CN104056612A - Preparation method of metallic oxide/silicon dioxide hybridized nanofiber photocatalytic material - Google Patents
Preparation method of metallic oxide/silicon dioxide hybridized nanofiber photocatalytic material Download PDFInfo
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- CN104056612A CN104056612A CN201410239146.1A CN201410239146A CN104056612A CN 104056612 A CN104056612 A CN 104056612A CN 201410239146 A CN201410239146 A CN 201410239146A CN 104056612 A CN104056612 A CN 104056612A
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Abstract
The invention relates to a preparation method of a metallic oxide/silicon dioxide hybridized nanofiber photocatalytic material. The preparation method comprises the following steps: (1) dissolving polyvinylpyrrolidone powder into absolute ethyl alcohol, and performing magnetic stirring at room temperature until the polyvinylpyrrolidone powder is fully dissolved; (2) slowly adding precursors of tetraethyl orthosilicate and metallic oxide to the system in sequence, and violently stirring, so as to obtain a homogeneous spinning precursor solution; (3) putting the spinning precursor solution obtained from the step (2) into an injector, and regulating and controlling the voltage of a high-voltage power supply, so as to stably spray a spinning precursor in a pipe and obtain required electrospinning fiber; and (4) putting the electrospinning fiber obtained in the step (3) into a muffle furnace, calcining at room temperature at controlled heating rate, and finally, cooling in air to room temperature, so as to obtain the metallic oxide/silicon dioxide hybridized nanofiber photocatalytic material. The preparation method has the advantages of simple preparation technique and good stability and repetitiveness, and obtained hybridized nanofiber has the advantages of controllable morphology, high catalytic activity and easiness in recycling.
Description
Technical field
The invention belongs to nano material preparation and nano-catalytic field, relate to a kind of preparation method of metal oxide/SiO 2 hybrid nanofiber catalysis material, this hybrid material can be for photocatalytically degradating organic dye and sensor field.
Background technology
Silica nano fibrous material has good biocompatibility, and outstanding heat endurance and chemical stability, and the series of advantages such as larger specific area (80-400m2/g) have extensively far-reaching application at catalyst and adsorbing domain.Prepare silica nano fibrous method and mainly contain traditional template and the approach based on electrostatic spinning technique and high temperature temperature programmed control process.Electrostatic spinning technique refers to that polymer solution or melt are charged and produce deformation under high voltage electrostatic field, through the high-speed stretch of electric field force, solvent evaporates and a series of processes such as curing, finally being deposited on and receiving the process that forms polymer fiber on pole plate, is the method for preparing at present the quickness and high efficiency of nanometer stage material.High temperature temperature programmed control process is to prepare the common method of inorganic oxide.
The metal oxide (as zinc oxide, titanium dioxide, indium oxide, iron oxide, manganese dioxide and cupric oxide etc.) of one-dimensional nano structure is because of its unique structure and morphology characteristic, lower synthetic cost, excellent stability, high sensitiveness and unique optical characteristics and having a wide range of applications aspect photocatalytically degradating organic dye and sensor.But because the difficult recovery of metal oxide and the loss of these nano-scales are very fast, this defect part has affected its application in actual production life significantly.
Summary of the invention
The present invention will solve the shortcoming of above-mentioned prior art, a kind of preparation method of metal oxide/SiO 2 hybrid nanofiber catalysis material is provided, this hybrid material has that pattern is controlled, technique is simple, stability and reproducible feature, utilizes hybrid material that the method makes to have higher catalytic activity and be easy to and reclaims.
The present invention solves the technical scheme that its technical problem adopts: adopt following steps:
1) polyvinylpyrrolidonepowder powder is dissolved in absolute ethyl alcohol, room temperature condition lower magnetic force stirs until dissolve completely;
2) successively the presoma of ethyl orthosilicate and metal oxide is slowly added in above-mentioned system, vigorous stirring, obtains the spinning precursor solution of homogeneous phase;
3) by step 2) the spinning precursor solution of gained is encased in syringe, regulates the voltage of controlling high voltage source to make to manage the stable ejection of interior spinning presoma, just obtains the electrospinning fibre needing;
4) by step 3) electrospinning fibre of gained is placed in Muffle furnace, calcines and control heating rate from room temperature, finally in air atmosphere, is cooled to room temperature, just can obtain metal oxide/SiO 2 hybrid nanofiber catalysis material.
As preferably, the mass range of described polyvinylpyrrolidone is 1.4-2.0g, the volume of absolute ethyl alcohol is 12-18mL, and the addition of ethyl orthosilicate is 2.4-3.5mL, and the presoma content of metal oxide and the mass ratio of ethyl orthosilicate are 0.06-0.42.
As preferably, described step 3) in the time utilizing electrostatic spinning technique electrospinning fibre, the voltage of high voltage source is 7-18kV, and receiving system is 10-21cm to the distance of spinning syringe needle, and solution flow rate is 0.4-1.2mL/h.
As preferably, described step 4) in the time that electrospinning fibre is carried out to high-temperature calcination, be fired to 200 DEG C and be incubated 1-6 hour under this temperature from room temperature, atmosphere is air; Then temperature rises to 450-550 DEG C, and insulation 2-10 hour is finally cooled to room temperature in air atmosphere; Heating rate is 0.1-12 DEG C/min.
As preferably, described step 3) diameter of the electrospinning fibre that obtains is 800-2500nm.
Inventing useful effect is: the present invention prepares spinning presoma by sol-gel process, utilize electrostatic spinning technique to prepare electrospinning fibre, finally obtain Hybrid nanofibers in conjunction with temperature programmed control process, technology of preparing is simple, stability and reproducible, and the Hybrid nanofibers pattern that obtains is controlled and have higher catalytic activity and easily reclaim.
Brief description of the drawings
Fig. 1 is titania/silica Hybrid nanofibers hybrid material field emission scanning electron microscope and the transmission electron microscope photo that the present invention utilizes technique scheme to obtain.
Fig. 2 is titania/silica Hybrid nanofibers hybrid material field emission scanning electron microscope and the transmission electron microscope photo that the present invention utilizes technique scheme to obtain.
Fig. 3 is zinc oxide/SiO 2 hybrid hybridization material of Nano fiber field emission scanning electron microscope and the transmission electron microscope photo that the present invention utilizes technique scheme to obtain.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1: get 1.5g polyvinylpyrrolidone it is dissolved in 15mL absolute ethyl alcohol completely, add successively 2.5mL ethyl orthosilicate and 1.0mL butyl titanate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 7kV, receiving system is 10cm to the distance of spinning syringe needle, solution flow rate is 0.5mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 2 hours from room temperature with 0.5 DEG C/min, then continue to be warming up at 525 DEG C and be incubated 10 hours, finally in air atmosphere, be cooled to room temperature, obtain titania/silica Hybrid nanofibers, pattern as shown in Figure 1.
Embodiment 2: get 1.4g polyvinylpyrrolidone it is dissolved in 12mL absolute ethyl alcohol completely, add successively 2.5mL ethyl orthosilicate and 1.0mL butyl titanate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 7kV, receiving system is 10cm to the distance of spinning syringe needle, solution flow rate is 0.4mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 1 hour from room temperature with 0.1 DEG C/min, then continue to be warming up at 450 DEG C and be incubated 2 hours, finally in air atmosphere, being cooled to room temperature, obtaining titania/silica Hybrid nanofibers.
Embodiment 3: get 1.5g polyvinylpyrrolidone it is dissolved in 15mL absolute ethyl alcohol completely, add successively 2.5mL ethyl orthosilicate and 0.5mL butyl titanate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 7kV, receiving system is 10cm to the distance of spinning syringe needle, solution flow rate is 0.5mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 2 hours from room temperature with 0.5 DEG C/min, then continue to be warming up at 525 DEG C and be incubated 10 hours, finally in air atmosphere, be cooled to room temperature, obtain titania/silica Hybrid nanofibers, pattern as shown in Figure 2.
Embodiment 4: get 1.7g polyvinylpyrrolidone it is dissolved in 15mL absolute ethyl alcohol completely, add successively 3.0mL ethyl orthosilicate and 0.5mL butyl titanate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 12kV, receiving system is 15cm to the distance of spinning syringe needle, solution flow rate is 0.9mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 3 hours from room temperature with 6 DEG C/min, then continue to be warming up at 500 DEG C and be incubated 7 hours, finally in air atmosphere, being cooled to room temperature, obtaining titania/silica Hybrid nanofibers.
Embodiment 5: get 1.6g polyvinylpyrrolidone it is dissolved in 16mL absolute ethyl alcohol completely, add successively 2.6mL ethyl orthosilicate and 0.18g zinc acetate dihydrate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 10kV, receiving system is 12cm to the distance of spinning syringe needle, solution flow rate is 0.6mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 4 hours from room temperature with 0.6 DEG C/min, then continue to be warming up at 525 DEG C and be incubated 8 hours, finally in air atmosphere, be cooled to room temperature, obtain zinc oxide/SiO 2 hybrid nanofiber, pattern as shown in Figure 3.
Embodiment 6: get 1.4g polyvinylpyrrolidone it is dissolved in 14mL absolute ethyl alcohol completely, add successively 2.8mL ethyl orthosilicate and 0.20g tin chloride dihydrate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 12kV, receiving system is 12cm to the distance of spinning syringe needle, solution flow rate is 0.4mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 6 hours from room temperature with 1.0 DEG C/min, then continue to be warming up at 525 DEG C and be incubated 12 hours, finally in air atmosphere, being cooled to room temperature, obtaining tin ash/SiO 2 hybrid nanofiber.
Embodiment 7: get 2.0g polyvinylpyrrolidone it is dissolved in 18mL absolute ethyl alcohol completely, add successively 3.5mL ethyl orthosilicate and 0.20g tin chloride dihydrate, then adopt method of electrostatic spinning to carry out spinning to this spinning presoma, control spinning voltage is 18kV, receiving system is 21cm to the distance of spinning syringe needle, solution flow rate is 1.2mL/h, obtains electrospinning fibre.
Gained electrospinning fibre is placed in to Muffle furnace, in air atmosphere, be warming up to 200 DEG C and be incubated 6 hours from room temperature with 12 DEG C/min, then continue to be warming up at 550 DEG C and be incubated 12 hours, finally in air atmosphere, being cooled to room temperature, obtaining tin ash/SiO 2 hybrid nanofiber.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (6)
1. a preparation method for metal oxide/SiO 2 hybrid nanofiber catalysis material, is characterized in that adopting following steps:
1) polyvinylpyrrolidonepowder powder is dissolved in absolute ethyl alcohol, room temperature condition lower magnetic force stirs until dissolve completely;
2) successively the presoma of ethyl orthosilicate and metal oxide is slowly added in above-mentioned system, vigorous stirring, obtains the spinning precursor solution of homogeneous phase;
3) by step 2) the spinning precursor solution of gained is encased in syringe, regulates the voltage of controlling high voltage source to make to manage the stable ejection of interior spinning presoma, just obtains the electrospinning fibre needing;
4) by step 3) electrospinning fibre of gained is placed in Muffle furnace, calcines and control heating rate from room temperature, finally in air atmosphere, is cooled to room temperature, just can obtain metal oxide/SiO 2 hybrid nanofiber catalysis material.
2. the light-catalysed preparation method of a kind of metal oxide/SiO 2 hybrid nano-fiber material according to claim 1, the presoma that it is characterized in that described metal oxide is butyl titanate, zinc acetate dihydrate or tin chloride dihydrate, iron chloride, copper nitrate, inidum chloride.
3. the preparation method of a kind of metal oxide/SiO 2 hybrid nanofiber catalysis material according to claim 1, the mass range that it is characterized in that described polyvinylpyrrolidone is 1.4-2.0g, the volume of absolute ethyl alcohol is 12-18mL, the addition of ethyl orthosilicate is 2.4-3.5mL, and the presoma content of metal oxide is 0.03-0.42 with the ratio of the amount of substance of ethyl orthosilicate.
4. the preparation method of a kind of metal oxide/SiO 2 hybrid nanofiber catalysis material according to claim 1, it is characterized in that described step 3) in the time utilizing electrostatic spinning technique electrospinning fibre, the voltage of high voltage source is 7-18kV, receiving system is 10-21cm to the distance of spinning syringe needle, and solution flow rate is 0.4-1.2mL/h.
5. the light-catalysed preparation method of a kind of metal oxide/SiO 2 hybrid nano-fiber material according to claim 1, it is characterized in that described step 4) in the time that electrospinning fibre is carried out to high-temperature calcination, be fired to 200 DEG C and be incubated 1-5 hour under this temperature from room temperature, atmosphere is air; Then temperature rises to 450-550 DEG C, and insulation 2-12 hour is finally cooled to room temperature in air atmosphere; Heating rate is 0.1-12 DEG C/min.
6. the light-catalysed preparation method of a kind of metal oxide/SiO 2 hybrid nano-fiber material according to claim 1, is characterized in that described step 3) the electrospinning fibre diameter that obtains is 800-2500nm.
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Cited By (8)
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| CN104264282A (en) * | 2014-10-20 | 2015-01-07 | 济南大学 | Preparation method for silicon dioxide/tin dioxide rodlike fibers in core-shell structure |
| CN104817281A (en) * | 2015-04-22 | 2015-08-05 | 陕西科技大学 | Preparation method of orange-yellow photonic crystal structure color thin film with photo-catalytic effect |
| WO2017186201A1 (en) | 2016-04-26 | 2017-11-02 | Pardam, S.R.O. | Precursor fibers intended for preparation of silica fibers, method of manufacture thereof, method of modification thereof, use of silica fibers |
| CN107376888A (en) * | 2017-07-18 | 2017-11-24 | 中国科学院城市环境研究所 | A kind of flexible titanium oxide/silica/carbon composite nano-fiber film and preparation method thereof |
| CN110042500A (en) * | 2018-01-15 | 2019-07-23 | 哈尔滨工业大学 | A kind of preparation method of ferroso-ferric oxide/silica composite fiber microwave absorbing material |
| CN115530183A (en) * | 2022-10-12 | 2022-12-30 | 南方科技大学 | C/N @ titanium dioxide, metal oxide doped C/N @ titanium dioxide, nano fiber thereof, preparation method and sterilization equipment |
| WO2023077673A1 (en) * | 2021-11-05 | 2023-05-11 | 岭东核电有限公司 | Membrane filtering material, preparation method therefor, and use thereof in treatment of aerosol |
| CN116377606A (en) * | 2023-04-25 | 2023-07-04 | 武汉纺织大学 | Spiral antibacterial nanofiber as well as preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104264282A (en) * | 2014-10-20 | 2015-01-07 | 济南大学 | Preparation method for silicon dioxide/tin dioxide rodlike fibers in core-shell structure |
| CN104817281A (en) * | 2015-04-22 | 2015-08-05 | 陕西科技大学 | Preparation method of orange-yellow photonic crystal structure color thin film with photo-catalytic effect |
| WO2017186201A1 (en) | 2016-04-26 | 2017-11-02 | Pardam, S.R.O. | Precursor fibers intended for preparation of silica fibers, method of manufacture thereof, method of modification thereof, use of silica fibers |
| CN107376888A (en) * | 2017-07-18 | 2017-11-24 | 中国科学院城市环境研究所 | A kind of flexible titanium oxide/silica/carbon composite nano-fiber film and preparation method thereof |
| CN107376888B (en) * | 2017-07-18 | 2020-04-24 | 中国科学院城市环境研究所 | Flexible titanium oxide/silicon oxide/carbon composite nanofiber membrane and preparation method thereof |
| CN110042500A (en) * | 2018-01-15 | 2019-07-23 | 哈尔滨工业大学 | A kind of preparation method of ferroso-ferric oxide/silica composite fiber microwave absorbing material |
| WO2023077673A1 (en) * | 2021-11-05 | 2023-05-11 | 岭东核电有限公司 | Membrane filtering material, preparation method therefor, and use thereof in treatment of aerosol |
| CN115530183A (en) * | 2022-10-12 | 2022-12-30 | 南方科技大学 | C/N @ titanium dioxide, metal oxide doped C/N @ titanium dioxide, nano fiber thereof, preparation method and sterilization equipment |
| CN115530183B (en) * | 2022-10-12 | 2023-11-07 | 南方科技大学 | C/N@ titanium dioxide, metal oxide doped C/N@ titanium dioxide, nanofiber thereof, preparation method and sterilization equipment |
| CN116377606A (en) * | 2023-04-25 | 2023-07-04 | 武汉纺织大学 | Spiral antibacterial nanofiber as well as preparation method and application thereof |
| CN116377606B (en) * | 2023-04-25 | 2024-03-22 | 武汉纺织大学 | Spiral antibacterial nanofiber as well as preparation method and application thereof |
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Application publication date: 20140924 |