CN106311266A - Preparation method of trace-iron-doped tungsten trioxide nanofiber photocatalyst - Google Patents
Preparation method of trace-iron-doped tungsten trioxide nanofiber photocatalyst Download PDFInfo
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- CN106311266A CN106311266A CN201610660255.XA CN201610660255A CN106311266A CN 106311266 A CN106311266 A CN 106311266A CN 201610660255 A CN201610660255 A CN 201610660255A CN 106311266 A CN106311266 A CN 106311266A
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- tungsten trioxide
- iron
- polyvinylpyrrolidone
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000002121 nanofiber Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 33
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 28
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 28
- 239000000835 fiber Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 19
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 150000002505 iron Chemical class 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007598 dipping method Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 47
- 229910052742 iron Inorganic materials 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical group [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 238000003911 water pollution Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 26
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000013507 mapping Methods 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013036 cure process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
-
- B01J35/39—
-
- B01J35/58—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention belongs to the technical field of nanomaterial preparation, and discloses a preparation method of a trace-iron-doped tungsten trioxide nanofiber photocatalyst. The method includes the following steps that 1, ammonium metatungstate is dissolved in water, polyvinylpyrrolidone is added, stirring is carried out, and a precursor solution is obtained; 2, the precursor solution obtained in the step 1 is subjected to electrostatic spinning, and as-spun fibers are obtained; 3, the as-spun fibers obtained in the step 2 are roasted, and after cooling, tungsten trioxide nanofibers are obtained; 4, the tungsten trioxide nanofibers obtained in the step 3 are dipped in an iron salt solution, and after drying, the photocatalyst is obtained. The preparation method is simple, low in cost and environmentally friendly. The electrostatic spinning technology and the dipping method are combined, operation is easy, the prepared trace-iron-doped tungsten trioxide nanofibers are stable in morphology and uniform in diameter distribution with the network distribution of original tungsten trioxide unchanged, and meanwhile the photocatalytic degradation performance of tungsten trioxide is greatly improved.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, the Tungstic anhydride. adulterated more particularly, to a kind of trace iron
The preparation method of nanofiber photocatalyst.
Background technology
In recent years, along with development and the rapid raising of people's living standard of process of industrialization, problem of environmental pollution becomes
The main bugbear of facing mankind, especially water pollution, more and more cause everybody concern at present.In pollution source of water body,
Industrial wastewater accounts for greatly, because its color is deep, and strong toxicity, it is difficult to process.
Semiconductor light-catalyst is with its stable physicochemical properties, the most widely distributed, is readily available, cheap and
The advantages such as non-secondary pollution have obtained widely studied.What traditional Study on photocatalyst was most is exactly titanium dioxide
(TiO2) and zinc oxide (ZnO), their greater band gap, the ultraviolet light that wavelength is shorter is had well response, but due to purple
Outer light only accounts for small part in sunlight so actual application is restricted.
As a member of transition metal oxide, tungsten oxide (WO3) it is a kind of indirect band gap n-type semiconductor, it is prohibited
Bandwidth is 2.2 ~ 2.8eV, has well absorption for visible ray, is therefore a kind of semiconductor light very with development potentiality
Catalyst.
Electrostatic spinning technique is a kind of method for quickly and easily preparing nanofiber, manufactures that device is simple, is spun to
Basis is the cheapest, it is various to spin substance classes, not only has the biggest progress in terms of laboratory research, and industrialization potential is the hugest
Greatly.Therefore method of electrostatic spinning batch prepare tungsten trioxide nano fiber and be used as photocatalyst have the biggest industrial value and
Social meaning.
But simple Tungstic anhydride. photocatalytic activity ratio is relatively low, metal-doped its photocatalytic can be improved by carrying out
Energy.Ferrum element is the most widely distributed, cheap and easy to get, water body will not be caused secondary pollution simultaneously, there are some researches show,
Semiconductor light-catalyst mixes metal ion, can substantially suppress the compound of electron-hole pair by IFCT effect, improve light and urge
The catalysis activity of agent.
Summary of the invention
It is an object of the invention to according to tungsten trioxide nano fiber in prior art as catalysis activity in catalyst
Not enough, it is provided that the preparation method of the tungsten trioxide nano fiber photocatalyst of a kind of trace iron doping.
The purpose of the present invention is achieved through the following technical solutions:
The invention provides the preparation method of the tungsten trioxide nano fiber photocatalyst of a kind of trace iron doping, including walking as follows
Rapid:
S1., ammonium metatungstate being dissolved in water, adds polyvinylpyrrolidone, stirring obtains precursor solution；
S2. precursor solution in S1 is carried out electrostatic spinning, obtain as-spun fibre；
S3. the as-spun fibre calcining that will prepare in S2, obtains tungsten trioxide nano fiber after cooling；
S4., by tungsten trioxide nano fiber impregnation in S3 in iron salt solutions, described photocatalyst is obtained after drying；
In S1, ammonium metatungstate is (0.2 ~ 0.6) with the solid-to-liquid ratio of water: 1；The molecular weight of described polyvinylpyrrolidone is (1 ~ 2)
×106；Polyvinylpyrrolidone is (0.1 ~ 0.3) with the solid-to-liquid ratio of water: 1；
In S2 step electrostatic spinning, voltage is 18 ~ 30KV, and receiving range is 15cm, and fltting speed is 0.01 ~ 0.1ml/min；
In S4, the concentration of iron salt solutions is 0.03 ~ 0.3g/L, and ferrum is 0.1 ~ 1% relative to the mass fraction of Tungstic anhydride..
The present invention first passes through and ammonium metatungstate is dissolved in water, adds polyvinylpyrrolidone, regulates and controls the ratio between each raw material
Example, obtains precursor solution, then by electrostatic spinning process, by molten for the above-mentioned presoma possessing preferable electric conductivity and viscosity
Liquid makes as-spun fibre, after calcining, prepares, by doping trace iron, the Tungstic anhydride. that photocatalysis performance gets a promotion
Nanofiber.
Preferably, ferrum is 0.3% relative to the mass fraction of Tungstic anhydride..
Preferably, in S1, the molecular weight of polyvinylpyrrolidone is 1.3 × 106.In the present invention effect of PVP be in order to
Ammonium metatungstate coordinates, and both increase the viscosity of precursor solution and electric conductivity for electrostatic spinning under appropriate proportioning, exist simultaneously
The effect that can also play support in fiber flash cure process later is become to keep the pattern of fiber.
Preferably, in S1, ammonium metatungstate is (0.35 ~ 0.5) with the solid-to-liquid ratio of water: 1；Polyvinylpyrrolidone is consolidated with water
Liquor ratio is (0.1 ~ 0.25): 1.
Preferably, in S1, mixing time is stirring 2 ~ 5 hours.
Preferably, in S3, calcining heat is 500 ~ 650 DEG C, and programming rate is 1 ~ 5 DEG C/min, and is incubated 0.5 hour.
Preferably, in S4, dipping temperature is 80 ~ 90 DEG C, and dip time is 2 ~ 4 hours.
Preferably, baking temperature is 110 DEG C, and drying time is 5 ~ 8 hours.
Preferably, described iron salt is iron chloride.
" solid-to-liquid ratio " mentioned in the present invention is the relation between weight portion and parts by volume, in terms of g/ml.
Compared with prior art, the present invention has the following advantages and beneficial effect:
Preparation method of the present invention is simple, with low cost, adopts and uses water as solvent, environmental protection；In conjunction with electrostatic spinning technique and leaching
Stain method, simple to operate, the trace iron doping Tungstic anhydride. that the method prepares does not changes the network-like distribution of Tungstic anhydride., pattern
Stable, diameter Distribution is uniform, drastically increases the Photocatalytic Degradation Property of Tungstic anhydride. simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the Tungstic anhydride. after the prepared tungsten trioxide nano fiber of embodiment 1 and Fe2O3 doping.
Fig. 2 is the TEM-mapping figure of the trace iron doping tungsten trioxide nano fiber of embodiment 1 preparation
Fig. 3 is the XRD figure of Tungstic anhydride. after the tungsten trioxide nano fiber of embodiment 1 preparation and Fe2O3 doping.
Fig. 4 is that methyl orange is degraded by the Fe2O3 doping Tungstic anhydride. using the inventive method to prepare as photocatalyst
Degradation effect figure.
Fig. 5 is to use what different trace iron doping in the inventive method prepared photocatalyst to enter methyl orange
The degradation effect comparison diagram of row degraded.
Fig. 6 is the SEM figure of the Fe2O3 doping Tungstic anhydride. prepared in comparative example 1.
Fig. 7 is the SEM figure of the Fe2O3 doping Tungstic anhydride. prepared in comparative example 2.
Fig. 8 is the SEM figure of the Fe2O3 doping Tungstic anhydride. prepared in comparative example 3.
Detailed description of the invention
Further illustrate the present invention below in conjunction with specific embodiments and the drawings, but the present invention is not done any by embodiment
The restriction of form.Unless stated otherwise, the present invention uses reagent, method and apparatus are the art conventional reagent, method
And equipment.
Unless stated otherwise, agents useful for same of the present invention and material are commercial.
Embodiment 1
Being dissolved in 10ml deionized water by ammonium metatungstate commercially available for 3.5g, adding molecular weight is the polyvinylpyrrolidine of 1300000
Ketone (PVP), addition is 1g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 20KV, receiving range 15cm, fltting speed 0.02ml/min, obtain white cloth-like as-spun fibre；As-spun fibre is put
Evacuation 600 DEG C calcining in tube furnace, 3 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain three oxygen
Change tungsten nanofiber.The FeCl of preparation 0.03g/L3Solution, take 50ml add 0.5g tungsten oxide nanofibers, on warm table with
85 DEG C are soaked and filter after 3 hours, are finally dried 5 hours in 110 DEG C of air dry ovens, obtain the Tungstic anhydride. of trace iron doping
Nanofiber.
The photocatalyst prepared by this embodiment is carried out SEM, TEM-mapping, XRD and characterizes, result such as Fig. 1 ~ 3
Shown in.
Wherein, Fig. 1 (a) is the SEM figure of the tungsten trioxide nano fibrous web-like distribution prepared.Fig. 1 (b) is for carrying out trace iron
SEM figure after doping treatment.Can be seen that carrying out Fe2O3 doping processes the net-shaped not affecting tungsten trioxide nano fiber
Looks.
Fig. 2 is the TEM-mapping figure of the trace iron doping tungsten trioxide nano fiber using the method to prepare.At Fig. 2
In, it can be seen that tungsten, oxygen, three kinds of elements of ferrum are evenly distributed in above tungsten oxide nanofibers.
Fig. 3 is the pure Tungstic anhydride. using the method to prepare and the XRD figure of trace iron doping Tungstic anhydride..In figure 3, spread out
Firing angle peak at 23.1,23.5,24.3,26.5,28.9,33.2,34.1 and 41.9 ° is belonging respectively to monoclinic form tungsten oxide
(002), (020), (200), (120), (112), (022), the diffraction of (202) and (222) crystal face.Can be seen that the product of preparation
It is exactly Tungstic anhydride., and crystallinity is good.After carrying out Fe2O3 doping, changing does not occurs in diffraction maximum, it is seen that the ferrum of doping trace is also
The crystalline structure of Tungstic anhydride. will not be changed.
Embodiment 2
Being dissolved in 10ml deionized water by 3.5g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 1.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 20KV, receiving range 15cm, fltting speed 0.02ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain tungsten trioxide nano
Fiber.The FeCl of preparation 0.06g/L3Solution, takes 50ml and adds 0.5g tungsten oxide nanofibers, with 85 DEG C of immersions on warm table
Filtering after 3 hours, be finally dried 5 hours in 110 DEG C of air dry ovens, the tungsten trioxide nano obtaining trace iron doping is fine
Dimension.
Embodiment 3
Being dissolved in 10ml deionized water by 5.0g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 1.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 24KV, receiving range 15cm, fltting speed 0.02ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 550 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain tungsten trioxide nano
Fiber.The FeCl of preparation 0.09g/L3Solution, takes 50ml and adds 0.5g tungsten oxide nanofibers, with 80 DEG C of immersions on warm table
Filtering after 3 hours, be finally dried 6 hours in 110 DEG C of air dry ovens, the tungsten trioxide nano obtaining trace iron doping is fine
Dimension.
Embodiment 4
Being dissolved in 10ml deionized water by 3.5g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 2.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 24KV, receiving range 15cm, fltting speed 0.02ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain tungsten trioxide nano
Fiber.The FeCl of preparation 0.12g/L3Solution, takes 50ml and adds 0.5g tungsten oxide nanofibers, with 85 DEG C of immersions on warm table
Filtering after 3 hours, be finally dried 6 hours in 110 DEG C of air dry ovens, the tungsten trioxide nano obtaining trace iron doping is fine
Dimension.
Embodiment 5
Being dissolved in 10ml deionized water by 3.5g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 2.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 30KV, receiving range 15cm, fltting speed 0.05ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain tungsten trioxide nano
Fiber.The FeCl of preparation 0.15g/L3Solution, takes 50ml and adds 0.5g tungsten oxide nanofibers, with 90 DEG C of immersions on warm table
Filtering after 3 hours, be finally dried 7 hours in 110 DEG C of air dry ovens, the tungsten trioxide nano obtaining trace iron doping is fine
Dimension.
Comparative example 1:
Being dissolved in 10ml deionized water by 5g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 1g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft method of electrostatic spinning,
Voltage 30KV, receiving range 15cm, fltting speed 0.05ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain Tungstic anhydride..Due to
Precursor solution, not in ratio range of the present invention, occurs in that the adhesion situation such as Fig. 6.
Comparative example 2:
Being dissolved in 10ml deionized water by 1g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 0.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 30KV, receiving range 15cm, fltting speed 0.05ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain Tungstic anhydride..By
In precursor solution not in ratio range of the present invention, occur in that the beadlet such as Fig. 7.
Comparative example 3:
Being dissolved in 10ml deionized water by 3.5g ammonium metatungstate hydrate, adding molecular weight is the polyvinylpyrrolidone of 1300000
(PVP), addition is 2.5g, and stirring obtains precursor solution after being homogeneous transparent to solution；Subsequently by single shaft electrostatic spinning
Method, voltage 15KV, receiving range 10cm, fltting speed 0.2ml/min, obtain as-spun fibre；As-spun fibre is placed in tube furnace
Middle evacuation 600 DEG C calcining, 2 DEG C/min of programming rate, it is incubated 0.5 hour, naturally cools to room temperature, obtain tungsten trioxide nano
Fiber.Due to electrospinning parameters the most within the scope of the present invention, occurring in that the situation such as Fig. 8, fiber bending, diameter Distribution is not
All.
Embodiment 6
The Photocatalytic Degradation Property of methyl orange is verified:
Verification method: adding 150ml concentration in reactor is the methyl orange solution of 10mg/L, takes 50mg embodiment 1 ~ 5 respectively
Prepare trace iron doping tungsten trioxide nano fiber put into wherein (and carry out with unadulterated tungsten trioxide nano fiber right
Than), reach adsorption equilibrium after dark reaction 30min, then irradiate under 300W xenon lamp, every 30min takes a sample, then with ultraviolet-
Visible spectrophotometer is measured the absorbance of solution and calculates degradation rate.Shown in degradation results as Fig. 4 and Biao 1, wherein 0.001-
0.005 represent respectively be relative Fe2O3 doping content be 0.1%-0.5%.Fig. 5 is different Fe2O3 doping amount tungsten oxide nanofibers
Photocatalysis effect contrast, it can be seen that when relatively doping is 0.3%, catalytic effect promotes the highest.
The catalyst degradation rate prepared in table 1 embodiment 1 ~ 5
| Embodiment is numbered | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Degradation rate (%) | 64.1% | 77.5% | 94.6% | 91% | 80.7% |
Claims (10)
1. the preparation method of the tungsten trioxide nano fiber photocatalyst of a trace iron doping, it is characterised in that include as follows
Step:
S1., ammonium metatungstate being dissolved in water, adds polyvinylpyrrolidone, stirring obtains precursor solution；
S2. precursor solution in S1 is carried out electrostatic spinning, obtain as-spun fibre；
S3. the as-spun fibre calcining that will prepare in S2, obtains tungsten trioxide nano fiber after cooling；
S4., by tungsten trioxide nano fiber impregnation in S3 in iron salt solutions, described photocatalyst is obtained after drying；
In S1, ammonium metatungstate is (0.2 ~ 0.6) with the solid-to-liquid ratio of water: 1；The molecular weight of described polyvinylpyrrolidone is (1 ~ 2)
×106；Polyvinylpyrrolidone is (0.1 ~ 0.3) with the solid-to-liquid ratio of water: 1；
In S2 step electrostatic spinning, voltage is 18 ~ 30KV, and receiving range is 15cm, and fltting speed is 0.01 ~ 0.1ml/min；
In S4, the concentration of iron salt solutions is 0.03 ~ 0.3g/L, and ferrum is 0.1 ~ 1% relative to the mass fraction of Tungstic anhydride..
Preparation method the most according to claim 1, it is characterised in that ferrum relative to the mass fraction of Tungstic anhydride. is
0.3%。
Preparation method the most according to claim 1, it is characterised in that in S1, the molecular weight of polyvinylpyrrolidone is 1.3
×106。
Preparation method the most according to claim 1, it is characterised in that in S1, ammonium metatungstate is (0.35 with the solid-to-liquid ratio of water
~ 0.5): 1；Polyvinylpyrrolidone is (0.1 ~ 0.25) with the solid-to-liquid ratio of water: 1.
Preparation method the most according to claim 1, it is characterised in that in S3, calcining heat is 500 ~ 650 DEG C, programming rate
It is 1 ~ 5 DEG C/min, and is incubated 0.5 hour.
Preparation method the most according to claim 1, it is characterised in that in S4, dipping temperature is 80 ~ 90 DEG C, dip time is
2 ~ 4 hours.
Preparation method the most according to claim 1, it is characterised in that baking temperature is 110 DEG C, drying time is 5 ~ 8 little
Time.
Preparation method the most according to claim 1, it is characterised in that in S4, iron salt is iron chloride.
9. the tungsten trioxide nano of the trace iron doping that the arbitrary described preparation method of a claim 1 to 8 prepares is fine
Dimension photocatalyst.
10. the tungsten trioxide nano fiber photocatalyst of the trace iron doping described in claim 9 application in water pollution.
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| CN108714424A (en) * | 2018-05-14 | 2018-10-30 | 中国地质大学（北京） | A kind of preparation method of the three compound crystalline phase WO 3 film of oblique-six sides of Fe2O3 doping |
| CN108745356A (en) * | 2018-06-13 | 2018-11-06 | 齐鲁工业大学 | A kind of porous WO of precious metals pt load3Nanofiber photocatalyst and preparation method |
| CN113398927A (en) * | 2021-07-06 | 2021-09-17 | 浙江晨阳新材料有限公司 | Tungsten trioxide nanoparticle modified platinum alloy nano-string catalyst, preparation method and application |
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| CN108714424A (en) * | 2018-05-14 | 2018-10-30 | 中国地质大学（北京） | A kind of preparation method of the three compound crystalline phase WO 3 film of oblique-six sides of Fe2O3 doping |
| CN108745356A (en) * | 2018-06-13 | 2018-11-06 | 齐鲁工业大学 | A kind of porous WO of precious metals pt load3Nanofiber photocatalyst and preparation method |
| CN113398927A (en) * | 2021-07-06 | 2021-09-17 | 浙江晨阳新材料有限公司 | Tungsten trioxide nanoparticle modified platinum alloy nano-string catalyst, preparation method and application |
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