CN105148965A - TiO2/WO3/g-C3N4 total mesoporous nanofiber - Google Patents
TiO2/WO3/g-C3N4 total mesoporous nanofiber Download PDFInfo
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- CN105148965A CN105148965A CN201510392188.3A CN201510392188A CN105148965A CN 105148965 A CN105148965 A CN 105148965A CN 201510392188 A CN201510392188 A CN 201510392188A CN 105148965 A CN105148965 A CN 105148965A
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Abstract
The invention relates to a TiO2/WO3/g-C3N4 total mesoporous nanofiber. TiO2/WO3 in the nanofiber exists in the form of TiO2/WO3 nanofiber, g-C3N4 is loaded on the TiO2/WO3 nanofiber, wherein the TiO2/WO3 nanofiber has a porous structure, which includes mesopores. The TiO2/WO3/g-C3N4 total mesoporous nanofiber provided by the invention has stable structure and high specific surface area.
Description
Technical field
The present invention relates to a kind of nanofiber, particularly relate to a kind of TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber.
In the present invention, the meaning of following expression formula is:
PVP: polyvinylpyrrolidone
WCl
6: tungsten hexachloride
TBOT: butyl titanate
Background technology
Along with the fast development of modern industry, energy crisis and problem of environmental pollution increasingly sharpen, and the development and utilization clean and effective energy becomes the task of top priority of various countries.Solar energy is as the reproducible clean energy resource of one, inexhaustible, how effectively to utilize solar energy to become the focus of research at present.
Photocatalysis technology has and at room temperature can directly absorb the advantages such as Driven by Solar Energy reaction, becomes desirable production technology solar energy being directly or indirectly converted to mankind's available energy.The core of photocatalysis technology application is the development of photochemical catalyst, in the development of decades in the past, has reported hundreds of photochemical catalyst.But the photochemical catalyst ubiquity photoresponse wavelength of report is narrow at present, and the problems such as poor stability, efficiency are low, seriously govern the extensive use of photochemical catalyst.Therefore, the development of high efficiency photocatalyst shoulders heavy responsibilities.
In order to solve photochemical catalyst Problems existing, researchers have done a large amount of exploration, are summed up and mainly set about from the aspect such as material structure and constituent optimization.The optimization of material structure mainly refers to the microscopic appearance feature changing catalyst, makes it to have the stable geometrical construction of high-ratio surface sum, improves the capture rate to light and the adsorption capacity to reactant.Research finds that one-dimensional mesoporous structure is if meso-porous nano fiber is due to the geometry of its uniqueness and high-specific surface area, gives the photocatalytic activity that it is efficient and stable.Constituent optimization, then by changing band structure, reducing energy gap, extending the life-span etc. of photo-generated carrier.Mainly comprise nonmetal doping, semiconductors coupling and noble-metal-supported etc.The wherein coupling of different semi-conducting material, especially ternary system composite photo-catalyst can effectively block photo-generated carrier compound, strengthen the utilization rate of solar energy.TiO
2, WO
3and g-C
3n
4be representational semiconductor light-catalyst material, had bibliographical information they separately as or the research work of wherein two kinds of composite semiconductor light-catalysts, but the TiO of ternary system
2/ WO
3/ g-C
3n
4photocatalyst material have not been reported.In conjunction with the advantage of one-dimensional mesoporous structure, if can TiO be prepared
2/ WO
3/ g-C
3n
4meso-porous nano fiber will strengthen its photocatalysis performance from both direction simultaneously, be expected to solve the subject matter existing for current traditional photochemical catalyst, for high efficiency photocatalyst especially visible-light photocatalyst establishes certain Research foundation and using value.
Summary of the invention
The object of the invention is for the above-mentioned problems in the prior art, propose a kind of Stability Analysis of Structures, TiO that specific area is high
2/ WO
3/ g-C
3n
4full meso-porous nano fiber.
Object of the present invention realizes by following technical proposal: a kind of TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, TiO
2/ WO
3with TiO
2/ WO
3form of nanofibers exists, g-C
3n
4load is at TiO
2/ WO
3on nanofiber, wherein TiO
2/ WO
3nanofiber has loose structure, and loose structure comprises mesoporous.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, TiO
2/ WO
3nanofiber is full meso-hole structure.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, TiO
2/ WO
3the mesoporous pore size of full meso-porous nano fiber is 2-30nm.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, TiO
2/ WO
3the specific area of full meso-porous nano fiber is 10-50m
2/ g.
TiO of the present invention
2/ WO
3/ g-C
3n
4full meso-porous nano fiber is by g-C
3n
4load TiO
2/ WO
3full meso-porous nano is fibrous, has high specific surface area and stable geometrical construction, can improve the capture rate to light and the adsorption capacity to reactant when being used for photocatalysis hydrolytic hydrogen production as photochemical catalyst.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, the preparation method of this nanofiber is: first prepare g-C
3n
4nano flake and TiO
2/ WO
3full meso-porous nano fiber, the g-C then will prepared
3n
4nano flake and TiO
2/ WO
3full meso-porous nano fiber dispersion forms solution, g-C in solvent
3n
4nano flake deposits to TiO
2/ WO
3be separated nanofiber after full meso-porous nano fiber, then drying and annealing obtains TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, g-C
3n
4nano flake obtains after urea being carried out roasting, grinding.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, sintering temperature is 450-550 DEG C, and temperature retention time is 3-5h.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, sintering temperature is 500 DEG C, and temperature retention time is 4h.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, TiO
2/ WO
3the preparation method of full meso-porous nano fiber is: by raw material PVP, TBOT, WCl
6be dissolved in solvent, and add blowing agent, obtain spinning liquid as precursor; Spinning liquid as precursor obtained organic precursor fiber through electrostatic spinning and dries, after obtaining solid-state organic precursor fiber, carrying out calcination processing, obtained TiO
2/ WO
3full meso-porous nano fiber.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, raw material PVP, TBOT, WCl
6mass ratio be (1-2): (1-5): 1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, raw material PVP, TBOT, WCl
6mass ratio be 1.4:3:1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, solvent is the mixed solvent of alcohol and acid, and the volume ratio of alcohol and acid is (2-5): 1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, blowing agent is DIPA.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, blowing agent and WCl
6mass ratio (1-5): 1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, blowing agent and WCl
6mass ratio 2:1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, electrostatic spinning voltage is 10-20kV, and the distance between negative electrode and positive electrode is 15-25cm.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, electrostatic spinning voltage is 15kV, and the distance between negative electrode and positive electrode is 20cm.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, calcining heat is 450-550 DEG C, and temperature retention time is 1-5h.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, calcining heat is 500 DEG C, and temperature retention time is 3h.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, g-C
3n
4nano flake and TiO
2/ WO
3the mass ratio of full meso-porous nano fiber is 1:(0.5-2).
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, g-C
3n
4nano flake and TiO
2/ WO
3the mass ratio of full meso-porous nano fiber is 1:1.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, annealing temperature is 250-350 DEG C, and the time is 1-5h.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, in step S3, annealing temperature is 300 DEG C, and the time is 2h.
Present invention achieves TiO
2/ WO
3/ g-C
3n
4the preparation of the full meso-porous nano fiber of ternary system, and this preparation method is simply controlled, has good repeatability.
At above-mentioned a kind of TiO
2/ WO
3/ g-C
3n
4in full meso-porous nano fiber, this TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber applications is in high efficiency photocatalyst.
As preferably, TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber is used for light hydrolytic hydrogen production.
The present invention is by the TiO of ternary system
2/ WO
3/ g-C
3n
4full meso-porous nano fiber is used for light hydrolytic hydrogen production as photochemical catalyst, enhances the catalytic performance of photochemical catalyst from material structure and constituent optimization two aspects simultaneously.
As preferably, TiO
2/ WO
3/ g-C
3n
4the mass ratio of full meso-porous nano fiber and water is 1:(500-1000).
As preferably, TiO
2/ WO
3/ g-C
3n
4the mass ratio of full meso-porous nano fiber and water is 1:800.
As preferably, TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber also needs to add sacrifice agent when being used for light hydrolytic hydrogen production.
As preferably, sacrifice agent is methyl alcohol.
As preferably, the volume ratio of sacrifice agent and water is 1:(2-5).
As preferably, the volume ratio of sacrifice agent and water is 1:4.
As preferably, TiO
2/ WO
3/ g-C
3n
4the photoresponse wavelength of full meso-porous nano fiber is 300-500nm.
As preferably, TiO
2/ WO
3/ g-C
3n
4the photoresponse wavelength of full meso-porous nano fiber is 400-500nm.
Compared with prior art, the present invention has following advantage:
1. TiO of the present invention
2/ WO
3/ g-C
3n
4full meso-porous nano fiber has the one-dimensional mesoporous structure of high-ratio surface.
2. present invention achieves TiO
2/ WO
3/ g-C
3n
4the preparation of full meso-porous nano fiber.
3. TiO of the present invention
2/ WO
3/ g-C
3n
4the preparation method of full meso-porous nano fiber is simply controlled, has good repeatability.
4. TiO of the present invention
2/ WO
3/ g-C
3n
4full meso-porous nano fiber is used for light hydrolytic hydrogen production, and have the visible light-responded of enhancing, good stability, solar energy utilization ratio is higher, in solution environmental problem and energy crisis, have better application prospect.
5. TiO of the present invention
2/ WO
3/ g-C
3n
4the compound that full meso-porous nano fiber can effectively suppress photo-generate electron-hole right as the photochemical catalyst of tri compound, cooperative reinforcing photocatalysis performance.
Accompanying drawing explanation
The g-C of Fig. 1 obtained by the embodiment of the present invention 1
3n
4nano flake ESEM (SEM) figure;
The g-C of Fig. 2 obtained by the embodiment of the present invention 1
3n
4nano flake X-ray diffraction (XRD) figure;
The PVP/TBOT/WCl of Fig. 3 obtained by the embodiment of the present invention 1
6/ DIPA precursor fibre ESEM (SEM) figure;
The TiO of Fig. 4 obtained by the embodiment of the present invention 1
2/ WO
3low power ESEM (SEM) figure of full meso-porous nano fiber;
The TiO of Fig. 5 obtained by the embodiment of the present invention 1
2/ WO
3high power ESEM (SEM) figure of full meso-porous nano fiber;
The TiO of Fig. 6 obtained by the embodiment of the present invention 1
2/ WO
3x-ray diffraction (XRD) figure of full meso-porous nano fiber;
The TiO of Fig. 7 obtained by the embodiment of the present invention 1
2/ WO
3the nitrogen adsorption desorption curve map of full meso-porous nano fiber;
The TiO of Fig. 8 obtained by the embodiment of the present invention 1
2/ WO
3the graph of pore diameter distribution of full meso-porous nano fiber;
The TiO of Fig. 9 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4low power ESEM (SEM) figure of full meso-porous nano fiber;
The TiO of Figure 10 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4high power ESEM (SEM) figure of full meso-porous nano fiber;
The TiO of Figure 11 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4transmission electron microscope (TEM) figure of full meso-porous nano fiber;
The TiO of Figure 12 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4high-resolution-ration transmission electric-lens (HRTEM) figure of full meso-porous nano fiberoptic fiber matrix;
The TiO of Figure 13 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber g-C
3n
4high-resolution-ration transmission electric-lens (HRTEM) figure;
Figure 14 is pure TiO
2, pure g-C
3n
4, TiO
2/ WO
3full meso-porous nano fiber, TiO
2/ WO
3/ g-C
3n
4the ultraviolet-visible absorption spectroscopy of full meso-porous nano fiber;
The TiO of Figure 15 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber and pure TiO
2, pure g-C
3n
4, TiO
2/ WO
3full meso-porous nano fiber optic catalyzing manufacturing of hydrogen efficiency comparative figure.
Detailed description of the invention
Be below specific embodiments of the invention, and accompanying drawings is further described technical scheme of the present invention, but the present invention is not limited to these embodiments.
Embodiment 1:
Urea is placed in alumina crucible, then at the mouth upper cover last layer carbon paper of crucible, is then placed in horse not sintering furnace, arranging process is that 1 DEG C/min is heated to 500 DEG C of insulation 4h, and stove is as cold as room temperature, is ground to Powdered rear obtained g-C after taking-up
3n
4nano flake, saves backup.
Get 0.7gPVP, 0.5gWCl
6be dissolved in the mixed solvent that 7ml ethanol and 3ml acetic acid forms, after magnetic agitation 5h, obtain homogeneous PVP/WCl
6solution, then slowly drips the TBOT of 3g, obtains PVP/WCl after continuing strong stirring 2h
6/ TBOT solution, finally adds 1.0g blowing agent DIPA, obtains the spinning liquid as precursor containing blowing agent.Then by spinning liquid as precursor spinning under the electrospinning condition of voltage 15kV, distance 20cm, obtain organic precursor fiber, organic precursor fiber, after 60 DEG C of constant temperature oven dryings, obtains solid-state organic precursor fiber.Finally solid-state organic precursor fiber is placed in horse not sintering procedure stove calcination processing, sintering temperature is 500 DEG C, and heating rate is 1 DEG C/min, temperature retention time 3h, obtains TiO after cooling to room temperature with the furnace
2/ WO
3full meso-porous nano fiber, saves backup.
Get the above-mentioned g-C prepared of 0.5g
3n
4nano flake joins in the beaker containing methanol solution, after ultrasonic process 60min, and g-C
3n
4nano flake is shelled into the nanostructured of fine platy, subsequently, takes the above-mentioned TiO prepared of 0.5g
2/ WO
3full meso-porous nano fiber adds rear continuation and stirs 24h, after methyl alcohol volatilization, obtains nontransparent powder, after being placed in 60 DEG C of constant temperature oven dryings, is placed in Muffle furnace, in air atmosphere 300 DEG C of annealing 2h, and stove obtains TiO after being as cold as room temperature
2/ WO
3/ g-C
3n
4full meso-porous nano fiber.
By the TiO prepared
2/ WO
3/ g-C
3n
4full meso-porous nano fiber takes 0.05g and is scattered in the distilled water of 40ml, and after ultrasonic disperse 15min, then the methyl alcohol adding 10ml is as sacrifice agent, and the optical filter adopting 300W xenon lamp to add 400nm carries out photocatalysis hydrogen production as simulated visible light light source.
Comparative example 1 is only with the difference of embodiment 1, and photochemical catalyst is TiO
2semiconductor light-catalyst.
Comparative example 2 is only with the difference of embodiment 1, and photochemical catalyst is g-C
3n
4semiconductor light-catalyst.
Comparative example 3 is only with the difference of embodiment 1, and photochemical catalyst is TiO
2/ WO
3composite semiconductor light-catalyst.
As shown in the figure: Fig. 1 is the preparation-obtained g-C of embodiment 1
3n
4the SEM picture of material, shows the microstructure of its nanometer thin sheet.Fig. 2 is preparation-obtained g-C
3n
4x-ray diffractogram (XRD) spectrum of material, result shows the diffraction maximum caused by the Stacking units in two planar structures, confirms that the nano flake of preparation is g-C
3n
4.
The PVP/TBOT/WCl of Fig. 3 obtained by the embodiment of the present invention 1
6/ DIPA precursor fibre ESEM (SEM) figure, shows that the material prepared is solid-state precursor nanofiber.The TiO of Fig. 4 and Fig. 5 prepared by embodiment 1
2/ WO
3the SEM picture of full meso-porous nano fiber under different amplification, shows that prepared material is highly purified full meso-porous nano fibrous material.Fig. 6 is X-ray diffraction (XRD) collection of illustrative plates of its correspondence, shows that prepared material is Anatase TiO
2and WO
3composition, has good crystallinity.Fig. 7, Fig. 8 are prepared TiO
2/ WO
3the nitrogen adsorption desorption curve of full meso-porous nano fiber and pore size distribution curve, the material synthesized by explanation exists mesoporous and has higher specific area, and its specific area and aperture value are respectively 31.37m
2/ g and 19.8nm.
Fig. 9, Figure 10 TiO prepared by embodiment 1
2/ WO
3/ g-C
3n
4the SEM picture of full meso-porous nano fiber under different enlargement ratio, show that prepared material is still full meso-porous nano fiber, surface is more coarse.Figure 11 is the TEM picture of prepared visible-light photocatalyst, and describing this visible-light photocatalyst is g-C
3n
4load TiO
2/ WO
3the ternary structural of full meso-porous nano fiber.Figure 12, Figure 13 are the high-resolution-ration transmission electric-lens photo (HRTEM) of its correspondence, confirm that this visible-light photocatalyst is by TiO
2, WO
3and g-C
3n
4composition.
Figure 14 is for being pure TiO
2, pure g-C
3n
4, TiO
2/ WO
3full meso-porous nano fiber, TiO
2/ WO
3/ g-C
3n
4the ultraviolet-visible absorption spectroscopy of full meso-porous nano fiber, as can be seen from the figure TiO
2/ WO
3/ g-C
3n
4the light absorption band edge of full meso-porous nano fiber can be extended to about 500nm, has good visible absorption ability.
The TiO of Figure 15 obtained by the embodiment of the present invention 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber and comparative example 1-3 photocatalysis hydrogen production efficiency comparative scheme, and the hydrogen produced in test process is detected by online gas chromatograph, detect once every 15min, terminate test after 5 hours.From testing result: TiO prepared by the present invention
2/ WO
3/ g-C
3n
4full meso-porous nano fiber has the visible light catalytic performance significantly improved, and its hydrogen generation efficiency can reach 285.4 μm of olg
-1h
-1, compare pure phase TiO
2, hydrogen generation efficiency raising reaches more than 65 times.
Embodiment 2 is only with the difference of embodiment 1, and the sintering temperature of urea is 450 DEG C.
Embodiment 3 is only with the difference of embodiment 1, and the sintering temperature of urea is 460 DEG C.
Embodiment 4 is only with the difference of embodiment 1, and the sintering temperature of urea is 480 DEG C.
Embodiment 5 is only with the difference of embodiment 1, and the sintering temperature of urea is 520 DEG C.
Embodiment 6 is only with the difference of embodiment 1, and the sintering temperature of urea is 550 DEG C.
The difference of embodiment 7-12 and embodiment 1-6 is only, during the roasting of urea, temperature retention time is 3h.
The difference of embodiment 13-18 and embodiment 1-6 is only, during the roasting of urea, temperature retention time is 5h.
The difference of embodiment 19-36 and embodiment 1-18 is only, the addition of raw material PVP is 0.5g.
The difference of embodiment 37-54 and embodiment 1-18 is only, the addition of raw material PVP is 0.6g.
The difference of embodiment 55-72 and embodiment 1-18 is only, the addition of raw material PVP is 0.8g.
The difference of embodiment 73-90 and embodiment 1-18 is only, the addition of raw material PVP is 1g.
The difference of embodiment 91-180 and embodiment 1-90 is only, the addition of raw material TBOT is 1g.
The difference of embodiment 181-270 and embodiment 1-90 is only, the addition of raw material TBOT is 2g.
The difference of embodiment 271-360 and embodiment 1-90 is only, the addition of raw material TBOT is 4g.
The difference of embodiment 361-450 and embodiment 1-90 is only, the addition of raw material TBOT is 5g.
The difference of embodiment 451-900 and embodiment 1-450 is only, the addition of blowing agent is 0.5g.
The difference of embodiment 901-1350 and embodiment 1-450 is only, the addition of blowing agent is 1.5g.
The difference of embodiment 1351-1800 and embodiment 1-450 is only, the addition of blowing agent is 2g.
The difference of embodiment 1801-2250 and embodiment 1-450 is only, the addition of blowing agent is 2.5g.
The difference of embodiment 2251-4500 and embodiment 1-2250 is only, electrostatic spinning voltage is 10kV, and the distance between negative electrode and positive electrode is 15cm.
The difference of embodiment 4501-6750 and embodiment 1-2250 is only, electrostatic spinning voltage is 18kV, and the distance between negative electrode and positive electrode is 18cm.
The difference of embodiment 6751-9000 and embodiment 1-2250 is only, electrostatic spinning voltage is 20kV, and the distance between negative electrode and positive electrode is 25cm.
The difference of embodiment 9001-18000 and embodiment 1-9000 is only, calcining heat is 450 DEG C.
The difference of embodiment 18001-27000 and embodiment 1-9000 is only, calcining heat is 480 DEG C.
The difference of embodiment 27001-36000 and embodiment 1-9000 is only, calcining heat is 520 DEG C.
The difference of embodiment 36001-45000 and embodiment 1-9000 is only, calcining heat is 550 DEG C.
The difference of embodiment 45001-90000 and embodiment 1-45000 is only, the sintering soak time is 1h.
The difference of embodiment 90001-13500 and embodiment 1-45000 is only, the sintering soak time is 2h.
The difference of embodiment 13501-18000 and embodiment 1-45000 is only, the sintering soak time is 4h.
The difference of embodiment 18001-225000 and embodiment 1-45000 is only, the sintering soak time is 5h.
The difference of embodiment 225001-450000 and embodiment 1-225000 is only, TiO
2/ WO
3the addition of full meso-porous nano fiber is 0.25g.
The difference of embodiment 450001-675000 and embodiment 1-225000 is only, TiO
2/ WO
3the addition of full meso-porous nano fiber is 1g.
The difference of embodiment 675001-1350000 and embodiment 1-675000 is only, annealing temperature is 250 DEG C.
The difference of embodiment 1350001-2025000 and embodiment 1-675000 is only, annealing temperature is 280 DEG C.
The difference of embodiment 2025001-2700000 and embodiment 1-675000 is only, annealing temperature is 320 DEG C.
The difference of embodiment 2700001-5400000 and embodiment 1-2700000 is only, annealing temperature is 350 DEG C.
The difference of embodiment 5400001-8100000 and embodiment 1-2700000 is only, annealing time is 1h.
The difference of embodiment 8100001-10800000 and embodiment 1-2700000 is only, annealing time is 3h.
The difference of embodiment 10800001-13500000 and embodiment 1-2700000 is only, annealing time is 5h.
The difference of embodiment 13500001-27000000 and embodiment 1-13500000 is only, by 0.05gTiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber dispersion is in the distilled water of 25ml.
The difference of embodiment 27000001-40500000 and embodiment 1-13500000 is only, by 0.05gTiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber dispersion is in the distilled water of 30ml.
The difference of embodiment 40500001-54000000 and embodiment 1-13500000 is only, by 0.05gTiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber dispersion is in the distilled water of 50ml.
The difference of embodiment 54000001-108000000 and embodiment 1-54000000 is only, the addition of sacrifice agent is 8ml.
The difference of embodiment 108000001-162000000 and embodiment 1-54000000 is only, the addition of sacrifice agent is 20ml.
The difference of embodiment 162000001-324000000 and embodiment 1-162000000 is only, adopts 300W xenon lamp to add the optical filter of 300nm as simulated visible light light source.
The difference of embodiment 324000001-486000000 and embodiment 1-162000000 is only, adopts 300W xenon lamp to add the optical filter of 500nm as simulated visible light light source.
In view of the present invention program's embodiment is numerous, each embodiment experimental data is huge numerous, be not suitable for particularize explanation herein, but the content of the required checking of each embodiment is all close with the final conclusion obtained, so do not illustrate one by one the checking content of each embodiment, only with embodiment 1, the excellent part of the present patent application is representatively described herein.
The non-limit part of technical scope midrange that this place embodiment is protected application claims, equally all in the scope of protection of present invention.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Although made a detailed description the present invention and quoted some specific embodiments as proof, to those skilled in the art, only otherwise it is obvious for leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (10)
1. a TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described TiO
2/ WO
3with TiO
2/ WO
3form of nanofibers exists, described g-C
3n
4load is at TiO
2/ WO
3on nanofiber, wherein TiO
2/ WO
3nanofiber has loose structure, and loose structure comprises mesoporous.
2. a kind of TiO according to claim 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described TiO
2/ WO
3nanofiber is full meso-hole structure.
3. a kind of TiO according to claim 2
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described TiO
2/ WO
3the mesoporous pore size of full meso-porous nano fiber is 2-30nm.
4. a kind of TiO according to claim 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described TiO
2/ WO
3the specific area of full meso-porous nano fiber is 10-50m
2/ g.
5. a kind of TiO according to claim 1
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, the preparation method of described nanofiber is: first prepare g-C
3n
4nano flake and TiO
2/ WO
3full meso-porous nano fiber, the g-C then will prepared
3n
4nano flake and TiO
2/ WO
3full meso-porous nano fiber dispersion forms solution, g-C in solvent
3n
4nano flake deposits to TiO
2/ WO
3be separated nanofiber after full meso-porous nano fiber, then drying and annealing obtains TiO
2/ WO
3/ g-C
3n
4full meso-porous nano fiber.
6. a kind of TiO according to claim 5
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described g-C
3n
4nano flake obtains after urea being carried out roasting, grinding.
7. a kind of TiO according to claim 5
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described TiO
2/ WO
3the preparation method of full meso-porous nano fiber is: by raw material PVP, TBOT, WCl
6be dissolved in solvent, and add blowing agent, obtain spinning liquid as precursor; Spinning liquid as precursor obtained organic precursor fiber through electrostatic spinning and dries, after obtaining solid-state organic precursor fiber, carrying out calcination processing, obtained TiO
2/ WO
3full meso-porous nano fiber.
8. a kind of TiO according to claim 7
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described raw material PVP, TBOT, WCl
6mass ratio be (1-2): (1-5): 1.
9. a kind of TiO according to claim 5
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described g-C
3n
4nano flake and TiO
2/ WO
3the mass ratio of full meso-porous nano fiber is 1:(0.5-2).
10. a kind of TiO according to claim 5
2/ WO
3/ g-C
3n
4full meso-porous nano fiber, is characterized in that, described annealing temperature is 250-350 DEG C, and the time is 1-5h.
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| CN105606655A (en) * | 2016-02-25 | 2016-05-25 | 济南大学 | Palladium-supported acetone gas sensor manufacturing method based on two-dimensional porous nano composite material and application |
| CN105628745A (en) * | 2016-02-25 | 2016-06-01 | 济南大学 | Preparation method and application for nitrogen dioxide gas sensor based on titanium-dioxide-based porous nanocomposite |
| CN105780191A (en) * | 2016-05-18 | 2016-07-20 | 海安县兄弟合成纤维有限公司 | WO3/TiO2/SiO2 composite fiber |
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