TiO2/WO3Quan Jie
The mass ratio of hole nanofiber is 1:(0.5-2).
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, g-C3N4Nano flake and TiO2/WO3Quan Jie
The mass ratio of hole nanofiber is 1:1.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, annealing temperature is 250-350 DEG C, and the time is
1-5h。
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, annealing temperature is 300 DEG C in step S3,
Time is 2h.
The present invention realizes TiO2/WO3/g-C3N4The preparation of the full meso-porous nano fiber of ternary system, and the preparation method
It is simple controllable, there is repeatability well.
In a kind of above-mentioned TiO2/WO3/g-C3N4In full meso-porous nano fiber, the TiO2/WO3/g-C3N4Full meso-porous nano
Fiber applications are in high efficiency photocatalyst.
Preferably, TiO2/WO3/g-C3N4Full meso-porous nano fiber is used for light hydrolytic hydrogen production.
The present invention is by the TiO of ternary system2/WO3/g-C3N4Full meso-porous nano fiber is hydrolyzed as photochemical catalyst for light
Hydrogen manufacturing enhances the catalytic performance of photochemical catalyst simultaneously in terms of material structure and constituent optimization two.
Preferably, TiO2/WO3/g-C3N4The mass ratio of full meso-porous nano fiber and water is 1:(500-1000).
Preferably, TiO2/WO3/g-C3N4The mass ratio of full meso-porous nano fiber and water is 1:800.
Preferably, TiO2/WO3/g-C3N4Full meso-porous nano fiber is used to when light hydrolytic hydrogen production also need that sacrifice is added
Agent.
Preferably, sacrifice agent is methanol.
Preferably, the volume ratio of sacrifice agent and water is 1:(2-5).
Preferably, the volume ratio of sacrifice agent and water is 1:4.
Preferably, TiO2/WO3/g-C3N4The photoresponse wavelength of full meso-porous nano fiber is 300-500nm.
Preferably, TiO2/WO3/g-C3N4The photoresponse wavelength of full meso-porous nano fiber is 400-500nm.
Compared with prior art, the method has the advantages that
1. TiO of the present invention2/WO3/g-C3N4Full meso-porous nano fiber has the one-dimensional mesoporous construction of high-ratio surface.
2. the present invention realizes TiO2/WO3/g-C3N4The preparation of full meso-porous nano fiber.
3. TiO of the present invention2/WO3/g-C3N4The preparation method of full meso-porous nano fiber is simply controllable, has and repeats well
Property.
4. TiO of the present invention2/WO3/g-C3N4Full meso-porous nano fiber is used for light hydrolytic hydrogen production, and there is the visible light of enhancing to ring
It answers, stability is good, and solar energy utilization ratio is higher, has better application prospect in terms of solving environmental problem and energy crisis.
5. TiO of the present invention2/WO3/g-C3N4Full meso-porous nano fiber can effectively press down as the photochemical catalyst of tri compound
Compound, the cooperative reinforcing photocatalysis performance of photo-generate electron-hole pair processed.
Detailed description of the invention
Fig. 1 is g-C obtained by the embodiment of the present invention 13N4Nano flake scanning electron microscope (SEM) figure；
Fig. 2 is g-C obtained by the embodiment of the present invention 13N4Nano flake X-ray diffraction (XRD) figure；
Fig. 3 is PVP/TBOT/WCl obtained by the embodiment of the present invention 16/ DIPA precursor fibre scanning electron microscope (SEM)
Figure；
Fig. 4 is TiO obtained by the embodiment of the present invention 12/WO3Low power scanning electron microscope (SEM) figure of full meso-porous nano fiber；
Fig. 5 is TiO obtained by the embodiment of the present invention 12/WO3High power scanning electron microscope (SEM) figure of full meso-porous nano fiber；
Fig. 6 is TiO obtained by the embodiment of the present invention 12/WO3X-ray diffraction (XRD) figure of full meso-porous nano fiber；
Fig. 7 is TiO obtained by the embodiment of the present invention 12/WO3The nitrogen adsorption desorption curve graph of full meso-porous nano fiber；
Fig. 8 is TiO obtained by the embodiment of the present invention 12/WO3The graph of pore diameter distribution of full meso-porous nano fiber；
Fig. 9 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4The low power scanning electron microscope of full meso-porous nano fiber
(SEM) figure；
Figure 10 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4The high power scanning electron microscope of full meso-porous nano fiber
(SEM) figure；
Figure 11 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4The transmission electron microscope of full meso-porous nano fiber
(TEM) figure；
Figure 12 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4The high score of full meso-porous nano fiberoptic fiber matrix
Distinguish transmission electron microscope (HRTEM) figure；
Figure 13 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4Full meso-porous nano fiber g-C3N4High-resolution
Transmission electron microscope (HRTEM) figure；
Figure 14 is pure TiO2, pure g-C3N4、TiO2/WO3Full meso-porous nano fiber, TiO2/WO3/g-C3N4Full meso-porous nano
The ultraviolet-visible absorption spectroscopy of fiber；
Figure 15 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4Full meso-porous nano fiber and pure TiO2, pure g-
C3N4、TiO2/WO3Full meso-porous nano fiber photocatalysis hydrogen production efficiency comparative figure.
Specific embodiment
The following is specific embodiments of the present invention, and is described with reference to the drawings and further retouches to technical solution of the present invention work
It states, however, the present invention is not limited to these examples.
Embodiment 1:
Urea is placed in alumina crucible, one layer of carbon paper is then covered on the mouth of crucible, is subsequently placed in Muffle sintering
In furnace, setting process is that 1 DEG C/min is heated to 500 DEG C of heat preservation 4h, and furnace is as cold as room temperature, and powdered rear system is ground to after taking-up
Obtain g-C3N4Nano flake saves backup.
Take 0.7g PVP, 0.5g WCl6It is dissolved in the in the mixed solvent of 7ml ethyl alcohol and 3ml acetic acid composition, after magnetic agitation 5h
Obtain uniform PVP/WCl6Then the TBOT of 3g is slowly added dropwise in solution, obtain PVP/WCl after continuing strong stirring 2h6/TBOT
Solution finally adds 1.0g foaming agent DIPA, obtains the spinning liquid as precursor containing foaming agent.Then spinning liquid as precursor is existed
Voltage 15kV, spinning under the conditions of the electrospinning of distance 20cm obtain organic precursor fiber, and organic precursor fiber passes through 60 DEG C of perseverances
After warm oven drying, solid-state organic precursor fiber is obtained.Solid-state organic precursor fiber is finally placed in Muffle sintering procedure
Calcination processing in furnace, sintering temperature are 500 DEG C, and heating rate is 1 DEG C/min, soaking time 3h, are obtained after cooling to room temperature with the furnace
To TiO2/WO3Full meso-porous nano fiber, saves backup.
Take the above-mentioned g-C being prepared of 0.5g3N4Nano flake is added in the beaker containing methanol solution, ultrasonic treatment
After 60min, g-C3N4Nano flake is shelled into the nanostructure of fine platy, then, weighs the above-mentioned TiO being prepared of 0.5g2/
WO3Full meso-porous nano fiber continues stirring for 24 hours after being added, and after methanol volatilization, obtains nontransparent powder, is placed in 60 DEG C of constant temperature ovens
It after drying, places it in Muffle furnace, 300 DEG C of annealing 2h, furnace obtain TiO after being as cold as room temperature in air atmosphere2/WO3/g-
C3N4Full meso-porous nano fiber.
The TiO that will be prepared2/WO3/g-C3N4Full meso-porous nano fiber weighs the distilled water that 0.05g is scattered in 40ml
In, after ultrasonic disperse 15min, the methanol of 10ml is added as sacrifice agent, the optical filter conduct of 400nm is added using 300W xenon lamp
Simulated visible light light source carries out photocatalysis hydrogen production.
Comparative example 1 and the difference of embodiment 1 be only that, photochemical catalyst TiO2Semiconductor light-catalyst.
Comparative example 2 and the difference of embodiment 1 be only that, photochemical catalyst g-C3N4Semiconductor light-catalyst.
Comparative example 3 and the difference of embodiment 1 be only that, photochemical catalyst TiO2/WO3Composite semiconductor light-catalyst.
As shown in the figure: Fig. 1 is the preparation-obtained g-C of embodiment 13N4The SEM picture of material, it is shown that its nano flake
The microstructure of shape.Fig. 2 is preparation-obtained g-C3N4The X-ray diffractogram (XRD) of material is composed, and there are two flat as the result is shown
Diffraction maximum caused by Stacking units in the structure of face, it was confirmed that the nano flake of preparation is g-C3N4。
Fig. 3 is PVP/TBOT/WCl obtained by the embodiment of the present invention 16/ DIPA precursor fibre scanning electron microscope (SEM)
Figure shows that the material being prepared is solid-state precursor nanofiber.Fig. 4 and Fig. 5 is TiO prepared by embodiment 12/WO3Entirely
SEM picture of the meso-porous nano fiber under different amplification shows that the full meso-porous nano that prepared material is high-purity is fine
Tie up material.Fig. 6 is its corresponding X-ray diffraction (XRD) map, shows that prepared material is Anatase TiO2And WO3Group
At with good crystallinity.Fig. 7, Fig. 8 are prepared TiO2/WO3The nitrogen adsorption desorption curve of full meso-porous nano fiber and hole
Diameter distribution curve, illustrating synthesized material, there are specific surface area mesoporous and with higher, specific surface area and aperture values point
It Wei not 31.37m2/ g and 19.8 nm.
Fig. 9, Figure 10 are TiO prepared by embodiment 12/WO3/g-C3N4Full meso-porous nano fiber is under different enlargement ratios
SEM picture, show that prepared material is still full meso-porous nano fiber, surface is more coarse.Figure 11 is prepared visible
The TEM picture of light photochemical catalyst illustrates that the visible-light photocatalyst is g-C3N4Load TiO2/WO3Full meso-porous nano fiber
Ternary structural.Figure 12, Figure 13 are its corresponding high-resolution-ration transmission electric-lens photo (HRTEM), it was confirmed that the visible-light photocatalyst
By TiO2、WO3And g-C3N4Composition.
Figure 14 is pure TiO2, pure g-C3N4、TiO2/WO3Full meso-porous nano fiber, TiO2/WO3/g-C3N4It is entirely mesoporous to receive
The ultraviolet-visible absorption spectroscopy of rice fiber, as can be seen from the figure TiO2/WO3/g-C3N4The optical absorption band of full meso-porous nano fiber
Side can be extended to 500nm or so, have good visible light absorption capacity.
Figure 15 is TiO obtained by the embodiment of the present invention 12/WO3/g-C3N4Full meso-porous nano fiber and comparative example 1-3 light
Catalyzing manufacturing of hydrogen efficiency comparative schemes, and the hydrogen generated in test process is detected by online gas chromatograph, detects every 15min
Once, terminate test after 5 hours.It was found from testing result: TiO prepared by the present invention2/WO3/g-C3N4Full meso-porous nano is fine
Tieing up has the visible light catalytic performance significantly improved, and hydrogen generation efficiency is up to 285.4 μm of ol g-1h-1, compare pure phase TiO2, produce hydrogen
Efficiency is improved up to 65 times or more.
Embodiment 2 and the difference of embodiment 1 are only that the maturing temperature of urea is 450 DEG C.
Embodiment 3 and the difference of embodiment 1 are only that the maturing temperature of urea is 460 DEG C.
Embodiment 4 and the difference of embodiment 1 are only that the maturing temperature of urea is 480 DEG C.
Embodiment 5 and the difference of embodiment 1 are only that the maturing temperature of urea is 520 DEG C.
Embodiment 6 and the difference of embodiment 1 are only that the maturing temperature of urea is 550 DEG C.
In view of the numerous embodiments of the scheme of the present invention, each embodiment experimental data is huge numerous, is not suitable for arranging one by one herein
Explanation is lifted, but the content verified required for each embodiment and obtained final conclusion are close, so herein not to each reality
The verifying content for applying example is explained one by one, and only illustrates the excellent place of the present patent application using embodiment 1 as representative.
Claimed midpoint of technical range is not exhaustive in this place embodiment, equally all wants in the present invention
In the range of asking protection.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can do various modifications or supplement or is substituted in a similar manner to described specific embodiment, but simultaneously
Spirit or beyond the scope defined by the appended claims of the invention is not deviated by.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (3)
1. a kind of TiO2/WO3/g-C3N4Full meso-porous nano fiber, which is characterized in that the TiO2/WO3With TiO2/WO3Nanowire
Dimension form exists, the g-C3N4It is supported on TiO2/WO3On nanofiber, wherein the TiO2/WO3Nanofiber is complete mesoporous
Structure；
The TiO2/WO3/g-C3N4Full meso-porous nano fiber the preparation method comprises the following steps: first preparing g-C3N4Nano flake and TiO2/WO3
Full meso-porous nano fiber, takes g-C3N4Nano flake is added in the beaker containing methanol solution, after being ultrasonically treated 60min, with
Afterwards, the TiO is added2/WO3Full meso-porous nano fiber, stirring for 24 hours, after methanol volatilization, obtain nontransparent powder, are placed in 60 DEG C of perseverances
After warm oven drying, 300 DEG C of annealing 2h, furnace obtain TiO after being as cold as room temperature in air atmosphere2/WO3/g-C3N4Full meso-porous nano
Fiber；
The g-C3N4Nano flake at 500 DEG C by roasting urea, insulation reaction 4h, is made after grinding；
The TiO2/WO3Full meso-porous nano fiber the preparation method comprises the following steps: taking PVP, WCl6It is dissolved in the mixing of ethyl alcohol and acetic acid composition
In solvent, the volume ratio of ethyl alcohol and acetic acid is (2-5): obtaining uniform PVP/WCl after 1, magnetic agitation 5h6Then solution drips
Add TBOT, obtains PVP/WCl after continuing strong stirring 2h6/ TBOT solution finally adds foaming agent DIPA, obtains containing foaming
The spinning liquid as precursor of agent obtains organic precursor fiber through electrostatic spinning and dries, after obtaining solid-state organic precursor fiber
Calcination processing is carried out, TiO is made2/WO3Full meso-porous nano fiber；The TiO2/WO3The mesoporous pore size of meso-porous nano fiber is entirely
2-30nm, the TiO2/WO3The specific surface area of full meso-porous nano fiber is 10-50m2/g。
2. a kind of TiO according to claim 12/WO3/g-C3N4Full meso-porous nano fiber, which is characterized in that raw material PVP,
TBOT、WCl6Mass ratio be (1-2): (1-5): 1.
3. a kind of TiO according to claim 12/WO3/g-C3N4Full meso-porous nano fiber, which is characterized in that the g-
C3N4Nano flake and TiO2/WO3The mass ratio of full meso-porous nano fiber is 1:(0.5-2).
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| CN105628745B (en) * | 2016-02-25 | 2018-06-29 | 济南大学 | A kind of preparation method and application of the nitrogen dioxide gas sensor based on titania-based porous nano composite material |
| CN105572175B (en) * | 2016-02-25 | 2018-05-25 | 济南大学 | A kind of preparation method and application of the dimethylbenzene gas sensor based on titanium dioxide nanoplate |
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| CN102358964A (en) * | 2011-08-12 | 2012-02-22 | 东华大学 | Method for preparing titanium-tungsten compound oxide nano-fiber |
| CN102962088A (en) * | 2012-11-06 | 2013-03-13 | 中国科学院广州地球化学研究所 | Composite visible-light catalyst for TiO2 microsphere and g-C3N4, as well as preparation method and application of catalyst |
| CN103418415A (en) * | 2013-08-22 | 2013-12-04 | 南昌航空大学 | Method for using ultrasonic mixing to prepare Ag-g-C3N4/TiO2 photocatalyst |
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