CN102125826A - Photocatalyst material diaphragm and preparation method thereof - Google Patents
Photocatalyst material diaphragm and preparation method thereof Download PDFInfo
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- CN102125826A CN102125826A CN 201010578896 CN201010578896A CN102125826A CN 102125826 A CN102125826 A CN 102125826A CN 201010578896 CN201010578896 CN 201010578896 CN 201010578896 A CN201010578896 A CN 201010578896A CN 102125826 A CN102125826 A CN 102125826A
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Abstract
The invention relates to a photocatalyst material diaphragm and a preparation method thereof, and the method comprises the following steps: using carbon fibers as a matrix material for growing and immobilizing a titanium dioxide photocatalyst, firstly performing activation pretreatment on the carbon fibers, then placing the carbon fibers after activation in the middle of a chemical gas phase reaction chamber, utilizing argon gas or nitrogen gas as a carrier gas, introducing titanium tetraisopropoxide into the reaction chamber, performing chemical vapor deposition, getting the material loaded with the titanium dioxide photocatalyst on the carbon fibers, further weaving the titanium dioxide photocatalyst material into a film according to the conventional method, further fixing the film by inner and outer rings of supports, and further getting the photocatalyst material diaphragm. The photocatalyst material diaphragm obtained through the method can solve the loading problem of the titanium dioxide photocatalyst material in actual use, and simultaneously well utilize high strength, higher thermal stability, chemical inertness and high-activity adsorption capacity of the carbon fibers.
Description
Technical field
The present invention relates to a kind of photocatalyst material diaphragm and preparation method thereof.
Background technology
As in purifying air and the most thorough otherwise effective technique of water pollutant, the conductor photocatalysis technology has become the research in present environmental pollution improvement field and has used focus.
The focal issue of using photocatalysis material of titanium dioxide concentrates on photocatalysis efficiency and the catalyst immobilization that how to improve nano titanium oxide.The factor that influences optically catalytic TiO 2 efficient mainly comprises: the crystal formation of (1) photocatalyst of titanium dioxide material, the surface characteristic of (2) photocatalyst material, the crystallite dimension of (3) photocatalyst material.The major technique that existing method prepares nano titanium dioxide photocatalyst comprises: hydro-thermal method, sol-gel process, electrochemistry anodic oxidation, vapor phase method.Use above-mentioned preparation method, obtained the nanometer titanium dioxide photocatalysis material of nano particle, nano wire, nanotube and nano thin-film structure, these work provide possibility for the catalytic mechanism of further investigation nano titanium oxide, and show that the nano titanium oxide photocatalyst has plurality of advantages: but cost is low, nonhazardous, greatly specific surface, the sensitization of can mixing, good stability and catalytic mechanism research are deep, are present most widely used photocatalyst materials.
But utilize above-mentioned preparation method, can't satisfy practical application, main weak point is: material structure that (1) prepares and dimensional controllability are not high, (2) can not prepare in enormous quantities, (4) sample structure for preparing and performance are difficult for further modulation, influence the raising of catalytic efficiency, the nanometer titania that (3) obtain all needs to be solidificated on other support materials and could drop into application.
In real world applications, a loading problem that greatest problem is exactly a photocatalyst that runs into.Because even if the nano titanium oxide photocatalyst has good photocatalytic degradation performance, load on the position that needs if in use can not guarantee it, but along with processing procedure constantly runs off, its service efficiency will reduce constantly so.
Therefore, realizing photocatalyst preparation and load how effectively, easily, is a big problem that must solve in the photocatalytic applications.
Load on photocatalyst of titanium dioxide on the carbon fibre material and can be effective to handle pollutant in gas phase or the liquid-phase system, but the photocatalytic degradation reaction is a kind of surface reaction, so the material that uses must have enough big surface, could guarantee the effect of catalytic degradation.And membrane technology and can solve this actual needs well, so photocatalyst of titanium dioxide material diaphragm becomes a basic equipment module in the photocatalyst application technology.
Load and efficient use problem for solving the photocatalyst of titanium dioxide material the invention provides a kind of photocatalyst material diaphragm and preparation method thereof.
Summary of the invention
The object of the invention is, a kind of photocatalyst material diaphragm and preparation method thereof is provided, this method is with the matrix material of carbon fiber as growth and immobilized photocatalyst of titanium dioxide, earlier carbon fiber being carried out pre-activated handles, carbon fiber after will activating then is placed on the centre of chemical gas phase reaction chamber, utilize argon gas or nitrogen to be carrier gas, tetraisopropoxy titanium is fed in the reative cell, through chemical vapour deposition (CVD), obtaining load on carbon fiber has the material of photocatalyst of titanium dioxide, again the photocatalyst of titanium dioxide material is woven film forming according to a conventional method, be fixed by the Internal and external cycle support again, can obtain the photocatalyst material diaphragm.The photocatalyst material diaphragm that obtains by this method has solved photocatalyst of titanium dioxide material loading problem in actual use, has also utilized the high strength of carbon fiber, higher heat endurance, chemical inertness and high activity adsorption capacity simultaneously well.
A kind of photocatalyst material diaphragm of the present invention, adopt chemical vapour deposition technique carried titanium dioxide photocatalyst on carbon fiber, can obtain the material of photocatalyst of titanium dioxide, again the photocatalyst of titanium dioxide material is woven according to a conventional method, get final product by interior support arm is fixing, concrete operations follow these steps to carry out:
A, carbon fiber is carried out pre-activated according to a conventional method handle, activation temperature is 600-950 ℃, and soak time is 5-15 minute;
B, will activate pretreated carbon fiber and be sent in the chemical vapor deposition reaction chamber, rise to 250-750 ℃ with 50 ℃/minute heating rates, with argon gas or nitrogen is carrier gas, tetraisopropoxy titanium is fed in the reative cell, and gas flow is 400-2000sccm, and the reaction time is 5-20 minute, after reaction is finished, naturally cooling is cooled to room temperature, and through chemical vapour deposition technique, growth obtains the photocatalyst of titanium dioxide material in the hole of surface and centre;
C, step b is obtained the photocatalyst of titanium dioxide material according to a conventional method by craft or mechanical system mesh grid trellis two dimension carbon-fiber film (2) again, the outer edge of latticed two-dimentional carbon-fiber film (2) is fixing with outer coil support (1), and the inside edge of latticed two-dimentional carbon-fiber film (2) can obtain the photocatalyst material diaphragm with interior coil support (3) is fixing.
A kind of preparation method of photocatalyst material diaphragm follows these steps to carry out:
A, carbon fiber is carried out pre-activated according to a conventional method handle, activation temperature is 600-950 ℃, and soak time is 5-15 minute;
B, will activate pretreated carbon fiber and be sent in the chemical vapor deposition reaction chamber, rise to 250-750 ℃ with 50 ℃/minute heating rates, with argon gas or nitrogen is carrier gas, tetraisopropoxy titanium is fed in the reative cell, and gas flow is 400-2000sccm, and the reaction time is 5-20 minute, after reaction is finished, naturally cooling is cooled to room temperature, and through chemical vapour deposition technique, growth obtains the photocatalyst of titanium dioxide material in the hole of surface and centre;
C, step b is obtained the photocatalyst of titanium dioxide material again and be woven into latticed two-dimentional carbon-fiber film (2) by craft or mechanical system according to a conventional method, to have the hole in the latticed two-dimentional carbon-fiber film (2) again, the outer edge of latticed two-dimentional carbon-fiber film (2) is fixing with outer coil support (1), and the inside edge, hole in the middle of the latticed two-dimentional carbon-fiber film (2) can obtain the photocatalyst material diaphragm with interior coil support (3) is fixing.
For fixing or portable, i.e. growth on one side is Yi Bian move continuously in CVD chamber for carbon fiber after the step b activation.
The anatase structured shared ratio of titanium dioxide is 90% in the titanium dioxide that the reaction growth obtains on the step b carbon fiber.
The mesh size of step c mesh grid trellis two dimension carbon-fiber film (2) is the 50-100 order.
Step c mesh grid trellis two dimension carbon fiber (2) is the one deck or the multilayer of intersecting.
Scribble conducting resinl on interior coil support (3) edge of step c mesh grid trellis two dimension carbon-fiber film (2).
The outer coil support (1) of step c is made into random geometry with interior coil support (3).
The preparation method of photocatalyst material diaphragm of the present invention, prepare the carbon fiber of carried titanium dioxide photocatalyst earlier by chemical vapour deposition (CVD), liquid phase process and spraying method, then carbon fiber knit is become the photocatalyst material film of two-dimensional structure, become the outer coil support and the interior coil support of fixed light catalyst material diaphragm again with suitable materials processing, at last photocatalyst material film and outer coil support and interior coil support are linked together, constituted the photocatalyst material diaphragm at last.
The preparation method of photocatalyst material diaphragm of the present invention, carbon fiber after the activation can be fixed in CVD chamber, also can be portable, i.e. growth on one side, move on one side continuously, can guarantee the continuity that carbon fiber is sent into and the continuity of growth like this.Wherein, the amount of the photocatalyst of titanium dioxide that growth obtains on carbon fiber is directly proportional with growth time and carrier gas flux.The phase structure of the photocatalyst of titanium dioxide that growth obtains on carbon fiber, relevant with reaction temperature, in order to obtain the titanium dioxide that most of phase structure is an anatase, needing the temperature of control growth is 250-750 ℃.
Using the method for the invention load has the carbon fiber of photocatalyst of titanium dioxide to prepare the photocatalyst material diaphragm, primary structure comprises film 2, outer coil support 1 and interior coil support 3, in outer coil support 1 and the interior coil support 3, having a support at least is that conductor material is made.Photocatalyst material film 2 is to be become by the carbon fiber knit of carried titanium dioxide; The braiding of photocatalyst material film can be one deck in the diaphragm, also can be the intersection multilayer.
Load on anatase structured photocatalyst of titanium dioxide on the carbon fiber by what the method for the invention obtained, solve photocatalyst of titanium dioxide material loading problem in actual use, also utilized the high strength of carbon fiber, higher heat endurance, chemical inertness and high activity adsorption capacity simultaneously well.
Description of drawings
Fig. 1 is the structural representation of photocatalyst material diaphragm of the present invention.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is prepared the process of photocatalyst material diaphragm, and the structure of photocatalyst material diaphragm is described in further detail.
Take by weighing the 50g polyacrylonitrile-based carbon fibre, join in 1 liter of distilled water and evenly stirred 5 minutes, then in ultrasonic cleaner to its ultrasonic cleaning 10 minutes, carbon fiber after cleaning is taken out from distilled water, put in the dilute hydrochloric acid solution that concentration is 0.15mol/L, soaked 24 hours, extremely neutral with distilled water flushing again, in 105 ℃ of oven dry down of temperature, carbon fiber after the oven dry is put into reacting furnace, with 20 ℃/minute heating rates the reacting furnace temperature is increased to 600 ℃, kept 5 minutes down at 600 ℃ then, carbon fiber is carried out pre-activated handle;
To activate pretreated carbon fiber is sent in the CVD chamber immediately, rise to 250 ℃ of reaction temperatures with 50 ℃/minute heating rates, with nitrogen is carrier gas, tetraisopropoxy titanium is sent in the reative cell, the flow of carrier gas is 400sccm, in the reaction time of 550 ℃ of temperature is 5 minutes, after reaction is finished, naturally cooling is cooled to room temperature, in the hole of surface and centre, grow, can obtain loading on the anatase structured photocatalyst of titanium dioxide material on the polyacrylonitrile-based carbon fibre;
To obtain the photocatalyst of titanium dioxide material again and be woven into the latticed two-dimentional carbon-fiber film 2 that area is 150mm * 150mm by manual mode according to a conventional method, the mesh size is 50 orders, be the 30mm hole with having diameter in the latticed two-dimentional carbon-fiber film 2 again, interior coil support 3 is placed in the latticed two-dimentional carbon-fiber film 2 in the circular opening, coat conducting resinl at its outward flange, again outer coil support 1 is placed on the outer edge place of latticed two-dimentional carbon-fiber film 2, with conducting resinl that outer coil support 1 is bonding, the carbon-fiber film of dismissing outer coil support 1 periphery at last can obtain the photocatalyst material diaphragm.
Take by weighing the 100g viscose-based carbon fiber, join in 2.5 liters of distilled water evenly and stirred 8 minutes, then in ultrasonic cleaner to its ultrasonic cleaning 8 minutes, the carbon fiber after the cleaning is taken out from distilled water, put in the dilute hydrochloric acid solution that concentration is 0.15mol/L, soaked 24 hours.Carbon fiber after immersion finished, extremely neutral with distilled water flushing, then under 100 ℃, to its oven dry, carbon fiber after the oven dry is put into reacting furnace, with 20 ℃/minute heating rates the reacting furnace temperature is increased to 800 ℃, kept 10 minutes down at 800 ℃ then, carbon fiber is carried out pre-activated handle;
Carbon fiber after pre-activated is finished dealing with is sent in the CVD chamber immediately, rise to 500 ℃ of reaction temperatures with 50 ℃/minute heating rates, with nitrogen is carrier gas, tetraisopropoxy titanium is sent in the reative cell, the flow of carrier gas is 1000sccm, 500 ℃ reaction time is 15 minutes, after reaction is finished, naturally cooling is cooled to room temperature, in the hole of surface and centre, grow, can obtain loading on the anatase structured photocatalyst of titanium dioxide material on the polyacrylonitrile-based carbon fibre;
To obtain the photocatalyst of titanium dioxide material again and be woven into the latticed two-dimentional carbon-fiber film 2 that area is 150mm * 300mm according to a conventional method mechanically, the mesh size is 80 orders, with area is 150mm * 300mm two dimension carbon-fiber film doubling, obtain double-deck two-dimentional carbon-fiber film, its area is 150mm * 150mm, be the 30mm hole with having diameter in the latticed two-dimentional carbon-fiber film 2 again, interior coil support 3 is placed in the latticed two-dimentional carbon-fiber film 2 in the circular opening, coat conducting resinl at its outward flange, again outer coil support 1 is placed on the outer edge place of latticed two-dimentional carbon-fiber film 2, with conducting resinl that outer coil support 1 is bonding, the carbon-fiber film of dismissing outer coil support 1 periphery at last can obtain the photocatalyst material diaphragm.
Take by weighing the 50g asphalt base carbon fiber, join in 1 liter of distilled water and evenly stirred 5 minutes, then in ultrasonic cleaner to its ultrasonic cleaning 10 minutes, carbon fiber after cleaning is taken out from distilled water, put in the dilute hydrochloric acid solution that concentration is 0.2mol/L, soaked 24 hours, carbon fiber after immersion finished, extremely neutral with distilled water flushing, then under 80 ℃, to its oven dry, carbon fiber after the oven dry is put into reacting furnace, with 20 ℃/minute heating rates the reacting furnace temperature is increased to 950 ℃, kept 15 minutes down at 950 ℃ then, carbon fiber is carried out pre-activated handle;
Carbon fiber after pre-activated is finished dealing with is sent in the CVD chamber immediately, rise to 750 ℃ of reaction temperatures with 50 ℃/minute heating rates, with the argon gas is carrier gas, tetraisopropoxy titanium is sent in the reative cell, the flow of carrier gas is 2000sccm, 750 ℃ reaction time is 20 minutes, after reaction is finished, naturally cooling is cooled to room temperature, in the hole of surface and centre, grow, can obtain loading on the anatase structured photocatalyst of titanium dioxide material on the polyacrylonitrile-based carbon fibre;
To obtain the photocatalyst of titanium dioxide material again, to be woven into area according to a conventional method mechanically be the latticed two-dimentional carbon-fiber film 2 of 150mm * 150mm, be the 30mm hole with having diameter in the latticed two-dimentional carbon-fiber film 2 again, interior coil support 3 is placed in the latticed two-dimentional carbon-fiber film 2 in the circular opening, coat conducting resinl at its outward flange, again outer coil support 1 is placed on the outer edge place of latticed two-dimentional carbon-fiber film 2, with conducting resinl that outer coil support 1 is bonding, the carbon-fiber film of dismissing outer coil support 1 periphery at last can obtain the photocatalyst material diaphragm.
Claims (8)
1. photocatalyst material diaphragm, it is characterized in that adopting chemical vapour deposition technique carried titanium dioxide photocatalyst on carbon fiber, can obtain the material of photocatalyst of titanium dioxide, again the photocatalyst of titanium dioxide material is woven according to a conventional method, get final product by interior support arm is fixing, concrete operations follow these steps to carry out:
A, carbon fiber is carried out pre-activated according to a conventional method handle, activation temperature is 600 ℃-950 ℃, and soak time is 5 minutes-15 minutes;
B, will activate pretreated carbon fiber and be sent in the chemical vapor deposition reaction chamber, rise to 250-750 ℃ with 50 ℃/minute heating rates, with argon gas or nitrogen is carrier gas, tetraisopropoxy titanium is fed in the reative cell, and gas flow is 400-2000sccm, and the reaction time is 5-20 minute, after reaction is finished, naturally cooling is cooled to room temperature, and through chemical vapour deposition technique, growth obtains the photocatalyst of titanium dioxide material in the hole of surface and centre;
C, step b is obtained the photocatalyst of titanium dioxide material again and be woven into latticed two-dimentional carbon-fiber film (2) by craft or mechanical system according to a conventional method, the outer edge of latticed two-dimentional carbon-fiber film (2) is fixing with outer coil support (1), and the inside edge of latticed two-dimentional carbon-fiber film (2) can obtain the photocatalyst material diaphragm with interior coil support (3) is fixing.
2. the preparation method of a kind of photocatalyst material diaphragm according to claim 1 is characterized in that following these steps to carrying out:
A, carbon fiber is carried out pre-activated according to a conventional method handle, activation temperature is 600-950 ℃, and soak time is 5-15 minute;
B, will activate pretreated carbon fiber and be sent in the chemical vapor deposition reaction chamber, rise to 250-750 ℃ with 50 ℃/minute heating rates, with argon gas or nitrogen is carrier gas, tetraisopropoxy titanium is fed in the reative cell, and gas flow is 400-2000sccm, and the reaction time is 5-20 minute, after reaction is finished, naturally cooling is cooled to room temperature, and through chemical vapour deposition technique, growth obtains the photocatalyst of titanium dioxide material in the hole of surface and centre;
C, step b is obtained the photocatalyst of titanium dioxide material again and be woven into latticed two-dimentional carbon-fiber film (2) by craft or mechanical system according to a conventional method, to have the hole in the latticed two-dimentional carbon-fiber film (2) again, the outer edge of latticed two-dimentional carbon-fiber film (2) is fixing with outer coil support (1), and the inside edge, hole in the middle of the latticed two-dimentional carbon-fiber film (2) can obtain the photocatalyst material diaphragm with interior coil support (3) is fixing.
3. method according to claim 2 is characterized in that the carbon fiber after the step b activation is fixing or portable in CVD chamber, i.e. growth on one side is Yi Bian move continuously.
4. method according to claim 2 is characterized in that on the step b carbon fiber that the anatase structured shared ratio of titanium dioxide is 90% in the titanium dioxide that the reaction growth obtains.
5. method according to claim 2 is characterized in that the mesh size of step c mesh grid trellis two dimension carbon-fiber film (2) is the 50-100 order.
6. method according to claim 5 is characterized in that step c mesh grid trellis two dimension carbon-fiber film (2) is the one deck or the multilayer of intersecting.
7. method according to claim 6 is characterized in that scribbling conducting resinl on interior coil support (3) edge of step c fixed network trellis two dimension carbon-fiber film (2).
8. method according to claim 7 is characterized in that the outer coil support (1) of step c is made into random geometry with interior coil support (3).
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| CN104355299A (en) * | 2014-10-21 | 2015-02-18 | 中南大学 | Doped carbon fiber net and preparation method thereof |
| CN104862948A (en) * | 2015-04-28 | 2015-08-26 | 武汉纺织大学 | Production method of color carbon fibers |
| CN108455699A (en) * | 2018-01-31 | 2018-08-28 | 常州澳弘电子有限公司 | A kind of photocatalysis large area sewage rectification processing scheme |
| CN112310377A (en) * | 2020-11-04 | 2021-02-02 | 四川轻化工大学 | Battery negative electrode material and preparation method thereof |
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| CN112310377A (en) * | 2020-11-04 | 2021-02-02 | 四川轻化工大学 | Battery negative electrode material and preparation method thereof |
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