CN104492413A - Quick preparation method of porous carbon/zinc oxide composite material for catalytic degradation in darkroom - Google Patents
Quick preparation method of porous carbon/zinc oxide composite material for catalytic degradation in darkroom Download PDFInfo
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- CN104492413A CN104492413A CN201510021168.5A CN201510021168A CN104492413A CN 104492413 A CN104492413 A CN 104492413A CN 201510021168 A CN201510021168 A CN 201510021168A CN 104492413 A CN104492413 A CN 104492413A
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Abstract
The invention relates to a quick preparation method of a porous carbon/zinc oxide composite material for catalytic degradation in a darkroom. The quick preparation method includes the steps of: mixing carbon nanotube with absolute ethyl alcohol according to a mass-to-volume ratio, putting into an ultrasound and microwave combined reaction system to disperse ultrasonically, and thereby obtaining a first mixture; adding the zinc oxide and the absolute ethyl alcohol into the first mixture according to a mass-to-volume ratio, ultrasonically dispersing for 20min in an ultrasonic cleaner to obtain a second mixture; adding polymethyl methacrylate with particle size of 2-20 microns into the second mixture, continuously dispersing ultrasonically, and thereby obtaining carbon nanotube/zinc oxide/polymethyl methacrylate suspension liquid; obtaining a filter cake by performing suction filtration on the suspension liquid; at last putting the filter cake into a batch-type furnace to heat to the thermal decomposition temperature of the polymethyl methacrylate, keeping the temperature for 102 house, and thereby obtaining the finished product after cooling. The process has the advantages of being simple in preparation technology, short in production time, high in efficiency, low in energy consumption, energy-saving, environment-friendly and free of pollution. The porous carbon/zinc oxide composite material prepared by the process has significant effect on catalytically degrading organic pollutant in the darkroom.
Description
Technical field
The present invention relates to a kind of fast preparation method of the porous carbon/zinc oxide composite for darkroom catalytic degradation, belong to advanced composite material (ACM) preparing technical field, for technical fields such as electrode of super capacitor, water pollution absorption, there is significant effect in particular for darkroom catalyze and degrade organic pollutants.
Background technology
The research that three dimensional pore structures constructed by material based on CNT causes concern in some fields.The three dimensional pore structures constructed by carbon nano-tube material combines the application advantage of micropore, mesopore and macropore---and micropore and mesopore provide the surface area of superelevation, macropore becomes again the passage entering micropore simultaneously, therefore the hierarchy of the three-dimensional network formation of this micropore, mesopore and macropore, can in some chemical reactions, ensure by molecular transport to the internal-response region in whole three-dimensional structure, for new material provides more reaction cavity and active surface.ZnO is because it is cheap, preparation method is various, technique is relatively simple and become widely used semi-conducting material.ZnO is a kind of electronic structure of semiconductor catalyst, can be used as strong oxidizer and complete the degraded to organic matter (or chloride), add the composite porous three dimensional pore structures that zinc oxide obtains, there is new application prospect, can be used for the technical fields such as catalyst carrier, water treatment, electrode material, the research of its synthetic method and the research of material property are hot research problems always.
At present, prepare porous carbon/zinc oxide composite, be mostly to adopt chemical vapour deposition technique or sol-gel process.These preparation method's complicated process of preparation on the one hand, the defects such as it is low that preparation process exists efficiency, and cost is high, and the production cycle is long, as longer in sol-gel process required time, several days or a few weeks of normal needs, and preparation method of the present invention at most only needs one day.On the other hand these preparation method's energy consumptions are high and have pollution to environment.Up to the present also do not have a kind of preparation technology simple, the production time is short, and efficiency is high, and energy consumption is low, and the fast preparation method of the free of contamination porous carbon/zinc oxide composite for darkroom catalytic degradation of energy-saving and environmental protection is come out.
Summary of the invention
The invention discloses a kind of fast preparation method of the porous carbon/zinc oxide composite for darkroom catalytic degradation, effectively can overcome the complicated process of preparation of prior art chemical vapour deposition technique or sol-gel process existence, efficiency is low, cost is high, have the defects such as pollution to environment.The whole technique of the present invention uses ultrasonic-microwave composite reaction system, ultrasonic cleaner, core Suction filtration device, batch-type furnace, and not only preparation technology is simple, and speed is fast, and efficiency is high, low energy consumption, and energy-saving and environmental protection are pollution-free.Be applicable to the technical field such as electrode of super capacitor, water pollution absorption, have significant effect in particular for darkroom catalyze and degrade organic pollutants.
Technical solution of the present invention is as follows:
A kind of fast preparation method of the porous carbon/zinc oxide composite for darkroom catalytic degradation, take absolute ethyl alcohol as dispersant, polymethyl methacrylate is pore creating material, mix ultrasonic by absolute ethyl alcohol with CNT, zinc oxide, polymethyl methacrylate, after suction filtration, heating and thermal insulation obtains porous carbon/zinc oxide composite again; Concrete preparation process is as follows:
A) with the ratio of mass volume ratio 30mg:50ml, CNT is joined in absolute ethyl alcohol, then in the ultrasonic-microwave composite reaction system be placed on, ultrasonic disperse obtains the first mixture;
B) with the ratio of mass volume ratio 80mg:100ml, zinc oxide and absolute ethyl alcohol are joined steps A) in the first mixture of obtaining, be placed in ultrasonic cleaner ultrasonic disperse, obtain the second mixture;
C) be that 6-24 μm of polymethyl methacrylate joins step B by 300mg average grain diameter) in the second mixture of obtaining, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension;
D) by step C) suspension prepared through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake;
E) described filter cake is placed in crucible, in batch-type furnace, is heated to polymethyl methacrylate heat decomposition temperature, then is incubated 1-2 hour, take out after cooling, obtain porous carbon/zinc oxide composite.
Steps A) described in ultrasonic-microwave composite reaction system power be 400W, ultrasonic disperse 20 minutes at normal temperatures.
Step B) described in ultrasonic cleaner frequency be 60kHz, power is 480W, at normal temperatures and pressures ultrasonic disperse 20 minutes.
Step e) described in polymethyl methacrylate burn to complete thermal decomposition.
The present invention provides a kind of new method for the quick preparation of the porous carbon/zinc oxide composite of darkroom catalytic degradation, there is preparation technology simple, production time is short, the advantages such as efficiency is high, and energy consumption is low, and energy-saving and environmental protection are pollution-free, obtained three-dimensional pore space material is used for the technical field such as electrode of super capacitor, water pollution absorption, and there is good darkroom catalytic degradation effect, especially darkroom catalyze and degrade organic pollutants, effect is more remarkable.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the porous carbon/zinc oxide composite for darkroom catalytic degradation prepared by embodiment 1;
Fig. 2 is the SEM figure of the porous carbon/zinc oxide composite for darkroom catalytic degradation prepared by embodiment 1;
Fig. 3 is that the porous carbon/zinc oxide composite for darkroom catalytic degradation prepared of embodiment 1 is for the design sketch of darkroom catalytic degradation methylene blue.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail, but embodiment is not limited to the present invention, and all employings similarity method of the present invention and similar change thereof, all should be classified as protection scope of the present invention.
CNT mixes with the ratio of mass volume ratio 30mg:50ml with absolute ethyl alcohol by [embodiment 1], and being placed on power is in the ultrasonic-microwave composite reaction system of 400W, ultrasonic disperse 20 minutes at normal temperatures, obtained first mixture; Bar-shaped zinc oxide grinding water solution obtained mixes with the ratio of mass volume ratio 80mg:100ml with absolute ethyl alcohol, be added to after in above-mentioned first mixture, being placed on frequency is 60kHz, power is in the ultrasonic cleaner of 480W, ultrasonic disperse 20 minutes, obtains the second mixture at normal temperatures and pressures; Be that 6 μm of polymethyl methacrylates (PMMA) join in above-mentioned second mixture by 300mg average grain diameter, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension; By described suspension through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake; Described filter cake is placed in crucible, heats at batch-type furnace 2 little of polymethyl methacrylate heat decomposition temperature 380 DEG C, then be incubated 2 hours, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
The XRD diffraction pattern of the porous carbon/zinc oxide composite for darkroom catalytic degradation of Fig. 1 prepared by this [embodiment 1], as shown in Figure 1, this collection of illustrative plates diffraction peak shape is sharp-pointed, and 26 ° and 44 ° of diffraction maximums located as C, all the other diffraction maximums are all mated with ZnO standard diffraction peak position.Illustrate that the porous carbon for darkroom catalytic degradation/zinc oxide composite composition prepared by the present invention meets.
The SEM figure of the porous carbon/zinc oxide composite for darkroom catalytic degradation of Fig. 2 prepared by this [embodiment 1], as can be seen from the figure, pore structure is obvious, and ZnO is evenly distributed, about 6 μm, aperture, suitable with PMMA average grain diameter.
Porous carbon/the zinc oxide composite for darkroom catalytic degradation of Fig. 3 prepared by this [embodiment 1] and pure nano-carbon tube film carry out the effect contrast figure of darkroom catalytic degradation methylene blue, as can be seen from the figure, porous carbon/zinc oxide composite construction was when darkroom catalytic degradation methylene blue 180 minutes, degrade about 97%, be much better than 11% of pure nano-carbon tube film, illustrate that it has extraordinary effect for darkroom catalytic degradation methylene blue.
CNT mixes with the ratio of mass volume ratio 30mg:50ml with absolute ethyl alcohol by [embodiment 2], and being placed on power is in the ultrasonic-microwave composite reaction system of 400W, ultrasonic disperse 20 minutes at normal temperatures, obtained first mixture; Bar-shaped zinc oxide grinding water solution obtained mixes with the ratio of mass volume ratio 80mg:100ml with absolute ethyl alcohol, be added to after in above-mentioned first mixture, being placed on frequency is 60kHz, power is in the ultrasonic cleaner of 480W, ultrasonic disperse 20 minutes, obtains the second mixture at normal temperatures and pressures; Be that 2 μm of polymethyl methacrylates (PMMA) join in above-mentioned second mixture by 300mg average grain diameter, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension; By described suspension through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake; Described filter cake is placed in crucible, heats at batch-type furnace 2 little of polymethyl methacrylate heat decomposition temperature 395 DEG C, then be incubated 2 hours, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
CNT mixes with the ratio of mass volume ratio 30mg:50ml with absolute ethyl alcohol by [embodiment 3], and being placed on power is in the ultrasonic-microwave composite reaction system of 400W, ultrasonic disperse 20 minutes at normal temperatures, obtained first mixture; Bar-shaped zinc oxide grinding water solution obtained mixes with the ratio of mass volume ratio 80mg:100ml with absolute ethyl alcohol, be added to after in above-mentioned first mixture, being placed on frequency is 60kHz, power is in the ultrasonic cleaner of 480W, ultrasonic disperse 20 minutes, obtains the second mixture at normal temperatures and pressures; Be that 10 μm of polymethyl methacrylates (PMMA) join in above-mentioned second mixture by 300mg average grain diameter, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension; By described suspension through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake; Described filter cake is placed in crucible, heats at batch-type furnace 2 little of polymethyl methacrylate heat decomposition temperature 345 DEG C, then be incubated 2 hours, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
CNT mixes with the ratio of mass volume ratio 30mg:50ml with absolute ethyl alcohol by [embodiment 4], and being placed on power is in the ultrasonic-microwave composite reaction system of 400W, ultrasonic disperse 20 minutes at normal temperatures, obtained first mixture; Bar-shaped zinc oxide grinding water solution obtained mixes with the ratio of mass volume ratio 80mg:100ml with absolute ethyl alcohol, be added to after in above-mentioned first mixture, being placed on frequency is 60kHz, power is in the ultrasonic cleaner of 480W, ultrasonic disperse 20 minutes, obtains the second mixture at normal temperatures and pressures; Be that 20 μm of polymethyl methacrylates (PMMA) join in above-mentioned second mixture by 300mg average grain diameter, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension; By described suspension through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake; Described filter cake is placed in crucible, heats at batch-type furnace 2 little of polymethyl methacrylate heat decomposition temperature 330 DEG C, then be incubated 2 hours, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
[embodiment 5], by CNT and absolute ethyl alcohol with the scalemic thereof of mass volume ratio 30mg:50ml, being placed on power is in the ultrasonic-microwave composite reaction system of 400W, ultrasonic disperse 20 minutes at normal temperatures, obtained first mixture; The zinc oxide bought is mixed with the ratio of mass volume ratio 80mg:100ml with absolute ethyl alcohol, be added to after in above-mentioned first mixture, being placed on frequency is 60kHz, and power is in the ultrasonic cleaner of 480W, ultrasonic disperse 20 minutes, obtains the second mixture at normal temperatures and pressures; Be that 6 μm of polymethyl methacrylates (PMMA) join in above-mentioned second mixture by 300mg average grain diameter, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension; By described suspension through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake; Described filter cake is placed in crucible, heats at batch-type furnace 2 little of polymethyl methacrylate heat decomposition temperature 380 DEG C, then be incubated 2 hours, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
Porous carbon/zinc oxide composite for darkroom catalytic degradation prepared by the present invention, pore structure is obvious, and aperture is suitable with PMMA average grain diameter, and ZnO is evenly distributed.This composite for darkroom catalytic degradation may be used for darkroom catalyzing and degrading pollutant, and experimental result shows, and this structure has good effect for darkroom catalytic degradation methylene blue.In addition, also can be used for the field such as electrode of super capacitor, water pollution absorption.And its preparation technology is simple, the production time is short, and efficiency is high, and energy consumption is low, and energy-saving and environmental protection are pollution-free.
Claims (4)
1. the fast preparation method for the porous carbon/zinc oxide composite of darkroom catalytic degradation, it is characterized in that: take absolute ethyl alcohol as dispersant, polymethyl methacrylate is pore creating material, mix ultrasonic by absolute ethyl alcohol with CNT, zinc oxide, polymethyl methacrylate, after suction filtration, heating and thermal insulation obtains again; Concrete preparation process is as follows:
A) with the ratio of mass volume ratio 30mg:50ml, CNT is joined in absolute ethyl alcohol, then be placed on ultrasonic disperse in ultrasonic-microwave composite reaction system and obtain the first mixture;
B) with the ratio of mass volume ratio 80mg:100ml, zinc oxide and absolute ethyl alcohol are joined steps A) in the first mixture of obtaining, be placed in ultrasonic cleaner ultrasonic disperse, obtain the second mixture;
C) be that 6-24 μm of polymethyl methacrylate joins step B by 300mg average grain diameter) in the second mixture of obtaining, continue ultrasonic disperse 10 minutes, obtain finely dispersed CNT/zinc oxide/polymethyl methacrylate suspension;
D) by step C) suspension prepared through core Suction filtration device suction filtration, obtain CNT/zinc oxide/polymethyl methacrylate filter cake;
E) described filter cake is placed in crucible, in batch-type furnace, is heated to polymethyl methacrylate heat decomposition temperature, then is incubated 1-2 hour, take out after cooling, obtain the porous carbon/zinc oxide composite for darkroom catalytic degradation.
2. the fast preparation method of a kind of porous carbon/zinc oxide composite for darkroom catalytic degradation according to claim 1, it is characterized in that: steps A) described in ultrasonic-microwave composite reaction system power be 400W, ultrasonic disperse 20 minutes at normal temperatures.
3. the fast preparation method of a kind of porous carbon/zinc oxide composite for darkroom catalytic degradation according to claim 1, it is characterized in that: step B) described in ultrasonic cleaner frequency be 60kHz, power is 480W, at normal temperatures and pressures ultrasonic disperse 20 minutes.
4. the fast preparation method of a kind of porous carbon/zinc oxide composite for darkroom catalytic degradation according to claim 1, is characterized in that: step e) described in polymethyl methacrylate burn to complete thermal decomposition.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
| CN103386303A (en) * | 2013-07-25 | 2013-11-13 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN103386303A (en) * | 2013-07-25 | 2013-11-13 | 中国石油化工股份有限公司 | Hydrogenation catalyst and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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