CN111850739A - Preparation method of tungsten trioxide/niobium pentoxide nanofiber - Google Patents
Preparation method of tungsten trioxide/niobium pentoxide nanofiber Download PDFInfo
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- CN111850739A CN111850739A CN202010221233.XA CN202010221233A CN111850739A CN 111850739 A CN111850739 A CN 111850739A CN 202010221233 A CN202010221233 A CN 202010221233A CN 111850739 A CN111850739 A CN 111850739A
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- tungsten trioxide
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 76
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000002121 nanofiber Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 10
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims abstract description 8
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 18
- 238000009987 spinning Methods 0.000 claims description 11
- 238000001523 electrospinning Methods 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 25
- 239000003054 catalyst Substances 0.000 description 21
- 238000011161 development Methods 0.000 description 6
- 230000018109 developmental process Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000011973 solid acid Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000007210 heterogeneous catalysis Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 238000006317 isomerization reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000029936 alkylation Effects 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006384 oligomerization reaction Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B01J35/58—
-
- B01J35/613—
-
- B01J35/647—
Abstract
The invention discloses a preparation method of tungsten trioxide/niobium pentoxide nano-fibers, which comprises the following steps: sequentially dissolving niobium pentachloride, phosphotungstic acid and polyvinylpyrrolidone in N, N-dimethylformamide to prepare a mixed solution, stirring for 6-8 h to make the mixed solution uniform, then carrying out electrostatic spinning, and calcining the spun product in a muffle furnace at 600 ℃ for 1h to prepare the tungsten trioxide/niobium pentoxide nanofiber. The preparation method disclosed by the invention is simple in preparation steps and low in cost, and the prepared tungsten trioxide/niobium pentoxide nanofiber is controllable in shape, large in specific surface area, high in catalytic activity and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to a preparation method of tungsten trioxide/niobium pentoxide nano fibers, and specifically relates to a preparation method of tungsten trioxide/niobium pentoxide nano fibers by adopting an electrostatic spinning technology.
Background
Catalytic chemistry plays a vital role in chemical industry and even world economy, and chemical raw materials can be converted into chemicals and energy with high added values in an economic, efficient and environment-friendly manner through a catalytic process. According to statistics, 90% of the catalytic processes are heterogeneous catalysis, and the heterogeneous catalysis has important application in the fields of chemicals, foods, medicines, even agriculture, automobile industry and the like. In recent years, heterogeneous catalysis is also continuously open in many emerging fields, such as fuel cells, green chemistry, nanochemistry, and biotechnology. Meanwhile, with the development of economy, environmental problems and energy crisis become more serious day by day, the continuous consumption of petrochemical energy, the pollution of air and water resources and the like become the bottleneck of sustainable development, and the development of a novel efficient heterogeneous catalysis process and a catalyst becomes one of research hotspots which are suitable for the requirements of society and science and technology development.
In practical application, because the reaction conditions are harsh, the components of reactants and products are complex, and the impurity content is high, the stability and the regeneration performance of the catalyst are very important. Specifically, many reactions are high temperature and high pressure processes, and by-products such as water vapor, sulfides and nitrides are generated, so that the surface area of the catalyst is sharply reduced, and the active center is poisoned and loses activity.
The solid acid catalyst is a non-toxic catalyst which is not easy to corrode candle equipment, can be recycled, is environment-friendly, and has wide industrial application prospect. Solid acids are used in the largest quantities in the petroleum processing and petrochemical industries, and the successful synthesis of a series of novel solid acid catalysts makes the petroleum processing technology change day by day. Meanwhile, the solid acid catalyst is also widely applied to other various industrial catalytic processes. However, the specific surface of the currently synthesized solid acid catalyst is relatively small, the stability is poor, and the catalytic activity is low, so that the development of a solid acid catalyst with high stability and high catalytic activity becomes a problem to be solved urgently. For this reason, people in recent years have come toSupported oxide type solid super acidic catalyst (e.g. WO)3/ZrO2) The preparation and the catalytic performance of the catalyst are researched a lot, and the results show that the catalyst has excellent activity and selectivity for acid catalytic reactions such as isomerization, alkylation, oligomerization, esterification and the like.
Research has shown that the development of highly efficient catalysts stems from the exploration of new active species and also from the tailored design of the catalyst morphology. The large specific surface area of the catalyst with the nano-morphology structure can increase the active sites and the reaction centers on the surface of the catalyst, and agglomeration is not caused, so that the catalytic activity of the photocatalyst is remarkably enhanced, and the preparation of nano-structure catalysts (nanorods, nanospheres, nanofibers and the like) with various morphologies becomes a hotspot of research in the field. Among them, the one-dimensional nano fibrous structure has a large length-diameter ratio and a relatively large specific surface area, and shows a series of unique chemical and physical properties. At present, there are many methods for preparing nanofibers, such as: solvothermal methods, spinning methods, arc evaporation methods, compound pyrolysis methods, and the like. Among them, the electrospinning method is one of the simpler and more effective methods for preparing nanofibers.
Niobium pentoxide (Nb)2O5) The catalyst has the advantages of strong acid surface and high stability in various acid catalysis of aqueous media, has wide application value in the industrial synthesis fields of isomerization, esterification, dehydration and the like, and attracts people's attention. So far, reports of preparing tungsten trioxide/niobium pentoxide nanofibers by adopting an electrostatic spinning technology are not found.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a preparation method of a supported solid super acidic tungsten trioxide/niobium pentoxide nanofiber. Mainly solves the problems of small specific surface area of solid super strong acid, poor thermal stability, easy loss of components, relatively low catalytic activity and the like.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of tungsten trioxide/niobium pentoxide nano-fibers comprises the following steps:
sequentially dissolving niobium pentachloride, phosphotungstic acid and polyvinylpyrrolidone in N, N-dimethylformamide to prepare a mixed solution, stirring for 6-8 h to make the mixed solution uniform, then carrying out electrostatic spinning, and calcining the spun product in a muffle furnace at 600 ℃ for 1h to prepare the tungsten trioxide/niobium pentoxide nanofiber.
As a preferable scheme, the mass ratio of the niobium pentachloride to the N, N-dimethylformamide in the mixed solution is 1: 10.
Preferably, the mass ratio of phosphotungstic acid to N, N-dimethylformamide in the mixed solution is 0.009: 1-0.027: 1.
In a preferred embodiment, the mass ratio of polyvinylpyrrolidone to N, N-dimethylformamide in the mixed solution is 0.14: 1.
As a preferable mode, the polyvinylpyrrolidone has an average molecular weight of 1300000.
Preferably, the receiving end of the electrostatic spinning is an aluminum foil with a surface of 25cm × 25cm covered with a polytetrafluoroethylene film, the other end of the electrostatic spinning is connected with a positive electrode, the voltage used is 20kV, the distance between the two electrodes is 15cm, the spinning speed is 5 μ L/min, and the specification of a spinning needle head is 22G.
As a preferable scheme, the ambient temperature of the electrostatic spinning is 30-40 ℃, and the relative humidity of air is 40-50%.
As a preferable scheme, the nanofiber obtained by electrostatic spinning is transferred to a muffle furnace for roasting, and the temperature rise speed is 10-15 ℃/min.
In a preferred embodiment, the atmosphere in which the nanofibers obtained by electrospinning are calcined in a muffle furnace is air.
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art, the tungsten trioxide/niobium pentoxide nanofiber supported solid super acidic catalyst with large length-diameter ratio and good thermal stability is successfully synthesized, the problems of small specific surface area, poor thermal stability, easy component loss, relatively low catalytic activity and the like of the solid super acidic catalyst are effectively solved, and the tungsten trioxide/niobium pentoxide nanofiber supported solid super acidic catalyst can be used for heterogeneous catalytic processes such as isomerization, alkylation, oligomerization and esterification.
Drawings
FIG. 1 is an SEM photograph of a sample obtained in example 1 of the present invention.
FIG. 2 is an XRD pattern of a sample obtained in example 1 of the present invention.
FIG. 3 is an XPS chart of a sample obtained in example 1 of the present invention.
FIG. 4 is a graph showing the nitrogen adsorption isotherm and the pore size distribution of the sample obtained in example 1 of the present invention.
Detailed Description
The following examples are given to illustrate specific embodiments of the present invention in detail. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
0.25g of niobium pentachloride, 0.067g of phosphotungstic acid and 0.35g of polyvinylpyrrolidone are sequentially dissolved in 2.5g N, N-dimethylformamide to prepare a mixed solution, and the mixed solution is stirred for 6 hours to be called as a uniform solution. And (3) carrying out electrostatic spinning on the obtained solution, wherein the receiving end of the electrostatic spinning is an aluminum foil with a surface of 25cm multiplied by 25cm covered by a polytetrafluoroethylene film, the other end of the electrostatic spinning is connected with a positive electrode, the voltage is 20kV, the distance between the two electrodes is 15cm, the spinning speed is 5 mu L/min, and the specification of a spinning needle head is 22G. The ambient temperature of the electrospinning was 30 ℃ and the relative air humidity was 40%. And transferring the nanofiber obtained by electrostatic spinning into a muffle furnace to be roasted for 1h at the temperature of 600 ℃, thus obtaining the tungsten trioxide/niobium pentoxide nanofiber. The temperature rise speed of the muffle furnace is 10 ℃/min, and the roasting atmosphere is air.
Example 2
0.25g of niobium pentachloride, 0.045g of phosphotungstic acid and 0.35g of polyvinylpyrrolidone are sequentially dissolved in 2.5g N, N-dimethylformamide to prepare a mixed solution, and the mixed solution is stirred for 6 hours to be called as a uniform solution. And (3) carrying out electrostatic spinning on the obtained solution, wherein the receiving end of the electrostatic spinning is an aluminum foil with a surface of 25cm multiplied by 25cm covered by a polytetrafluoroethylene film, the other end of the electrostatic spinning is connected with a positive electrode, the voltage is 20kV, the distance between the two electrodes is 15cm, the spinning speed is 5 mu L/min, and the specification of a spinning needle head is 22G. The ambient temperature of the electrospinning was 30 ℃ and the relative air humidity was 50%. And transferring the nanofiber obtained by electrostatic spinning into a muffle furnace to be roasted for 1h at the temperature of 600 ℃, thus obtaining the tungsten trioxide/niobium pentoxide nanofiber. The temperature rise speed of the muffle furnace is 10 ℃/min, and the roasting atmosphere is air.
Example 3
0.25g of niobium pentachloride, 0.022g of phosphotungstic acid and 0.35g of polyvinylpyrrolidone are sequentially dissolved in 2.5g N, N-dimethylformamide to prepare a mixed solution, and the mixed solution is stirred for 8 hours to be called as a uniform solution. And (3) carrying out electrostatic spinning on the obtained solution, wherein the receiving end of the electrostatic spinning is an aluminum foil with a surface of 25cm multiplied by 25cm covered by a polytetrafluoroethylene film, the other end of the electrostatic spinning is connected with a positive electrode, the voltage is 20kV, the distance between the two electrodes is 15cm, the spinning speed is 5 mu L/min, and the specification of a spinning needle head is 22G. The ambient temperature of the electrospinning was 40 ℃ and the relative air humidity was 40%. And transferring the nanofiber obtained by electrostatic spinning into a muffle furnace to be roasted for 1h at the temperature of 600 ℃, thus obtaining the tungsten trioxide/niobium pentoxide nanofiber. The temperature rise speed of the muffle furnace is 15 ℃/min, and the roasting atmosphere is air.
Characterization of tungsten trioxide/niobium pentoxide nanofibers
The tungsten trioxide/niobium pentoxide nanofibers prepared in example 1 were subjected to microscopic morphology testing using a JSM-6510 type scanning electron microscope. As can be seen from figure 1, the prepared sample is fibrous, the diameter of the nanofiber is 200-300 nm, the length of the nanofiber is tens of microns, and the possibility of large specific surface area and high catalytic activity of the sample is provided.
The crystal structure of example 1 was analyzed using an ULTIMA type IV X-ray diffractometer. As can be seen from fig. 2, the tungsten trioxide/niobium pentoxide nanofibers do not have a diffraction peak of tungsten trioxide clearly in comparison to the pure niobium pentoxide fibers, because the tungsten trioxide is distributed more uniformly in the fibers and forms a solid solution with niobium pentoxide at high temperature. Meanwhile, the diffraction peak intensities of the (180), (200) and (181) crystal planes of niobium pentoxide are reduced, but the diffraction peak of the (001) crystal plane is obviously enhanced and widened due to the existence of tungsten trioxide, indicating that the tungsten trioxide component exists in the nanofiber.
Tungsten trioxide/niobium pentoxide nanofibers produced in example 1 were tabulated using K-Alpha type X-ray photoelectron spectroscopy (XPS) And (6) performing surface element analysis. From the XPS chromatogram (FIG. 3), it can be seen that tungsten trioxide/niobium pentoxide, in addition to containing Nb, O and C, has a characteristic peak of W4f in the vicinity of the binding energy of 37 eV. As can be seen from the high resolution spectrum of W4f, the absorption peaks at the binding energies of 37.8eV and 35.8eV are W4f5/2And W4f7/2The characteristic peak indicates that the tungsten element in the tungsten trioxide/niobium pentoxide nano-fiber is W6+The form exists.
The specific surface area and pore structure of the tungsten trioxide/niobium pentoxide nanofibers prepared in example 1 were analyzed using a model ASAP2460 nitrogen adsorber. The specific surface area of the tungsten trioxide/niobium pentoxide nano-fiber calculated by a BET method is 24.5m2(ii) in terms of/g. The results of BJH desorption pore size distribution (inset) (fig. 4) show that the average pore size of the tungsten trioxide/niobium pentoxide nanofibers is about 17 nm.
It is to be understood that the above embodiments are merely illustrative for clarity of description and are not restrictive. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are possible within the scope of the invention as claimed.
Claims (9)
1. A preparation method of tungsten trioxide/niobium pentoxide nano-fibers is characterized by comprising the following steps:
sequentially dissolving niobium pentachloride, phosphotungstic acid and polyvinylpyrrolidone in N, N-dimethylformamide to prepare a mixed solution, stirring for 6-8 h to make the mixed solution uniform, then carrying out electrostatic spinning, and calcining the spun product in a muffle furnace at 600 ℃ for 1h to prepare the tungsten trioxide/niobium pentoxide nanofiber.
2. The method for preparing the tungsten trioxide/niobium pentoxide nanofiber as claimed in claim 1, wherein the mass ratio of niobium pentachloride to N, N-dimethylformamide in the mixed solution is 1: 10.
3. The preparation method of the tungsten trioxide/niobium pentoxide nanofiber as claimed in claim 1, wherein the mass ratio of phosphotungstic acid to N, N-dimethylformamide in the mixed solution is 0.009: 1-0.027: 1.
4. The method for preparing tungsten trioxide/niobium pentoxide nanofibers according to claim 1, wherein the mass ratio of polyvinylpyrrolidone to N, N-dimethylformamide in the mixed solution is 0.14: 1.
5. The method of claim 1, wherein the polyvinylpyrrolidone has an average molecular weight of 1300000.
6. The method for preparing the tungsten trioxide/niobium pentoxide nanofiber as claimed in claim 1, wherein the receiving end of the electrostatic spinning is an aluminum foil with a surface of 25cm × 25cm covered with a polytetrafluoroethylene film, the other end is connected with a positive electrode, the voltage used is 20kV, the distance between the two electrodes is 15cm, the spinning speed is 5 μ L/min, and the specification of the spinning needle is 22G.
7. The method for preparing the tungsten trioxide/niobium pentoxide nanofiber as claimed in claim 1, wherein the ambient temperature of the electrospinning is 30 to 40 ℃ and the relative humidity of air is 40 to 50%.
8. The method for preparing the tungsten trioxide/niobium pentoxide nanofiber according to claim 1, wherein the nanofiber obtained by electrospinning is transferred to a muffle furnace and calcined, and the temperature rise rate is 10-15 ℃/min.
9. The method for preparing the tungsten trioxide/niobium pentoxide nanofibers according to claim 1, wherein the atmosphere in which the nanofibers obtained by electrospinning are calcined in a muffle furnace is air.
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CN112808261A (en) * | 2021-02-08 | 2021-05-18 | 长江师范学院 | Preparation method of nest-shaped niobium oxide |
WO2022120578A1 (en) * | 2020-12-08 | 2022-06-16 | Dic Corporation | Niobium oxide particles and method for producing niobium oxide particles |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4233139A (en) * | 1978-07-25 | 1980-11-11 | Exxon Research & Engineering Co. | Acid catalyzed hydrocarbon conversion processes utilizing a catalyst comprising a Group IVB, VB or VIB metal oxide on an inorganic refractory oxide support |
JPH09263554A (en) * | 1996-03-29 | 1997-10-07 | Tsushosangyosho Kiso Sangyokyokucho | Production of ethanol |
US20100147684A1 (en) * | 2008-12-12 | 2010-06-17 | Electronics And Telecommunications Research Institute | Ultra-sensitive gas sensor using oxide semiconductor nanofiber and method of fabricating the same |
CN107460562A (en) * | 2017-08-02 | 2017-12-12 | 肇庆市华师大光电产业研究院 | One-step method prepares Copper-cladding Aluminum Bar tungstic acid composite nano-fiber material |
CN108172796A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of nanometer fibrous niobium pentaoxide/sulphur composite positive pole |
-
2020
- 2020-03-26 CN CN202010221233.XA patent/CN111850739A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4233139A (en) * | 1978-07-25 | 1980-11-11 | Exxon Research & Engineering Co. | Acid catalyzed hydrocarbon conversion processes utilizing a catalyst comprising a Group IVB, VB or VIB metal oxide on an inorganic refractory oxide support |
JPH09263554A (en) * | 1996-03-29 | 1997-10-07 | Tsushosangyosho Kiso Sangyokyokucho | Production of ethanol |
US20100147684A1 (en) * | 2008-12-12 | 2010-06-17 | Electronics And Telecommunications Research Institute | Ultra-sensitive gas sensor using oxide semiconductor nanofiber and method of fabricating the same |
CN107460562A (en) * | 2017-08-02 | 2017-12-12 | 肇庆市华师大光电产业研究院 | One-step method prepares Copper-cladding Aluminum Bar tungstic acid composite nano-fiber material |
CN108172796A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of nanometer fibrous niobium pentaoxide/sulphur composite positive pole |
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WO2022120578A1 (en) * | 2020-12-08 | 2022-06-16 | Dic Corporation | Niobium oxide particles and method for producing niobium oxide particles |
CN112808261A (en) * | 2021-02-08 | 2021-05-18 | 长江师范学院 | Preparation method of nest-shaped niobium oxide |
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