CN103111277A - Zinc oxide composite flexible membrane with catalytic degradation effect and preparation method and application of membrane - Google Patents
Zinc oxide composite flexible membrane with catalytic degradation effect and preparation method and application of membrane Download PDFInfo
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- CN103111277A CN103111277A CN2013100279570A CN201310027957A CN103111277A CN 103111277 A CN103111277 A CN 103111277A CN 2013100279570 A CN2013100279570 A CN 2013100279570A CN 201310027957 A CN201310027957 A CN 201310027957A CN 103111277 A CN103111277 A CN 103111277A
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Abstract
The invention discloses a zinc oxide composite flexible membrane with a catalytic degradation effect and a preparation method of the membrane, which belong to the field of organic pollutant degradation. The preparation method comprises the following steps of: performing strong ultrasonic dispersion on a multi-wall carbon nanotube, prepared by a chemical vapor deposition process, in an isopropanol solution until the multi-wall carbon nanotube is fully dispersed and suspended in the isopropanol solution, thus obtaining multi-wall carbon nanotube suspending liquid which is uniformly dispersed; and performing hydrolysis reaction on zinc powder nanoparticles prepared by vibration grinding to obtain composite powder containing zinc oxide nanorods, mixing the composite powder with the multi-wall carbon nanotube suspending liquid, carrying out suction filtration, peeling and vacuum drying on the mixture which is uniform after being subjected to ultrasonic dispersion, thus obtaining the zinc oxide composite flexible membrane with the catalytic degradation effect. The zinc oxide composite flexible membrane with the catalytic degradation effect can be folded at will, has the characteristics of organics with good catalytic degradation without a special light source condition, and is easy to recycle and reutilize.
Description
Technical field
The present invention relates to a kind of zinc oxide composite and flexible film with catalytic degradation effect and its preparation method and application, belong to the organic pollutant degradation field.
Background technology
Zinc oxide particularly plumbous zinc ore nano zinc oxide material is a kind of novel wide bandgap semiconductor materials, the wide 3.37eV in forbidden band under room temperature, exciton bind energy 60meV.The nano zine oxide one-dimentional structure has unique characteristic, is being widely used aspect solar cell, ultraviolet laser, light emitting diode and Photocatalytic Degradation of Organic.It is all to utilize it as the function of photochemical catalyst that zinc oxide is used for degradation catalyst, catalytic reaction will be carried out under certain light conditions, and the film forming of zinc oxide mainly contains the methods such as magnetron sputtering method, sol-gel process, laser ablation method, it is film forming on certain substrate, because the existence of substrate can limit its application in catalytic degradation, also be unfavorable for recycling.
Patent Office of the People's Republic of China has announced a kind of film build method (application number: 200610080698.8) of Zinc oxide film, this invention provides uses the CVD method to form the film build method of Zinc oxide film at various substrate surfaces, zinc methide or diethyl zinc are dissolved into other alternate supplies of forming gasifying gas in organic solvent and containing oxidant gas to the CVD device, form Zinc oxide film comprising on silicon substrate, sapphire substrate etc.Be a kind of fixing inflexibility film, equipment is complicated, and operation is loaded down with trivial details, and there is no the organic function of catalytic degradation.
(application number: 03116798.5), the film of this invention is comprised of the nanometer rods of three-dimensional arrangement the preparation method of the 3 D tropism zinc-oxide film that Patent Office of the People's Republic of China announces; Another kind of method (the application number: 03129300.X), be to use magnetically controlled sputter method to generate zinc-oxide film on substrate, but these films are all to grow on substrate, the inflexibility film for preparing the p-type zinc-oxide film.
Summary of the invention
One of purpose of the present invention is for a kind of zinc oxide composite and flexible film that illumination namely can be used for organic pollutant degradation that need not is provided.
Two of purpose of the present invention is to provide above-mentioned a kind of preparation method who can be used for the zinc oxide composite and flexible film of organic pollutant degradation.
Technical scheme of the present invention
A kind of zinc oxide composite and flexible film with catalytic degradation effect, namely utilize the composite powder that contains zinc oxide nano rod of the hydrolytic process preparation of lower powered process of lapping and low temperature, pliability in conjunction with multi-walled carbon nano-tubes has been prepared into certain flexible zinc oxide composite and flexible film, the preparation method is simple, the zinc oxide composite and flexible film of gained need not illumination namely good catalytic degradation effect, and is easy to recycling.
A kind of zinc oxide composite and flexible film with catalytic degradation effect is prepared by a method comprising the following steps:
(1), be at first that the atomized zinc dust of 3-5 μ m is inserted in the mill tube of roll extrusion vibration mill with granularity, with the air in vavuum pump extraction system, then the inert gas injecting argon gas, carry out vibro-grinding 1-15h under the protection of inert gas argon gas, namely gets the zinc powder nano particle that grinds refinement;
(2), zinc powder nano particle that step (1) is ground refinement is placed in container, is preheating to temperature and is that to pass into temperature after 120-300 ℃ be that the water vapour of 100 ℃ fully reacts 30-150min and generates the composite powder that contains zinc oxide nano rod;
The zinc oxide nano rod diameter of gained is about 10-50nm, and length dimension is distributed in 1-5 μ m;
(3), the multi-walled carbon nano-tubes of chemical vapour deposition technique preparation is placed in aqueous isopropanol with powerful ultrasonic dispersion 10～40min, till fully disperseing and be suspended in solution to multi-walled carbon nano-tubes, obtain finely dispersed multi-walled carbon nano-tubes suspension;
Described multi-walled carbon nano-tubes diameter is at 5-15nm, and length is at 100-400 μ m;
(4), calculate in mass ratio, the composite powder that namely contains zinc oxide nano rod: multi-walled carbon nano-tubes is 0.5-10:1, the composite powder that contains zinc oxide nano rod with step (2) gained mixes with the finely dispersed multi-walled carbon nano-tubes suspension of step (3) gained respectively, mix rear ultrasonic dispersion 10-40min, namely obtain the mixed liquor of finely dispersed zinc oxide and multi-walled carbon nano-tubes;
(5), the mixed liquor of the finely dispersed zinc oxide of step (4) gained and multi-walled carbon nano-tubes being carried out suction filtration peels off and is placed in vacuum drying chamber and control vacuum and be-0.1MPa, temperature is 50-100 ℃ and carries out drying, namely gets thickness and be 15-30 μ m, the bent zinc oxide composite and flexible film with catalytic degradation effect.
a kind of zinc oxide composite and flexible film with catalytic degradation effect of above-mentioned gained can be used for organic pollutant degradation, the present invention only gives an example as the simulating pollution thing with aqueous solution of methylene blue, but do not limit a kind of application of zinc oxide composite and flexible film in other organic pollution with catalytic degradation effect of the present invention, the zinc oxide composite and flexible film that its using method is about to have the catalytic degradation effect fixedly is suspended from organic pollution solution with respect to organic contamination solution incoming flow perpendicular direction with thin stainless steel iron wire, need not special light shines, can be with organic pollutant degradation.
Beneficial effect of the present invention
A kind of zinc oxide composite and flexible film with catalytic degradation effect of the present invention, because the method that has adopted physical grinding prepares the zinc powder nano particle, hydrolysis by lower temperature obtains containing and mixes with multi-walled carbon nano-tubes suspension after the composite powder of zinc oxide nano rod and zinc oxide composite and flexible film that the ultrasonic rear suction filtration that is uniformly dispersed, vacuum drying obtain having the catalytic degradation effect again, its preparation process is simple, easy to operate, equipment cost is low, easily realizes industrialization production.
A kind of zinc oxide composite and flexible film with catalytic degradation effect of the present invention, its degraded that is used for organic pollution is that the zinc oxide composite and flexible film that will have the catalytic degradation effect fixedly is suspended from organic pollution solution with respect to organic contamination solution incoming flow perpendicular direction, need not special light shines, namely just can carry out catalyze and degrade organic pollutants unglazed according in situation, therefore a kind of zinc oxide composite and flexible film with catalytic degradation effect of the present invention has easy to use, can be recycling, the convenient characteristics that reclaim have good prospects for commercial application.
Description of drawings
The content of the composite powder that contains zinc oxide nano rod of Fig. 1 a, embodiment 1 gained is the scanning electron microscope (SEM) photograph of 41% the zinc oxide composite and flexible film with catalytic degradation effect;
The content of the composite powder that contains zinc oxide nano rod of Fig. 1 b, embodiment 1 gained is the scanning electron microscope (SEM) photograph of 52% the zinc oxide composite and flexible film with catalytic degradation effect;
The content of the composite powder that contains zinc oxide nano rod of Fig. 2, embodiment 1 gained is respectively the design sketch of 41%, 52% the zinc oxide composite and flexible film catalytic degradation methylene blue with catalytic degradation effect.
The specific embodiment
Also further set forth by reference to the accompanying drawings the present invention below in conjunction with embodiment, but be not limited to the present invention.
The present invention's roll extrusion vibration mill used has obtained national patent, and patent No. ZL 99112092.2, is that the Wang Shulin by one of inventor herein develops voluntarily.
Powerful ultrasonic dispersion equipment used is Sonicator 3000, and U.S. Misonix company produces.
A kind of zinc oxide composite and flexible film with catalytic degradation effect is prepared by a method comprising the following steps:
(1), with granularity be at first 3-5 μ m, the commercial atomized zinc dust that purity is 95%, quality is 150g is inserted in the mill tube of roll extrusion vibration mill, with the air in vavuum pump extraction system, then inert gas injecting argon gas in the system, when pressure returns to normal pressure, close argon gas valve opening motor, carry out vibro-grinding 13h under the protection of inert gas argon gas, namely get the zinc powder nano particle that grinds refinement;
In order to discharge the zinc particle internal stress, during vibromill grinds, grind 1h, 3h, 5h, 7h, respectively shutting down 30min after 9h restarts again, continue to grind, milling time ends and shuts down sampling, and sampling is carried out and deposit in the sample bottle of inert gas argon gas protection isolated air in placing under the protection of inert gas argon gas;
(2), zinc powder nano particle that step (1) is ground refinement is placed in there-necked flask, is preheating to temperature and is that to pass into temperature after 120-300 ℃ be that the water vapour of 100 ℃ fully reacts 30-150min and generates the composite powder that contains zinc oxide nano rod;
(3), the multi-walled carbon nano-tubes of the 3mg of chemical vapour deposition technique preparation is placed in aqueous isopropanol with powerful ultrasonic dispersion 10～40min, till fully disperseing and be suspended in aqueous isopropanol to multi-walled carbon nano-tubes, obtain finely dispersed multi-walled carbon nano-tubes suspension;
The multi-walled carbon nano-tubes of described chemical vapour deposition technique preparation, namely make catalyst with iron, silicon chip is substrate, passing into the acetylene gas of 5mol%, is deposition of carbon nanotubes in the tube furnace of 45mm at diameter, gas flow 580 sccm, 680 ℃ of reaction temperatures, reaction time 10min makes diameter 10nm, the multi-walled carbon nano-tubes of long 300 μ m;
(4), respectively the composite powder that contains zinc oxide nano rod of step (2) gained and the finely dispersed multi-walled carbon nano-tubes suspension of step (3) gained are calculated in mass ratio, the composite powder that namely contains zinc oxide nano rod: multi-walled carbon nano-tubes is that 0.7:1 and 1.1:1 mix, mix rear ultrasonic dispersion 10-40min respectively, namely obtain respectively the mixed solution of finely dispersed zinc oxide and multi-walled carbon nano-tubes;
(5), pour respectively the finely dispersed zinc oxide of step (4) gained and the mixed solution of multi-walled carbon nano-tubes into the suction filtration device, fall on filter paper, peel off from filter paper respectively after bone dry, being placed in vacuum drying chamber control vacuum is-0.1MPa, temperature is 60 ℃ of fully dryings, remove residual solution, namely get thickness and all be respectively 41%, 52% the zinc oxide composite and flexible film with catalytic degradation effect at 15-30 μ m, the content that contains the composite powder of zinc oxide nano rod.
The content of the composite powder that contains zinc oxide nano rod of above-mentioned gained is respectively 41%, 52% the zinc oxide composite and flexible film with catalytic degradation effect, SEM by NSK JEOL JSM-7401F model scans, the scanning electron microscope (SEM) photograph of gained is as shown in Fig. 1 a, Fig. 1 b, can find out that from Fig. 1 a, Fig. 1 b zinc oxide nano rod is dispersed in the three-dimensional net structure of multi-walled carbon nano-tubes, multi-walled carbon nano-tubes has played to zinc oxide nano rod the effect of supporting and fettering.
Application Example
configuration concentration be 16mg/L aqueous solution of methylene blue as the simulation organic pollution, the content of the composite powder that contains zinc oxide nano rod of embodiment 1 preparation is respectively 41%, 52% the zinc oxide composite and flexible film with catalytic degradation effect fixedly is suspended from above-mentioned simulation organic pollution with thin stainless steel iron wire, need not special light shines, the simulation organic pollution is degraded, situation is as shown in Figure 2 over time for the degradation rate of organic pollution methylene blue, the content that in Fig. 2, Film-1 represents to contain the composite powder of zinc oxide nano rod is respectively 41% the zinc oxide composite and flexible film with catalytic degradation effect, the content that Film-2 represents to contain the composite powder of zinc oxide nano rod is respectively 52% the zinc oxide composite and flexible film with catalytic degradation effect, as can be seen from Figure 2 the concentration of methylene blue in time increase and reduce, degradation effect is obvious.
Above said content is the basic explanation under conceiving for the present invention only, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (9)
1. zinc oxide composite and flexible film with catalytic degradation effect is characterized in that being prepared by a method comprising the following steps:
(1), be at first that the atomized zinc dust of 3-5 μ m is inserted in the mill tube of roll extrusion vibration mill with granularity, with the air in vavuum pump extraction system, then the inert gas injecting argon gas, carry out vibro-grinding 1-15h under the protection of inert gas argon gas, namely gets the zinc powder nano particle that grinds refinement;
(2), the zinc powder nano particle of the grinding refinement of step (1) gained is placed in container, be preheating to temperature and be that to pass into temperature after 120-300 ℃ be that the water vapour of 100 ℃ fully reacts 30-150min and generates the composite powder that contains zinc oxide nano rod;
(3), the multi-walled carbon nano-tubes of chemical vapour deposition technique preparation is placed in aqueous isopropanol with powerful ultrasonic dispersion 10～40min, till fully disperseing and be suspended in aqueous isopropanol to multi-walled carbon nano-tubes, obtain finely dispersed multi-walled carbon nano-tubes suspension;
(4), calculate in mass ratio, the composite powder that namely contains zinc oxide nano rod: multi-walled carbon nano-tubes is 0.5-10:1, the composite powder that contains zinc oxide nano rod with step (2) gained mixes with the finely dispersed multi-walled carbon nano-tubes solution of step (3) gained respectively, mix rear ultrasonic dispersion 10-40min, namely obtain the mixed liquor of finely dispersed zinc oxide and multi-walled carbon nano-tubes;
(5), the mixed solution of the finely dispersed zinc oxide of step (4) gained and multi-walled carbon nano-tubes carried out suction filtration peel off, then carry out vacuum drying, namely get the zinc oxide composite and flexible film with catalytic degradation effect.
2. a kind of zinc oxide composite and flexible film with catalytic degradation effect as claimed in claim 1, is characterized in that the zinc oxide nano rod diameter of gained in preparation process (2) is about 10-50nm, and length dimension is distributed in 1-5 μ m.
3. a kind of zinc oxide composite and flexible film with catalytic degradation effect as claimed in claim 2, is characterized in that the multi-walled carbon nano-tubes diameter of the chemical vapour deposition technique preparation described in preparation process (3) at 5-15nm, and length is at 100-400 μ m.
4. a kind of zinc oxide composite and flexible film with catalytic degradation effect as claimed in claim 3, is characterized in that it is-0.1MPa that temperature is 50-100 ℃ and carries out drying that vacuum is namely controlled in the vacuum drying described in preparation process (5).
5. as claim 1,2, the 3 or 4 described a kind of application of zinc oxide composite and flexible film in catalyze and degrade organic pollutants with catalytic degradation effect.
6. as claim 1,2,3 or 4 described a kind of preparation methods with zinc oxide composite and flexible film of catalytic degradation effect, it is characterized in that specifically comprising the steps:
(1), be at first that the atomized zinc dust of 3-5 μ m is inserted in the mill tube of roll extrusion vibration mill with granularity, with the air in vavuum pump extraction system, then the inert gas injecting argon gas, carry out vibro-grinding under the protection of inert gas argon gas, 1-15h namely gets the zinc powder nano particle that grinds refinement;
(2), the zinc powder nano particle of the grinding refinement of step (1) gained is placed in container, be preheating to temperature and be that to pass into temperature after 120-300 ℃ be that the water vapour of 100 ℃ fully reacts 30-150min and generates the composite powder that contains zinc oxide nano rod;
(3), the multi-walled carbon nano-tubes of chemical vapour deposition technique preparation is placed in aqueous isopropanol with powerful ultrasonic dispersion 10～40min, till fully disperseing and be suspended in aqueous isopropanol to multi-walled carbon nano-tubes, obtain finely dispersed multi-walled carbon nano-tubes suspension;
(4), calculate in mass ratio, the composite powder that namely contains zinc oxide nano rod: multi-walled carbon nano-tubes is 0.5-10:1, the composite powder that contains zinc oxide nano rod with step (2) gained mixes with the finely dispersed multi-walled carbon nano-tubes solution of step (3) gained respectively, mix rear ultrasonic dispersion 10-40min, namely obtain the mixed solution of finely dispersed zinc oxide and multi-walled carbon nano-tubes;
(5), the finely dispersed zinc oxide of step (4) gained and the mixed solution of multi-walled carbon nano-tubes are carried out carrying out vacuum drying after suction filtration is peeled off, namely get the zinc oxide composite and flexible film with catalytic degradation effect.
7. a kind of preparation method with zinc oxide composite and flexible film of catalytic degradation effect as claimed in claim 6, is characterized in that the described calculating in mass ratio of step (4), and namely contain the composite powder of zinc oxide nano rod: multi-walled carbon nano-tubes is 0.5-10:1.
8. a kind of preparation method with zinc oxide composite and flexible film of catalytic degradation effect as claimed in claim 6, it is characterized in that the described calculating in mass ratio of step (4), namely contain the composite powder of zinc oxide nano rod: multi-walled carbon nano-tubes is 0.7-1.1:1.
9. a kind of preparation method with zinc oxide composite and flexible film of catalytic degradation effect as claimed in claim 7, is characterized in that the described control vacuum of step (5) is-0.1MPa, and temperature is 50-100 ℃ and carries out drying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103394341A (en) * | 2013-08-19 | 2013-11-20 | 上海理工大学 | Preparation method and applications of zinc and zinc oxide nanorod and carbon nano tube composite flexible membrane |
| CN104492413A (en) * | 2015-01-16 | 2015-04-08 | 上海理工大学 | Quick preparation method of porous carbon/zinc oxide composite material for catalytic degradation in darkroom |
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| US20100330008A1 (en) * | 2008-02-07 | 2010-12-30 | Noriya Izu | Core-Shell Type Zinc Oxide Microparticle or Dispersion Containing the Microparticle, and Production Process and Use of the Microparticle or the Dispersion |
| CN102485330A (en) * | 2010-12-06 | 2012-06-06 | 吉林师范大学 | Zinc oxide nano-wire film photocatalyst and preparation method thereof |
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- 2013-01-25 CN CN2013100279570A patent/CN103111277A/en active Pending
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| US20100330008A1 (en) * | 2008-02-07 | 2010-12-30 | Noriya Izu | Core-Shell Type Zinc Oxide Microparticle or Dispersion Containing the Microparticle, and Production Process and Use of the Microparticle or the Dispersion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103394341A (en) * | 2013-08-19 | 2013-11-20 | 上海理工大学 | Preparation method and applications of zinc and zinc oxide nanorod and carbon nano tube composite flexible membrane |
| CN104492413A (en) * | 2015-01-16 | 2015-04-08 | 上海理工大学 | Quick preparation method of porous carbon/zinc oxide composite material for catalytic degradation in darkroom |
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Application publication date: 20130522 |