CN103394341A - Preparation method and applications of zinc and zinc oxide nanorod and carbon nano tube composite flexible membrane - Google Patents
Preparation method and applications of zinc and zinc oxide nanorod and carbon nano tube composite flexible membrane Download PDFInfo
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- CN103394341A CN103394341A CN2013103630361A CN201310363036A CN103394341A CN 103394341 A CN103394341 A CN 103394341A CN 2013103630361 A CN2013103630361 A CN 2013103630361A CN 201310363036 A CN201310363036 A CN 201310363036A CN 103394341 A CN103394341 A CN 103394341A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 63
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002073 nanorod Substances 0.000 title claims abstract description 52
- 239000011701 zinc Substances 0.000 title claims abstract description 51
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 51
- 239000012528 membrane Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 7
- 230000015556 catabolic process Effects 0.000 claims abstract description 20
- 238000006731 degradation reaction Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 19
- 239000002048 multi walled nanotube Substances 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 210000000988 bone and bone Anatomy 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 3
- 238000001914 filtration Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 41
- 239000000758 substrate Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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Abstract
The invention discloses a preparation method and applications of a zinc and zinc oxide nanorod and a carbon nano tube composite flexible membrane. The preparation method comprises following steps: putting a raw material of zinc powder in a vibration mill to prepare zinc nano particles, subjecting the prepared zinc nano particles to carry out reactions with water steam to generate a zinc and zinc oxide nanorod complex, which has a diameter of 10 to 50 nm and a length of 1 to 5 [mu]m, putting the zinc and zinc oxide nanorod complex in the prepared carbon nano tube mixed liquid, evenly mixing, then subjecting the liquid to an ultrasonic dispersion treatment, wherein the mass ratio of the zinc and zinc oxide nanorod complex to the carbon nano tube being 7 to 87:10, pouring the prepared mixed liquid into a filtration device, making the solid to participate on the filter paper, drying and then separating out the flexible membrane, drying the flexible membrane in vacuum to remove residual solution to obtain the zinc oxide nanorod and carbon nano tube composite flexible membrane. The preparation method has the advantages of simple preparation process, low equipment cost, and easy industrialization. The prepared flexible membrane has a very good catalytic degradation effect on organic pollutants in the absence of light.
Description
Technical field
The present invention relates to the Preparation method and use of a kind of zinc, zinc oxide nano rod and CNT composite and flexible film, for the organic pollutant degradation technical 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, aspect solar cell, ultraviolet laser, light emitting diode and Photocatalytic Degradation of Organic, is being widely used.Zinc oxide is all to utilize its function as photochemical catalyst 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, the invention provides and use the CVD method at various substrate surfaces, to form the film build method of Zinc oxide film, zinc methide or diethyl zinc are dissolved in organic solvent to other alternate supplies of forming gasifying gas and containing oxidant gas to the CVD device, form Zinc oxide film comprising on silicon substrate, sapphire substrate etc.A kind of fixing inflexibility film, the equipment complexity, operation is loaded down with trivial details, and does not have the organic function of catalytic degradation.
Patent Office of the People's Republic of China has announced a kind of method (application number: 03129300.X), be that the use magnetically controlled sputter method generates zinc-oxide film on substrate, but these films are all to grow on substrate, are not flexible membrane for preparing the p-type zinc-oxide film.
Summary of the invention
The invention provides a kind of Preparation method and use with zinc, zinc oxide nano rod and CNT composite and flexible film of catalytic degradation effect, the zinc oxide nano rod and the compound flexible membrane that is prepared into of CNT that utilize the hydrolytic process of lower powered process of lapping and low temperature to prepare, what overcome the prior art existence only can prepare the inflexibility film, and equipment complexity, operation is loaded down with trivial details, the inflexibility film that makes can not catalyze and degrade organic pollutants etc. drawback.This method not only preparation technology is simple, is easy to recycling, and the flexible membrane that makes has the advantages such as catalyze and degrade organic pollutants in the situation that there is no illumination.
Technical solution of the present invention is achieved in that
The milling apparatus that the present invention adopts is roll extrusion vibration mill, has obtained national patent, and patent No. ZL 99112092.2, the pollution that equipment energy consumption is low, do not bring other impurity.
The preparation method of a kind of zinc, zinc oxide nano rod and CNT composite and flexible film, at first zinc particle is prepared to zinc, zinc oxide nano rod complex through the hydrolytic process of lower powered process of lapping and low temperature, then zinc, zinc oxide nano rod complex are compound in carbon nanotube network by ultrasonic dispersion, through precipitating, peel off, drying makes flexible membrane, it is characterized in that: concrete steps are as follows:
A) multi-walled carbon nano-tubes that prepared by chemical vapour deposition technique is placed in absolute ethyl alcohol or aqueous isopropanol, powerful ultrasonic be dispersed to CNT and fully disperse and be suspended in solution till;
B) the raw material zinc powder of 3～5 μ m is placed in to vibromill, under the effect of vibration external force, grain refine becomes faller gill shape 10-20nm wide, the nano particle that 70-80nm is long; The nano particle and the steam reaction that make are generated to zinc nanoparticles and diameter 10～50nm, the zinc oxide nano rod complex of length 1～5 μ m, zinc, zinc oxide nano rod complex are placed in to steps A) the CNT mixed liquor that makes mixes, ultrasonic dispersion, wherein: the mass ratio of zinc, zinc oxide nano rod complex and CNT is: 7-87:10;
C) by step B) mixed liquor for preparing pours the suction filtration device into, falls on filter paper, after bone dry, from filter paper, separates flexible membrane;
D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc, zinc oxide nano rod and CNT composite and flexible film.
A) diameter of multi-walled carbon nano-tubes described in is at 5-15nm, and length is in 100-400 μ m left and right.
The ultrasonic jitter time of the brute force of the CNT A) is 20min, and CNT such as flocculence after dispersion are suspended in solution.
B) zinc described in, zinc oxide nano rod complex and the ultrasonic jitter time of CNT mixed liquor are 15min.
Described D) zinc that makes in, zinc oxide and its thickness of CNT composite and flexible film are 5-40 μ m.
The purposes of a kind of zinc, zinc oxide nano rod and CNT composite and flexible film: the zinc that will make, zinc oxide nano rod and CNT composite and flexible film fixedly are suspended from organic pollution with thin stainless steel iron wire, in the situation that without the special light photograph by contaminant degradation.
The present invention compares with other film build method, has preparation process simple, equipment cost is low, easily realize the advantages such as industrialization production, especially the flexible membrane for preparing of this method has good catalytic degradation effect to organic pollution, especially unglazed, according in situation, just can carry out catalytic degradation, and flexible membrane can also recycle, the convenient recovery, have good prospects for commercial application.
The accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the present invention zinc, zinc oxide nano rod and the CNT composite and flexible film that prepare;
Fig. 2 is the degradation effect figure of the flexible membrane for preparing of zinc, zinc oxide nano rod and CNT different proportion.
The specific embodiment
Below in conjunction with embodiment, further set forth the present invention, but the present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof, all should list protection scope of the present invention in.
The preparation method of a kind of zinc, zinc oxide nano rod and CNT composite and flexible film, at first by granularity, be 3～5 μ m, the commercial atomized zinc dust that purity is 95%, quality is 150g is inserted in the mill tube of vibromill, and the air with in vavuum pump extraction system, then inject argon gas in system.When pressure returns to normal pressure, close argon gas valve opening motor, under inert gas shielding, carry out vibro-grinding.In order to discharge the zinc particle internal stress, vibromill is shut down according to plan 30min during grinding and is restarted, according to the milling time of setting, ends and shuts down sampling, generates the nano zinc powder particle; Sampling is carried out and deposits isolated air in the sample bottle of inert gas shielding in placing under inert gas shielding.
[embodiment 1]
A) multi-walled carbon nano-tubes that prepared by chemical vapour deposition technique is placed in absolute ethyl alcohol, powerful ultrasonic dispersion 20min, and multi-walled carbon nano-tubes fully disperses and is suspended in solution.Selected multi-walled carbon nano-tubes diameter is at 5-15nm, and length is in 100-400 μ m left and right.
B) the nano zinc powder particle and the zinc oxide nano rod complex that prepared by vibro-grinding are placed in there-necked flask, after being preheating to reaction temperature, pass into the water vapour hydrolysis, fully reaction obtains zinc nanoparticles and diameter 10～50nm, the zinc oxide nano rod complex of length 1～5 μ m, then zinc, zinc oxide nano rod complex being placed in to steps A) the CNT mixed liquor that makes mixes, ultrasonic dispersion 15min, wherein: the mass ratio of zinc oxide nano rod powder and CNT is 7:10.
C) by step B) mixed liquor for preparing pours the suction filtration device into, falls on filter paper, after bone dry, from filter paper, separates flexible membrane;
D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc oxide nano rod and CNT composite and flexible film, thickness is in 12-15 μ m left and right.
zinc, the purposes of zinc oxide nano rod and CNT composite and flexible film: configuration concentration is that the methylene blue solution of 16mg/L is as the simulating pollution thing, prepare zinc, zinc oxide nano rod is the flexible membrane of the different proportionings of 7-87:10 from the CNT mass ratio, with thin stainless steel iron wire, fixedly be suspended from organic pollution flexible membrane, without special light, shine, the simulating pollution thing is degraded, degradation effect is shown in shown in Fig. 2 film-1 curve, in 50ml simulation organic pollution, put into the flexible membrane that area is 2cm * 2.5cm, contained zinc, the mass ratio of zinc oxide nano rod complex and CNT is 7:10, the 140min degradation rate is 24.07%.
[embodiment 2]
With [embodiment 1], step B just) mass ratio of zinc, zinc oxide nano rod powder and CNT is 11:10; Step D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc oxide nano rod and CNT composite and flexible film, thickness is in 15-20 μ m left and right.Degradation effect is shown in that shown in Fig. 2 film-2 curve, the 140min degradation rate is 56.73%.
[embodiment 3]
With [embodiment 1], step B just) mass ratio of zinc, zinc oxide nano rod and CNT is 16:10, prepares flexible membrane; Step D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc oxide nano rod and CNT composite and flexible film, thickness is in 20-22 μ m left and right.Degradation effect is shown in that shown in Fig. 2 film-3 curve, the 140min degradation rate is 74.73%.
[embodiment 4]
With [embodiment 1], step B just) mass ratio of zinc, zinc oxide nano rod powder and CNT is 87:10; Step D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc oxide nano rod and CNT composite and flexible film, thickness is in 80-90 μ m left and right.Degradation effect is shown in that shown in Fig. 2 film-4 curve, the 140min degradation rate is 78.64%.
Claims (6)
1. the preparation method of a zinc, zinc oxide nano rod and CNT composite and flexible film, at first zinc particle is prepared to zinc, zinc oxide nano rod complex through the hydrolytic process of lower powered process of lapping and low temperature, then zinc, zinc oxide nano rod complex are compound in carbon nanotube network by ultrasonic dispersion, through precipitating, peel off, drying makes flexible membrane, it is characterized in that: concrete steps are as follows:
A) multi-walled carbon nano-tubes that prepared by chemical vapour deposition technique is placed in absolute ethyl alcohol or aqueous isopropanol, powerful ultrasonic be dispersed to CNT and fully disperse and be suspended in solution till;
B) the raw material zinc powder of 3～5 μ m is placed in to vibromill, under the effect of vibration external force, grain refine becomes faller gill shape 10-20nm wide, the nano particle that 70-80nm is long; The nano particle and the steam reaction that make are generated to zinc nanoparticles and diameter 10～50nm, the zinc oxide nano rod complex of length 1～5 μ m, zinc, zinc oxide nano rod complex are placed in to steps A) the CNT mixed liquor that makes mixes, ultrasonic dispersion, wherein: the mass ratio of zinc, zinc oxide nano rod complex and CNT is: 7-87:10;
C) by step B) mixed liquor for preparing pours the suction filtration device into, falls on filter paper, after bone dry, from filter paper, separates flexible membrane;
D) flexible membrane is placed in to fully drying of vacuum drying chamber, removes residual solution, obtain zinc, zinc oxide nano rod and CNT composite and flexible film.
2. the preparation method of zinc according to claim 1, zinc oxide nano rod and CNT composite and flexible film, it is characterized in that: the diameter of multi-walled carbon nano-tubes A) is 5-15nm, length is between 100-400 μ m.
3. the preparation method of zinc according to claim 1, zinc oxide nano rod and CNT composite and flexible film, it is characterized in that: the ultrasonic jitter time of the brute force of the CNT A) is 20min, and CNT such as flocculence after dispersion are suspended in solution.
4. the preparation method of zinc according to claim 1, zinc oxide nano rod and CNT composite and flexible film, it is characterized in that: the zinc oxide nano rod B) and the ultrasonic jitter time of CNT mixed liquor are 15min.
5. the preparation method of zinc according to claim 1, zinc oxide nano rod and CNT composite and flexible film, it is characterized in that: its thickness of zinc oxide composite and flexible film that makes described D) is 5-40 μ m.
6. the purposes of zinc, zinc oxide nano rod and CNT composite and flexible film, it is characterized in that: the zinc that will make, zinc oxide nano rod and CNT composite and flexible film fixedly are suspended from organic pollution with thin stainless steel iron wire, in the situation that without the special light photograph by organic pollutant degradation; (50ml concentration is to put into the flexible membrane that area is 2cm * 2.5cm in the organic pollution of 16g/ml, and the mass ratio of contained zinc, zinc oxide nano rod complex and CNT is 7-87:10, and the 140min degradation rate reaches 75%).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434360A (en) * | 2017-08-25 | 2017-12-05 | 福耀玻璃工业集团股份有限公司 | A kind of super hydrophilic dose, preparation method and super hydrophilic glass for vehicle window |
| CN107445487A (en) * | 2017-08-25 | 2017-12-08 | 福耀玻璃工业集团股份有限公司 | A kind of super hydrophilic dose, preparation method and super hydrophilic glass for vehicle window |
| CN108335916A (en) * | 2017-12-20 | 2018-07-27 | 肇庆市华师大光电产业研究院 | A kind of multi-walled carbon nanotube@X combination electrodes and its preparation method and application |
| CN109046310A (en) * | 2018-08-22 | 2018-12-21 | 东莞理工学院 | A kind of zinc oxide photocatalysis film of two-layer composite and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111277A (en) * | 2013-01-25 | 2013-05-22 | 上海理工大学 | Zinc oxide composite flexible membrane with catalytic degradation effect and preparation method and application of membrane |
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- 2013-08-19 CN CN2013103630361A patent/CN103394341A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111277A (en) * | 2013-01-25 | 2013-05-22 | 上海理工大学 | Zinc oxide composite flexible membrane with catalytic degradation effect and preparation method and application of membrane |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434360A (en) * | 2017-08-25 | 2017-12-05 | 福耀玻璃工业集团股份有限公司 | A kind of super hydrophilic dose, preparation method and super hydrophilic glass for vehicle window |
| CN107445487A (en) * | 2017-08-25 | 2017-12-08 | 福耀玻璃工业集团股份有限公司 | A kind of super hydrophilic dose, preparation method and super hydrophilic glass for vehicle window |
| CN108335916A (en) * | 2017-12-20 | 2018-07-27 | 肇庆市华师大光电产业研究院 | A kind of multi-walled carbon nanotube@X combination electrodes and its preparation method and application |
| CN109046310A (en) * | 2018-08-22 | 2018-12-21 | 东莞理工学院 | A kind of zinc oxide photocatalysis film of two-layer composite and its preparation method and application |
| CN109046310B (en) * | 2018-08-22 | 2023-04-28 | 东莞理工学院 | Zinc oxide photocatalytic film with double-layer composite structure and preparation method and application thereof |
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Application publication date: 20131120 |