CN108467024A - A kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch - Google Patents
A kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch Download PDFInfo
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- CN108467024A CN108467024A CN201810542437.6A CN201810542437A CN108467024A CN 108467024 A CN108467024 A CN 108467024A CN 201810542437 A CN201810542437 A CN 201810542437A CN 108467024 A CN108467024 A CN 108467024A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/164—Preparation involving continuous processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
Abstract
The invention discloses a kind of fluid beds preparing carbon nanotube based on chemical vapour deposition technique batch, include automatic liquid feeder, ultrasonic mist generating device, gas supply device, gas flow control device, three-temperature-zone fluidized-bed reactor and heating device, cyclone separator, solid collection device and purifying processing device;The present invention uniformly puddles gas by flowmeter and static mixing chamber, and by upper ventilation, gas passes through bimetallic tube;Ensure that the gas being passed through enters growth chamber body temperature always, by the structure design of more empty ceramic networks, to solve the problems, such as uniform air inlet, the growth chamber thermal field flow field made is stablized, it is ensured that obtains the reproducible carbon nanotube of high quality;It is exactly that gas field and flow field temperature difference influence each other that carbon nano tube growth is most rambunctious, since variable is too many, the carbon nanotube morphology for being unable to ensure growth is consistent, and to which quality quality is very low, this programme is fully solved influencing each other for gas field and flow field and temperature variable.
Description
Technical field
The invention belongs to fluid bed fields, are related to a kind of chemical vapour deposition technique, specifically a kind of to be based on chemical vapor deposition
Area method batch prepares the fluid bed of carbon nanotube.
Background technology
Carbon nanotube is due to its excellent electricity, mechanics and thermal property, in hydrogen storage, Flied emission, suction wave, electrode material etc.
Field has good application prospect.But at present many methods can only small lot preparation carbon nanotube, it is difficult to reduce cost, sternly
Its industrialized application is constrained again.Thus extensive controllable preparation carbon nanotube is one of current carbon nanotube research field
Hot spot.
Fluid bed-chemical vapour deposition technique yield is larger, and purity is higher, it is possible to realize high-volume continuous production.Due to
The chemical vapor deposition of carbon nanotube, which prepares to belong to, puts by force/absorbs heat gas-solid reaction, and fluid bed is more satisfactory reactor.Fluid bed
Method is that the operation of serialization is realized using air-flow, and common fluid bed cannot be to there is the catalyst uniform flow of certain particle size distribution
Change, be based on such factor, we use three layers of alternating temperature fluid bed, and catalyst is sent into before the fluidising chamber of set temperature first
It is pre-processed by ultrasonic atomizer.The activity of catalyst can not only be improved by being ultrasonically treated by atomizer, and can be repeated back to
It receives and utilizes.Meanwhile three layers of alternating temperature fluid bed can allow the catalyst on not at the same level to be operated using different temperatures, so as to
The high temperature active of regulating catalyst is to improve the yield of carbon nanotube.
And fluidized bed process is the operation that serialization is realized using air-flow, common fluid unit cannot be to there is certain grain
The catalyst for spending distribution is even fluidizing, to influence the activity of catalyst and the yield of carbon nanotube.To solve drawbacks described above,
A solution is now provided.
Invention content
The purpose of the present invention is to provide a kind of fluid beds preparing carbon nanotube based on chemical vapour deposition technique batch.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch, includes automatic liquid feeder, super
Sound wave mist generating device, gas supply device, gas flow control device, three-temperature-zone fluidized-bed reactor and heating device,
Cyclone separator, solid collection device and purifying processing device;
Wherein, the gas outlet of the gas supply device is connect with gas flow control device by tracheae, the gas
The volume control device other end is also connected with each other with the air inlet of ultrasonic mist generating device;The gas flow control device
Upper end is additionally provided with contact action interface, and the contact action interface is used to carry out operation and control to device in the present invention;It is described
The inlet of automatic liquid feeder liquid outlet and ultrasonic mist generating device is connected with each other, and passes through ultrasonic mist generating device
Internal liquid control device controls liquid feeding;
The feed inlet phase of the outlet of the ultrasonic mist generating device and three-temperature-zone fluidized-bed reactor and heating device
It connects, the discharge port of the three-temperature-zone fluidized-bed reactor and heating device is mutually interconnected by transparent pipe with cyclone separator
It connects, the gas vent above the cyclone separator is connected with purifying processing device, the solid of the cyclone separator lower end
Trapping outlet is connected with solid collection device.
Further, it is additionally provided with the first inner tube inside the three-temperature-zone fluidized-bed reactor and heating device, described
One upper end of inner tube is connected with each other with transparent pipe;
First inner tube lower end is also socketed with the second inner tube, the three-temperature-zone fluidized-bed reactor and heating device lower end
It is additionally provided with catalyst inlet, second inner tube is catalyst inlet connecting tube, and second inner tube is injected with catalyst
Mouth is connected with each other;Catalyst inlet upper end is additionally provided with the first metal flange.
Further, first inner tube outer end is additionally provided with casing, and first inner tube is set to inside pipe casing, the set
Pipe upper end is further opened with air inlet, and the air inlet upper end is additionally provided with the second metal flange;
Both sides also offer the first import at the top of second inner tube, and first import is passed through with catalyst inlet
It is logical;First bottom of inner tube both sides also offer the second import, and second import is porous ceramics pore.
Beneficial effects of the present invention:The present invention uniformly puddles gas by flowmeter and static mixing chamber, by upper logical
Gas, gas is by bimetallic tube, and using interlayer pipe preheating gas, inner chamber body grows carbon nanotube;Ensure that the gas being passed through enters life
Long cavity inner temperature always, passes through the structure design of more empty ceramic networks, to solve the problems, such as uniform air inlet, the growth chamber made
Stablize in thermal field flow field, it is ensured that obtain the reproducible carbon nanotube of high quality;It is exactly gas field that carbon nano tube growth is most rambunctious
It influences each other with flow field temperature difference, since variable is too many, the carbon nanotube morphology for being unable to ensure growth is consistent, to quality matter
Measure very low, this programme is fully solved influencing each other for gas field and flow field and temperature variable.
Description of the drawings
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is schematic structural view of the invention;
Fig. 2 is structural schematic diagram at the first inner tube and the second inner tube of the invention;
Each label is schematically as follows in figure:Inner tube -1, the second metal flange -2, air inlet -3, three-temperature-zone fluidized-bed reactor
And heating device -4, the first metal flange -5, catalyst inlet -6, transparent pipe -7, cyclone separator -8, solid collect dress
Set -9, contact action interface -10, gas flow control device -11, ultrasonic mist generating device -14, automatic liquid feeder -
15, purifying processing device -16, gas supply device -17.
Specific implementation mode
As shown in Figs. 1-2, it is a kind of based on chemical vapour deposition technique batch prepare carbon nanotube fluid bed, include:From
Dynamic liquid-adding device 15, ultrasonic mist generating device 14, gas supply device 17, gas flow control device 11, three-temperature-zone stream
Fluidized bed reactor and heating device 4, cyclone separator 8, solid collection device 9, purifying processing device 16.
Wherein, the gas outlet of the gas supply device 17 is connect with gas flow control device 11 by tracheae, described
11 other end of gas flow control device is also connected with each other with the air inlet of ultrasonic mist generating device 14;The gas flow
11 upper end of control device is additionally provided with contact action interface 10, and the contact action interface 10 is for carrying out device in the present invention
Operation and control;15 liquid outlet of the automatic liquid feeder and the inlet of ultrasonic mist generating device 14 are connected with each other, and are passed through
Liquid control device inside ultrasonic mist generating device 14 controls liquid feeding;
The outlet of the ultrasonic mist generating device 14 and three-temperature-zone fluidized-bed reactor and the feed inlet of heating device 4
It is connected with each other, the discharge port of the three-temperature-zone fluidized-bed reactor and heating device 4 passes through transparent pipe 7 and 8 phase of cyclone separator
It connects, the gas vent above the cyclone separator 8 is connected with purifying processing device 16, under the cyclone separator 8
The solid trapping outlet at end is connected with solid collection device 9;
Further, it is additionally provided with the first inner tube 1 inside the three-temperature-zone fluidized-bed reactor and heating device 4, it is described
First inner tube, 1 upper end is connected with each other with transparent pipe 7;
First inner tube, 1 lower end is also socketed with the second inner tube 13, the three-temperature-zone fluidized-bed reactor and heating device 4
Lower end is additionally provided with catalyst inlet 6, and second inner tube 13 is catalyst inlet connecting tube, second inner tube 13 with urge
Agent inlet 6 is connected with each other;6 upper end of catalyst inlet is additionally provided with the first metal flange 5.
Further, 1 outer end of the first inner tube is additionally provided with casing 12, and first inner tube 1 is set to inside casing 12,
12 upper end of described sleeve pipe is further opened with air inlet 3, and 3 upper end of the air inlet is additionally provided with the second metal flange 2;
Second inner tube, 13 top both sides also offer the first import 1301, first import 1301 and catalyst
Inlet 6 penetrates through;First inner tube, 1 two bottom sides also offer the second import 101, and second import 101 is porous
Ceramic pore.
After cyclone separator 8, a large amount of gas is upwardly through 16 heel row of purifying processing device to air, and solid is then
It traps in solid collection device 9.It is exactly that gas field and flow field temperature difference influence each other that carbon nano tube growth is most rambunctious, by
Too many in variable, the carbon nanotube morphology for being unable to ensure growth is consistent, and to which quality quality is very low, the present invention is fully solved gas
And flow field and temperature variable influence each other.
The present invention uniformly puddles gas by flowmeter and static mixing chamber, by upper ventilation, gas by bimetallic tube,
Using interlayer pipe preheating gas, inner chamber body grows carbon nanotube;Ensure that the gas being passed through enters growth chamber body temperature always, leads to
The structure design of excessive sky ceramic network, to solve the problems, such as uniform air inlet.Stablize in the growth chamber thermal field flow field made, it is ensured that
The carbon nanotube reproducible to high quality.It is exactly gas field and the mutual shadow of flow field temperature difference that carbon nano tube growth is most rambunctious
It rings, since variable is too many, the carbon nanotube morphology for being unable to ensure growth is consistent, and to which quality quality is very low, this programme is complete
Solve influencing each other for gas field and flow field and temperature variable.
Above content is only to structure of the invention example and explanation, affiliated those skilled in the art couple
Described specific embodiment does various modifications or additions or substitutes by a similar method, without departing from invention
Structure or beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (3)
1. a kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch, which is characterized in that include automatic add
Liquid device (15), ultrasonic mist generating device (14), gas supply device (17), gas flow control device (11), three temperature
Area's fluidized-bed reactor and heating device (4), cyclone separator (8), solid collection device (9) and purifying processing device (16);
Wherein, the gas outlet of the gas supply device (17) is connect with gas flow control device (11) by tracheae, described
Gas flow control device (11) other end is also connected with each other with the air inlet of ultrasonic mist generating device (14);The gas
Volume control device (11) upper end is additionally provided with contact action interface (10), and the contact action interface (10) is used for the present invention
Middle device carries out operation and control;The inlet of automatic liquid feeder (15) liquid outlet and ultrasonic mist generating device (14)
It is connected with each other, liquid feeding is controlled by the internal liquid control device of ultrasonic mist generating device (14);
The outlet of the ultrasonic mist generating device (14) and three-temperature-zone fluidized-bed reactor and the feed inlet of heating device (4)
It is connected with each other, the discharge port of the three-temperature-zone fluidized-bed reactor and heating device (4) passes through transparent pipe (7) and cyclone separator
(8) it is connected with each other, the gas vent of the cyclone separator (8) above is connected with purifying processing device (16), the whirlwind
The solid trapping outlet of separator (8) lower end is connected with solid collection device (9).
2. a kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch according to claim 1, special
Sign is, is additionally provided with the first inner tube (1) inside the three-temperature-zone fluidized-bed reactor and heating device (4), in described first
(1) upper end is managed to be connected with each other with transparent pipe (7);
First inner tube (1) lower end is also socketed with the second inner tube (13), the three-temperature-zone fluidized-bed reactor and heating device
(4) lower end is additionally provided with catalyst inlet (6), and second inner tube (13) is catalyst inlet connecting tube, in described second
(13) are managed to be connected with each other with catalyst inlet (6);Catalyst inlet (6) upper end is additionally provided with the first metal flange
(5)。
3. a kind of fluid bed preparing carbon nanotube based on chemical vapour deposition technique batch according to claim 2, special
Sign is that the first inner tube (1) outer end is additionally provided with casing (12), and first inner tube (1) is set to casing (12) inside, institute
It states casing (12) upper end and is further opened with air inlet (3), air inlet (3) upper end is additionally provided with the second metal flange (2);
Both sides also offer the first import (1301), first import (1301) and catalysis at the top of second inner tube (13)
Agent inlet (6) penetrates through;First inner tube (1) two bottom sides also offer the second import (101), second import
(101) it is porous ceramics pore.
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CN114181815A (en) * | 2021-12-06 | 2022-03-15 | 清华大学 | Large-flow ambient air bioaerosol sampling device and method |
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Effective date of registration: 20230109 Address after: 238000 101, Baisi Group office building, northwest corner of the intersection of Heping Avenue and Xiuhu Road, Chaohu Economic Development Zone, Hefei, Anhui Province Patentee after: Hefei Baisi Intelligent Equipment Co.,Ltd. Address before: 230000 Northwest corner of the intersection of Heping Avenue and Xiuhu Road, Chaohu Economic Development Zone, Hefei, Anhui Province Patentee before: HEFEI BAISI NEW MATERIALS RESEARCH INSTITUTE Co.,Ltd. |
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