CN110451486A - A kind of device and method of batch preparation carbon nanotube - Google Patents
A kind of device and method of batch preparation carbon nanotube Download PDFInfo
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- CN110451486A CN110451486A CN201910730497.5A CN201910730497A CN110451486A CN 110451486 A CN110451486 A CN 110451486A CN 201910730497 A CN201910730497 A CN 201910730497A CN 110451486 A CN110451486 A CN 110451486A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/164—Preparation involving continuous processes
Abstract
The present invention discloses a kind of device and method of batch preparation carbon nanotube, which is made of tiltable tubular type rotary furnace, solids feeder, solid powder separator, powder catcher and auxiliary system etc..Based on floating catalytic chemical vapor deposition preparation carbon nanotube technology, it is to collect carrier with inorganic ceramic pearl, is placed in tiltable tubular type rotary furnace high-temperature region, is passed through carbon source and catalyst carries out carbon nano tube growth.After growth terminates, tilting furnace simultaneously turns round simultaneously, scrapes off the carbon nanotube for being deposited on revolution furnace wall using ceramic bead, is separated into solid powder separator, carbon nanotube dust is brought into powder catcher by inert gas to collect, and finally obtains carbon nanotube.The preparation of carbon nanotube continuous batch can be achieved in the present invention, under the reaction condition for obtaining steady air flow field distribution, solves the problems, such as that carbon nano tube products Yi Lu inner tubal wall deposits, obtain high-quality carbon nanotube, and it is easy to amplify realization industrialization, there is Important Economic value.
Description
Technical field
The invention belongs to new material technology fields, are related to a kind of nano-carbon material, in particular to a kind of batch prepares carbon and receives
The device and method of mitron.
Background technique
The distinctive nanotube tubular structure of carbon nanotube imparts its excellent comprehensive performance, fills out in mechanics enhancing, conduction
It fills, the fields such as thermally conductive modification have important application.Wherein multi-walled carbon nanotube has been carried out industrialization, and large-scale application is in lithium electricity
Conductive additive field, new application field also constantly tend to be mature, gradually show a huge market space.Therefore,
It is great to realize that continuous batch production is that current carbon nanotube preparation technology further develops for the scale controllable preparation of carbon nanotube
Demand.The mainstream preparation method of field of carbon nanotubes is chemical vapour deposition technique at present, using splitting for organic carbon source at high temperature
Solution, goes out the sp2 hydridization carbon material of crystal type in catalyst surface deposition growing.Chinese invention patent CN200710098478.2 is public
The method and device for having opened a kind of producing Nano carbon tubes continuously, using fluidized-bed process, using catalyst in reaction cavity
Fluidized suspension state, is prepared carbon nanotube dust.Chinese invention patent CN201610378632.0 has disclosed one kind and has been used for
The automatically cleaning fluidized-bed reactor of carbon nanotube production, using the intracorporal stirring scratch board device of reaction chamber fluidisation may be adhered to
The carbon nanotube of bed reactor wall scrapes off, and shuts down cleaning without interval, obtains higher production efficiency.Chinese invention patent
CN201610772335.4 discloses a kind of carbon nanotube continuous generation device, by the laminate devices of setting, solves carbon nanometer
The problem of cavity inner wall is easily adhered in pipe production process, improves production efficiency.Existing technology of preparing is most of cannot be very
Solve the problems, such as that carbon nanotube is collected well, when preparing carbon nanotube in particular by floating chemical vapour deposition technique, carbon is received
Mitron is largely deposited on inside reaction cavity, cannot effectively be collected, extreme influence preparation efficiency and production cost.
Summary of the invention
The main purpose of the embodiment of the present disclosure is to provide a kind of device and method of batch preparation carbon nanotube, to overcome
Deficiency in the prior art.
To realize aforementioned invention purpose, the technical solution of the embodiment of the present disclosure are as follows: a kind of side of batch preparation carbon nanotube
Method, the method specifically includes the following steps:
S1 carrier) will be collected to be fitted into solids feeder, inert gas is passed through and empties air；
S2 tiltable tubular type rotary furnace) is adjusted to horizontality, is vacuumized, then switching is passed through inert gas；
S3 solids feeder) is opened, carrier will be collected and be fitted into tiltable tubular type rotary furnace；
S4 tubular type rotary furnace temperature program) is opened, assigned temperature is warming up to, switching is passed through carbon source, catalyst and mixing and carries
Gas；
S5) after reaction, stop being passed through gaseous mixture, switching is passed through inert gas, opens boiler tube slewing equipment, makes boiler tube
Certain time is rotated under certain revolving speed, later on tilting furnace mechanism tilts down furnace body towards discharge port, opens solid
Products therefrom is poured into and has been filled in the solid powder separator of inert gas by powder separator valve；
S6 after) closing the link valve of tube furnace and solid powder separator, solid powder separator turntable is opened, simultaneously
It is passed through inert gas, carrier will be collected and separated with powder product, into powder catcher, final product is obtained after separation.
S7) repeating S3-S6 can be realized the continuous batch preparation of carbon nanotube.
The S7) in iterative process, furnace body can not cool down, and realize continuous production.
According to the embodiment of the present disclosure, the S1) in collect supports-inorganic ceramic bead be zirconium oxide, aluminium oxide, silicon nitride, not
Come stone or quartz, 0.1 millimeter -5 millimeters of diameter；The inert gas can be nitrogen, argon gas and helium.
According to the embodiment of the present disclosure, the S4) specific temperature is 600-1200 DEG C, the reaction time -5 hours 10 minutes；
Mass ratio between the carbon source, catalyst and mixed carrier gas three are as follows: 5-30:0.05-5:50-200.
According to the embodiment of the present disclosure, the carbon source be methane, ethane, propane, n-hexane, heptane, ethylene, propylene, acetylene,
Methanol, ethyl alcohol, isopropanol, n-butanol, methyl ether, ether, benzene, toluene or dimethylbenzene；Catalyst is ferrocene；The mixed carrier gas
It is the gaseous mixture of inert gas and hydrogen, volume ratio between the two are as follows: 20:1~1:90.
According to the embodiment of the present disclosure, the S5) in 10-200 revs/min of boiler tube revolving speed, time 2-30 minute, inclined angle
10-45 ° of degree.
According to the embodiment of the present disclosure, the S6) in 50-200 revs/min of rotary speed of solid powder separator, time 2-
30 minutes.
According to the embodiment of the present disclosure, the S4) in growth promoter can also be added, the growth promoter is thiophene, is added
Entering mass ratio is 0.01-0.5.
The another object of the embodiment of the present disclosure is to provide a kind of device of the batch preparation carbon nanotube of above method, described
Device includes solids feeder, tiltable tubular type rotary furnace, solid powder separator, powder catcher, collects carrier and auxiliary
System；
The solids feeder, for adding materials into tiltable tubular type rotary furnace；
The tiltable tubular type rotary furnace is used for synthesizing carbon nanotubes；
The collection carrier, for being sticked to being collected in tiltable tubular type revolution furnace sidewall；
The solid powder separator, for being separated to the carbon nanotube being bonded on collection carrier surface；
The powder catcher, for the carbon nanotube after separation to be collected；
The auxiliary system, for being supplied for the tiltable tubular type rotary furnace, solid powder separator and powder catcher
Electricity, and provide reaction required unstrpped gas, reaction atmosphere and reaction environment；
Wherein, the solids feeder, tiltable tubular type rotary furnace, solid powder separator and powder catcher are successively close
Envelope series connection, and controlled and opened and closed by valve,
The auxiliary system includes vacuum system, air-channel system, power-supply system and cooling system, the vacuum system and institute
State the connection of tiltable tubular type rotary furnace；The air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid powder
Expect the air inlet connection of separator；The inside of the solids feeder is arranged in the cooling system.
According to the embodiment of the present disclosure, the furnace tube material of the tiltable tubular type rotary furnace is quartzy tube material, mid diameter
Greater than both ends diameter, both ends diameter: mid diameter=1:1.1~1:5, and boiler tube can continuous rotation, entire furnace body can be to boiler tube
Tail down tilts 0-45 °.
According to the embodiment of the present disclosure, the solid powder separator is the Double water-cooled stainless steel of bottom belt stirring blade
Bucket, and it can be passed through inert gas from bottom, the separation of solid material and powder is realized in whipping process, and powder is brought by air-flow
Collector.
The solids feeder is screw feed mechanism, and has inert gas shielding.
The powder catcher be centrifuge separation, cyclonic separation and be separated by filtration mode any one.
Compared with prior art, the invention has the advantages that
(1) it is used as the collection carrier of floating catalyst system preparation carbon nanotube simultaneously using ceramic bead, is also used as subsequent grinding
Carbon nanotube, the grinding inside the reaction chamber scrapes off abrasive media in the process, can will be in ceramic ball surface and reaction chamber
The carbon nano tube products of wall all collect；
(2) device realizes Ceramic Balls charging, chemical vapor deposition preparation, powder separation and collecting function simultaneously, can
Next batch production is gone successively in the case where furnace body does not cool down, and is realized prepared by batch, is reduced energy consumption, improve efficiency；
(3) using boiler tube rotating technics after reaction, during solving floating catalytic chemical deposition preparation carbon nanotube, greatly
The problem that amount carbon nanotube deposits inside reaction chamber, can not only effectively keep the technology stability of the preparation method, avoid rapids
Stream causes air-flow unstable, and realizes and quickly collect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the device that a kind of batch of the present invention prepares carbon nanotube.
Fig. 2 embodiment 1 is deposited directly to the Product scan electron micrograph of ceramic bead surface.
Figure is further amplified in the Product scan electron micrograph that Fig. 3 embodiment 1 is deposited directly to ceramic bead surface.
Carbon nano tube products electron scanning micrograph after the final separation of Fig. 4 embodiment 1.
The carbon nano tube products electron scanning micrograph that Fig. 5 embodiment 2 is prepared.
The carbon nano tube products electron scanning micrograph that Fig. 6 embodiment 3 is prepared.
In figure
1. tilting furnace device；2. feeding-in solid body device；3. boiler tube rotating device；4. quartzy burner hearth；5. reacting furnace；6. solid
Body powder separator；7. powder collector
Specific embodiment
Technical scheme is described further in the following with reference to the drawings and specific embodiments.
As shown in Figure 1, a kind of device of present invention batch preparation carbon nanotube, described device includes solids feeder, can
It tilts tubular type rotary furnace, solid powder separator, powder catcher, collect carrier and auxiliary system；
The solids feeder, for adding materials into tiltable tubular type rotary furnace；
The tiltable tubular type rotary furnace is used for synthesizing carbon nanotubes；
The collection carrier, for being sticked to being collected in tiltable tubular type revolution furnace sidewall；
The solid powder separator, for being separated to the carbon nanotube being bonded on collection carrier surface；
The powder catcher, for the carbon nanotube after separation to be collected；
The auxiliary system, for being supplied for the tiltable tubular type rotary furnace, solid powder separator and powder catcher
Electricity, and provide reaction required unstrpped gas, reaction atmosphere and reaction environment；
Wherein, the solids feeder, tiltable tubular type rotary furnace, solid powder separator and powder catcher are successively close
Envelope series connection, and controlled and opened and closed by valve,
The auxiliary system includes vacuum system, air-channel system, power-supply system and cooling system, the vacuum system and institute
State the connection of tiltable tubular type rotary furnace；The air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid powder
Expect the air inlet connection of separator；The inside of the solids feeder is arranged in the cooling system.
According to the embodiment of the present disclosure, the tiltable tubular type rotary furnace includes tilting furnace device and furnace body, the furnace body
It is arranged on the tilting furnace device, the furnace body includes reacting furnace and boiler tube, and the mid diameter of the boiler tube is greater than both ends
The medium position of the boiler tube is arranged in diameter, the reacting furnace；
Boiler tube both ends diameter: mid diameter=1:1.1~1:5, and boiler tube can continuous rotation, entire furnace body can be to furnace
Pipe tail down tilts 0-45 °.
According to the embodiment of the present disclosure, the solid powder separator is the Double water-cooled stainless steel of bottom belt stirring blade
Bucket, and it can be passed through inert gas from bottom, the separation of solid material and powder is realized in whipping process, and powder is brought by air-flow
Collector.
The solids feeder is screw feed mechanism, and has inert gas shielding.
The powder catcher be centrifuge separation, cyclonic separation and be separated by filtration mode any one
The another object of the embodiment of the present disclosure is to provide a kind of method of batch preparation carbon nanotube, and the method is specifically wrapped
Include following steps:
S1 carrier) will be collected to be fitted into solids feeder, inert gas is passed through and empties air；
S2 tiltable tubular type rotary furnace) is adjusted to horizontality, is vacuumized, then switching is passed through inert gas；
S3 solids feeder) is opened, carrier will be collected and be fitted into tiltable tubular type rotary furnace；
S4 tubular type rotary furnace temperature program) is opened, assigned temperature is warming up to, switching is passed through carbon source, catalyst and mixing and carries
Gas；
S5) after reaction, stop being passed through gaseous mixture, switching is passed through inert gas, opens boiler tube slewing equipment, makes boiler tube
Certain time is rotated under certain revolving speed, later on tilting furnace mechanism tilts down furnace body towards discharge port, opens solid
Products therefrom is poured into and has been filled in the solid powder separator of inert gas by powder separator valve；
S6 after) closing the link valve of tube furnace and solid powder separator, solid powder separator turntable is opened, simultaneously
It is passed through inert gas, carrier will be collected and separated with powder product, into powder catcher, final product is obtained after separation.
S7) repeating S3-S6 can be realized the continuous batch preparation of carbon nanotube.
The S7) in iterative process, furnace body can not cool down, and realize continuous production.
Embodiment 1
Batch prepare carbon nanotube device, by tiltable tubular type rotary furnace, solids feeder, solid powder separator,
Powder catcher successively seals series connection, and is controlled and opened and closed by valve.Solids feeder is screw feed mechanism, and is had lazy
Property gas shield；The furnace tube material of tiltable tubular type rotary furnace is quartzy tube material, and mid diameter is greater than both ends diameter, both ends
Diameter: mid diameter=1:1.5, boiler tube can continuous rotation, entire furnace body can to boiler tube tail down tilt 0-45 degree angle；Gu
Body powder separator is the Double water-cooled stainless steel barrel of bottom belt stirring blade, and can be passed through inert gas from bottom；Powder is received
Storage is to be separated by filtration mode；It in addition include vacuum system, air-channel system, power-supply system and cooling system there are also auxiliary system；
Vacuum system is connect with tiltable tubular type rotary furnace；Air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid
The air inlet of body powder separator connects；Cooling system is arranged in the double-jacket of solids feeder.
Carbon nanotube preparation flow are as follows: the mullite ceramic pearl of diameter 2mm is fitted into solids feeder, is passed through argon gas gas
Body empties air；Tubular type rotary furnace is adjusted to horizontality, is vacuumized, then switching is passed through argon gas；Open solid into
Porcelain bead is fitted into tubular type rotary furnace by glassware；Tubular type rotary furnace temperature program is opened, is warming up to 800 DEG C.By what is dissolved in advance
Catalyst solution (toluene solution of ferrocene) and mixed carrier gas (argon gas and hydrogen mixed gas, mass ratio 9:1) are passed through together
In reacting furnace, wherein carbon source: catalyst: mixed carrier gas mass ratio is 10:0.4:100, the reaction time 1 hour.After reaction,
Switching is passed through argon gas, opens boiler tube slewing equipment, rotates boiler tube 30 minutes under 50 revs/min of revolving speed, later on furnace
Body leaning device, make furnace body towards discharge port to 30 degree of angles of lower inclination, open solid powder separator valve, in turning course
It is middle to pour into ceramic bead and products therefrom in the solid powder separator for being filled with inert gas argon gas.Close tube furnace and solid
After the link valve of powder separator, solid powder separator turntable is opened, while being passed through big air-flow inert gas argon gas, will divided
It improves from device rotary speed to 100 revs/min, stirs 30 minutes, ceramic bead is separated with powder product, into powder catcher
In, final product is obtained after separation.Ceramic bead after separation can continue to reuse, and furnace body can enter next without cooling
Batch production.
The product appearance photo that Fig. 2 show ceramic bead used in embodiment 1 and preparation is collected.Fig. 3 is 1 ceramic bead of embodiment
Electron scanning micrograph after the deposition of carbon nanotubes of surface.Fig. 4 is embodiment after the separation of solid powder separator, powder
The Product scan electron micrograph collected in collecting bag.
Embodiment 2
Batch prepare carbon nanotube device, by tiltable tubular type rotary furnace, solids feeder, solid powder separator,
Powder catcher successively seals series connection, and is controlled and opened and closed by valve.Solids feeder is screw feed mechanism, and is had lazy
Property gas shield；The furnace tube material of tiltable tubular type rotary furnace is quartzy tube material, and mid diameter is greater than both ends diameter, both ends
Diameter: mid diameter=1:1.1, boiler tube can continuous rotation, entire furnace body can to boiler tube tail down tilt 0-45 degree angle；Gu
Body powder separator is the Double water-cooled stainless steel barrel of bottom belt stirring blade, and can be passed through inert gas from bottom；Powder is received
Storage is cyclonic separation mode；It in addition include vacuum system, air-channel system, power-supply system and cooling system there are also auxiliary system；
Vacuum system is connect with tiltable tubular type rotary furnace；Air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid
The air inlet of body powder separator connects；Cooling system is arranged in the double-jacket of solids feeder.
Carbon nanotube preparation flow are as follows: the zirconia ceramics pearl of diameter 0.1mm is fitted into solids feeder, is passed through nitrogen
Gas empties air；Tubular type rotary furnace is adjusted to horizontality, is vacuumized, then switching is passed through nitrogen gas；Open solid
Porcelain bead is fitted into tubular type rotary furnace by feeder；Tubular type rotary furnace temperature program is opened, is warming up to 600 DEG C.It will dissolve in advance
Catalyst solution (hexane solution of ferrocene) and mixed carrier gas (nitrogen and hydrogen mixed gas, mass ratio 20:1) together
Be passed through in reacting furnace, wherein carbon source: catalyst: mixed carrier gas mass ratio be 10:0.05:100, the reaction time 10 minutes.Reaction
After, switching is passed through nitrogen, opens boiler tube slewing equipment, so that boiler tube is rotated 30 minutes under 10 revs/min of revolving speed, then
Open tilting furnace mechanism, make furnace body towards discharge port to 30 degree angles of lower inclination, open solid powder separator valve, time
Ceramic bead and products therefrom are poured into the solid powder separator for being filled with inert nitrogen gas during turning.Close tube furnace
After the link valve of solid powder separator, solid powder separator turntable is opened, while being passed through big air-flow inert gas nitrogen
Gas improves separator rotary speed to 50 revs/min, stirs 30 minutes, ceramic bead is separated with powder product, into powder
In collector, final product is obtained after separation.
Embodiment 3
Batch prepare carbon nanotube device, by tiltable tubular type rotary furnace, solids feeder, solid powder separator,
Powder catcher successively seals series connection, and is controlled and opened and closed by valve.Solids feeder is screw feed mechanism, and is had lazy
Property gas shield；The furnace tube material of tiltable tubular type rotary furnace is quartzy tube material, and mid diameter is greater than both ends diameter, both ends
Diameter: mid diameter=1:5, boiler tube can continuous rotation, entire furnace body can to boiler tube tail down tilt 0-45 degree angle；Solid
Powder separator is the Double water-cooled stainless steel barrel of bottom belt stirring blade, and can be passed through inert gas from bottom；Powder is collected
Device is to be separated by filtration mode；It in addition include vacuum system, air-channel system, power-supply system and cooling system there are also auxiliary system；Very
Empty set system is connect with tiltable tubular type rotary furnace；Air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid
The air inlet of powder separator connects；Cooling system is arranged in the double-jacket of solids feeder.
Carbon nanotube preparation flow are as follows: the aluminium oxide ceramics pearl of diameter 5mm is fitted into solids feeder, is passed through helium gas
Body empties air；Tubular type rotary furnace is adjusted to horizontality, is vacuumized, then switching is passed through helium atmosphere；Open solid into
Porcelain bead is fitted into tubular type rotary furnace by glassware；Tubular type rotary furnace temperature program is opened, is warming up to 1200 DEG C.It will dissolve in advance
Catalyst solution (ethanol solution of ferrocene) and growth promoter thiophene, mixed carrier gas (helium and hydrogen mixed gas, quality
Than being passed through in reacting furnace together for 1:90), wherein carbon source: catalyst: growth promoter: mixed carrier gas mass ratio is 30:5:
0.5:200, the reaction time 1 hour.After reaction, switching is passed through helium, opens boiler tube slewing equipment, make boiler tube 200 turns/
Minute revolving speed under rotate 2 minutes, later on tilting furnace mechanism, make furnace body towards discharge port to 30 degree of angles of lower inclination,
Solid powder separator valve is opened, ceramic bead and products therefrom are poured into turning course and have been filled with inert gas helium
In solid powder separator.After closing the link valve of tube furnace and solid powder separator, opens solid powder separator and turn
Disk, while it being passed through big air-flow inert gas helium, separator rotary speed is improved to 200 revs/min, stirs 2 minutes, will make pottery
Porcelain bead is separated with powder product, and into powder catcher, final product is obtained after separation.
Embodiment 4
Batch prepare carbon nanotube device, by tiltable tubular type rotary furnace, solids feeder, solid powder separator,
Powder catcher successively seals series connection, and is controlled and opened and closed by valve.Solids feeder is screw feed mechanism, and is had lazy
Property gas shield；The furnace tube material of tiltable tubular type rotary furnace is quartzy tube material, and mid diameter is greater than both ends diameter, both ends
Diameter: mid diameter=1:1.5, boiler tube can continuous rotation, entire furnace body can to boiler tube tail down tilt 0-45 degree angle；Gu
Body powder separator is the Double water-cooled stainless steel barrel of bottom belt stirring blade, and can be passed through inert gas from bottom；Powder is received
Storage is to be separated by filtration mode；It in addition include vacuum system, air-channel system, power-supply system and cooling system there are also auxiliary system；
Vacuum system is connect with tiltable tubular type rotary furnace；Air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid
The air inlet of body powder separator connects；Cooling system is arranged in the double-jacket of solids feeder.
Carbon nanotube preparation flow are as follows: the quartz-ceramics pearl of diameter 2mm is fitted into solids feeder, is passed through argon gas
Air is emptied；Tubular type rotary furnace is adjusted to horizontality, is vacuumized, then switching is passed through argon gas；Open feeding-in solid body
Porcelain bead is fitted into tubular type rotary furnace by device；Tubular type rotary furnace temperature program is opened, is warming up to 850 DEG C.It is urged what is dissolved in advance
(argon gas and hydrogen mixed gas, mass ratio are for agent solution (diethyl ether solution of ferrocene) and carbon-source gas (methane), mixed carrier gas
It 9:1) is passed through in reacting furnace together, wherein carbon source (ether and methane): catalyst (ferrocene): mixed carrier gas (argon gas and hydrogen)
Mass ratio is 10:1:100, the reaction time 5 hours.After reaction, switching is passed through argon gas, opens boiler tube slewing equipment, makes furnace
Pipe rotates 30 minutes under 100 revs/min of revolving speed, later on tilting furnace mechanism, make furnace body towards discharge port to have a down dip
Oblique 30 degree of angles, open solid powder separator valve, ceramic bead and products therefrom poured into turning course be filled with it is lazy
In the solid powder separator of property gases argon.After closing the link valve of tube furnace and solid powder separator, solid is opened
Powder separator turntable, while it being passed through big air-flow inert gas argon gas, separator rotary speed is improved to 200 revs/min, is stirred
It mixes 30 minutes, ceramic bead is separated with powder product, into powder catcher, final product is obtained after separation.
Embodiment 5
Batch prepare carbon nanotube device, by tiltable tubular type rotary furnace, solids feeder, solid powder separator,
Powder catcher successively seals series connection, and is controlled and opened and closed by valve.Solids feeder is screw feed mechanism, and is had lazy
Property gas shield；The furnace tube material of tiltable tubular type rotary furnace is quartzy tube material, and mid diameter is greater than both ends diameter, both ends
Diameter: mid diameter=1:1.5, boiler tube can continuous rotation, entire furnace body can to boiler tube tail down tilt 0-45 degree angle；Gu
Body powder separator is the Double water-cooled stainless steel barrel of bottom belt stirring blade, and can be passed through inert gas from bottom；Powder is received
Storage is to be separated by filtration mode；It in addition include vacuum system, air-channel system, power-supply system and cooling system there are also auxiliary system；
Vacuum system is connect with tiltable tubular type rotary furnace；Air-channel system respectively with tiltable tubular type rotary furnace, solids feeder and solid
The air inlet of body powder separator connects；Cooling system is arranged in the double-jacket of solids feeder.
Carbon nanotube preparation flow are as follows: the silicon nitride ceramics pearl of diameter 0.8mm is fitted into solids feeder, is passed through argon gas
Gas empties air；Tubular type rotary furnace is adjusted to horizontality, is vacuumized, then switching is passed through argon gas；Open solid
Porcelain bead is fitted into tubular type rotary furnace by feeder；Tubular type rotary furnace temperature program is opened, is warming up to 950 DEG C.It will dissolve in advance
Catalyst solution (ethanol solution of ferrocene) and carbon-source gas (ethylene), growth promoter (thiophene), mixed carrier gas (argon gas
And hydrogen mixed gas, mass ratio 1:1) it is passed through in reacting furnace together, wherein carbon source (ethyl alcohol and ethylene): catalyst (two cyclopentadienyls
Iron): growth promoter (thiophene): mixed carrier gas (argon gas and hydrogen) mass ratio be 10:1:0.1:100, the reaction time 2 hours.
After reaction, switching is passed through argon gas, opens boiler tube slewing equipment, rotates boiler tube 30 minutes under 50 revs/min of revolving speed,
Later on tilting furnace mechanism, make furnace body towards discharge port to 30 degree of angles of lower inclination, open solid powder separator valve,
Ceramic bead and products therefrom are poured into the solid powder separator for being filled with inert gas argon gas in turning course.Close pipe
After the link valve of formula furnace and solid powder separator, solid powder separator turntable is opened, while being passed through big air-flow indifferent gas
Body argon gas improves separator rotary speed to 100 revs/min, stirs 30 minutes, ceramic bead is separated with powder product, into
Enter in powder catcher, final product is obtained after separation.
Although several embodiments of the present invention are had been presented for herein, it will be appreciated by those of skill in the art that In
Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment is only exemplary, no
It should be using the embodiments herein as the restriction of interest field of the present invention.
Claims (10)
1. a kind of device of batch preparation carbon nanotube, which is characterized in that described device includes solids feeder, tiltable tubular type
Rotary furnace, powder catcher, collects carrier and auxiliary system at solid powder separator；
The solids feeder, for adding materials into tiltable tubular type rotary furnace；
The tiltable tubular type rotary furnace is used for synthesizing carbon nanotubes；
The collection carrier, for being sticked to being collected in tiltable tubular type revolution furnace sidewall；
The solid powder separator, for being separated to the carbon nanotube being bonded on collection carrier surface；
The powder catcher, for the carbon nanotube after separation to be collected；
The auxiliary system, for powering for the tiltable tubular type rotary furnace, solid powder separator and powder catcher, with
And unstrpped gas, reaction atmosphere and reaction environment needed for reaction is provided；
Wherein, the solids feeder, tiltable tubular type rotary furnace, solid powder separator and powder catcher successively seal string
Connection, and controlled and opened and closed by valve,
The auxiliary system includes vacuum system, air-channel system, power-supply system and cooling system, the vacuum system and it is described can
Tilt the connection of tubular type rotary furnace；The air-channel system divides with tiltable tubular type rotary furnace, solids feeder and solid powder respectively
Air inlet connection from device；The inside of the solids feeder is arranged in the cooling system.
2. the apparatus according to claim 1, which is characterized in that the furnace tube material of the tiltable tubular type rotary furnace is quartz
Tube material, mid diameter be greater than both ends diameter, both ends diameter: mid diameter=1:1.1~1:5, and boiler tube can continuous rotation, it is whole
A furnace body can tilt 10-45 ° to boiler tube tail down.
3. the apparatus according to claim 1, which is characterized in that the solid powder separator is bottom belt stirring blade
Double water-cooled stainless steel barrel, and it can be passed through inert gas from bottom, the separation of solid material and powder is realized in whipping process,
Powder catcher is brought by air-flow.
4. according to device described in claim 1, which is characterized in that the collection supports-inorganic ceramic bead be zirconium oxide, aluminium oxide,
Silicon nitride, mullite or quartz；0.1 millimeter -5 millimeters of diameter.
5. a kind of method that batch using as described in claim 1-4 any one prepares carbon nanotube device batch preparation,
It is characterized by: the method specifically includes the following steps:
S1 carrier) will be collected to be fitted into solids feeder, be passed through inert gas evacuation of air；The inert gas is nitrogen, argon
Gas or helium；
S2 tiltable tubular type rotary furnace) is adjusted to horizontality, is vacuumized, then switching is passed through inert gas；
S3 solids feeder) is opened, carrier will be collected and be fitted into tiltable tubular type rotary furnace；
S4 tubular type rotary furnace temperature program) is opened, assigned temperature is warming up to, switching is passed through carbon source, catalyst and mixed carrier gas；
S5) after reaction, stop being passed through gaseous mixture, switching is passed through inert gas, opens boiler tube slewing equipment, makes boiler tube one
Determine to rotate certain time under revolving speed, later on tilting furnace mechanism tilts down furnace body towards discharge port, opens solid powder
Products therefrom is poured into and has been filled in the solid powder separator of inert gas by separator valve；
S6 after) closing the link valve of tube furnace and solid powder separator, solid powder separator turntable is opened, is passed through simultaneously
Inert gas will be collected carrier and be separated with powder product, into powder catcher, final product, carbon nanometer are obtained after separation
Pipe；
S7) repeating S3-S6 can be realized the continuous batch preparation of carbon nanotube.
6. according to the method described in claim 5, the it is characterized by: S4) specific temperature is 600-1200 DEG C, when reaction
Between -5 hours 10 minutes；Mass ratio between the carbon source, catalyst and mixed carrier gas three are as follows: 5-30:0.05-5:50-
200。
7. according to the method described in claim 6, it is characterized in that, the carbon source is methane, ethane, propane, n-hexane, heptan
Alkane, ethylene, propylene, acetylene, methanol, ethyl alcohol, isopropanol, n-butanol, methyl ether, ether, benzene, toluene or dimethylbenzene；Catalyst is
Ferrocene；The mixed carrier gas is the gaseous mixture of inert gas and hydrogen, volume ratio between the two are as follows: 20:1~1:90.
8. according to the method described in claim 5, the it is characterized by: S5) in 10-200 revs/min of boiler tube revolving speed, the time
2-30 minutes, 0-45 ° of inclined angle.
9. according to the method described in claim 5, the it is characterized by: S6) in solid powder separator rotary speed 50-
200 revs/min, time 2-30 minute.
10. according to the method described in claim 5, the it is characterized by: S4) in growth promoter, the life can also be added
Long promotor is thiophene, and addition mass ratio is 0.01-0.5.
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