CN110143583A - A kind of magnanimity prepares the method and device of carbon nanomaterial - Google Patents
A kind of magnanimity prepares the method and device of carbon nanomaterial Download PDFInfo
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- CN110143583A CN110143583A CN201910606995.9A CN201910606995A CN110143583A CN 110143583 A CN110143583 A CN 110143583A CN 201910606995 A CN201910606995 A CN 201910606995A CN 110143583 A CN110143583 A CN 110143583A
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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
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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
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/34—Length
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
Abstract
The invention belongs to technical field of nano material, are related to a kind of method that magnanimity prepares carbon nanomaterial, include the following steps: for hydrocarbon gas and inert gas to be input in plasma gun, carbon ion and hydrogen ion are ionized and thermally decomposed out in plasma gun；Make to enter in growth controller by ionizing and thermally decomposing open carbon ion and hydrogen ion, regenerates carbon nanocoils pipe or/and carbon nanopowder particle；The carbon nanocoils pipe or/and carbon nanopowder particle regenerated enters in cooling container, and the cooling gas released through cooling gas ring is quickly cooled down stable molding.The present invention also provides the devices that a kind of magnanimity prepares carbon nanomaterial.Magnanimity provided by the invention prepares the method and device of carbon nanomaterial, realizes the preparation of industrialization of carbon nanomaterial especially carbon nanocoils pipe, considerably reduces material manufacturing cost.
Description
Technical field
The invention belongs to technical field of nano material, it is related to the method and device that a kind of magnanimity prepares carbon nanomaterial.
Background technique
Carbon nanocoils pipe, carbon nanopowder particle are a kind of high performance nano materials, have excellent optical property, electricity
Performance and mechanical property become the hot spot of nano materials research in recent years.Especially carbon nanocoils pipe, when in electrocondution slurry
When, conductivity performance boost several times, electric conductivity is better than carbon nanopowder.The very good mechanical properties and electrochemistry having due to it
Performance, in lithium ion battery, photoelectric functional material, electromagnetic shielding, absorbing material, the fields such as high-performance composite materials have been obtained extensively
General application.But it is compressed in terms of due to current volume production, price is still high, at the main barrier of carbon nanomaterial large-scale application
Hinder.
Chinese invention patent CN102602912A discloses a kind of synthesizer of continuous production crystal whisker-shaped carbon nanotube, by
Spraying feeder, vertical synthetic furnace, heating device, the annular piston of hydraulic-driven, valve composition；The top of vertical synthetic furnace is
Storehouse is synthesized, centre is vacuum warehouse, and lower part is collecting bin, and atomization charger is mounted on the cover board of synthetic furnace top, and cover board solid exists
Synthetic furnace top, heating device along the synthesis storehouse position of vertical synthetic furnace external installation, the first valve be mounted on synthesis storehouse with
Between vacuum warehouse, the second valve is mounted between vacuum warehouse and collecting bin, and vacuum warehouse is equipped with a gas vent, and gas vent is connected to very
Sky pump.The patent produces carbon nanotube by way of being atomized and heating, and preparation efficiency is not high, cannot achieve magnanimity preparation.
Summary of the invention
The object of the present invention is to provide the method and devices that a kind of magnanimity prepares carbon nanomaterial, realize carbon nanometer material
The preparation of industrialization of material especially carbon nanocoils pipe, considerably reduces material manufacturing cost.
The purpose of the present invention is what is realized by following technological means:
A kind of method that magnanimity prepares carbon nanomaterial, includes the following steps:
(1) hydrocarbon gas and inert gas are input in plasma gun, ionize and thermally decomposes in plasma gun
Carbon ion and hydrogen ion out；
(2) make to enter in growth controller by ionizing and thermally decomposing open carbon ion and hydrogen ion, regenerate carbon
Nanometer spool or/and carbon nanopowder particle；
(3) the carbon nanocoils pipe or/and carbon nanopowder particle regenerated enters in cooling container, releases through cooling gas ring
The cooling gas of releasing is quickly cooled down stable molding.
(4) carbon nanocoils pipe or/and carbon nanopowder particle, cooling gas and the hydrogen for reconfiguring generation regenerated
Gas solid separation is carried out into gas-solid separator, carbon nanocoils pipe or/and carbon nanopowder particle are deposited in gas-solid separator bottom, gas
Body enters pipeline and enters circulation after heat exchanger is quickly cooled down.
Above-mentioned cooling gas can be recyclegas, be also possible to the disposable gas using rear emptying.
Above-mentioned plasma gun is catalytic behavior of materials rifle or DC power supply non-transferred arc plasma rifle.
Further include substitution gas before above-mentioned steps 1, the oxygen in system is first used into inert gas replacement, until oxygen content
Reach 5000ppm hereinafter, again using making the pressure in system between 50kpa-200kpa in inert gas input unit, it is excellent
106kpa-150kpa is selected, plasma electrical source is opened.
Above-mentioned DC power supply non-transferred arc plasma power supply adjusts required production in work according to hydrocarbon gas air inflow
Raw electric current is in 400A-1350A, and operating voltage is in 80-250V.
Above-mentioned hydrocarbon gas is selected from one of methane, ethane, ethylene, acetylene, styrene, benzene, toluene or a variety of, preferably
For methane, the inert gas is selected from one of argon gas, neon, xenon, helium or a variety of, preferably argon gas.
It is 1:5-0 that above-mentioned hydrocarbon gas and inert gas, which enter the intracavitary ratio of plasma,.
Temperature control in above-mentioned growth controller is for 2500 DEG C hereinafter, being by temperature control when producing carbon nanopowder particle
1500 DEG C hereinafter, controlling temperature when producing carbon nanocoils pipe is 1500 DEG C -2500 DEG C.
The conveying speed of above-mentioned hydrocarbon gas is the mark side 3-35/hour, and the line footpath of carbon nanocoils pipe is 35-280nm, long
Degree is 300-3000nm, and the diameter D50 of carbon nanopowder particle is 50-500nm.
The present invention also provides the device that a kind of magnanimity prepares carbon nanomaterial, the plasma including plasma power supply control
Body rifle, the inner cavity of plasma gun are connected with inertial gas tank, hydrocarbon gas storage tank, and the lower end of plasma gun is provided with life
Long controller, the lower end of growth controller are provided with cooling container, and gas cooling ring, the cooling appearance are provided in cooling container
Device connection gas-solid separator is simultaneously provided with getter device, and the gas vent of the gas-solid separator is sequentially connected heat exchanger and mixes
Gas reservoir is closed, mixed gas storage tank is connected to export mixed gas after cooling with gas cooling ring.
Above-mentioned mixed gas storage tank is connected by pipeline with growth controller, and gas flow is arranged on pipeline and controls
Device.
When above-mentioned plasma gun is DC power supply non-transferred arc plasma rifle, chamber set is using round shape inlet chamber set
By conductive metal material, such as copper alloy, carbon steel material, stainless steel material are made.Above-mentioned plasma gun is high-frequency induction etc.
When gas ions rifle, chamber set is using quartz or aluminum oxide material.
Above-mentioned growth controller includes cylindrical high-temperature resistant tube, is provided with high temperature heater (HTH) outside high-temperature resistant tube, outside heater
It is provided with for example heat-insulated carbon felt insulation of insulating or asbestos insulating layer, is provided with outside the cold protection of stainless steel water outside insulating layer
Shell, water cooling protection shell are provided with two layers, centre setting cooling medium.
High temperature heater (HTH) in above-mentioned growth controller generates heat using conventional Electric heating heating.
The diameter and length ratio of above-mentioned high-temperature resistant tube inner cylinder high temperature channel are 1:5-200.
Above-mentioned getter device is air blower or vacuum pump, after air blower or vacuum pump are separated for gas displacement and suction
Mixed gas, the gas-solid separator lower end are provided at solid collection, and vacuum intake storage barrel, vacuum are connected at solid collection
Suction storage barrel connects vacuum pump.
The power of above-mentioned air blower or vacuum pump is 10kw/h-100kw/h, per hour the largest of about carbon of output 32000g
Nanometer spool or/and carbon nanopowder particle.
Above-mentioned plasma gun is DC power supply non-transferred arc plasma rifle, is provided with inert gas, hydro carbons in cavity
The input channel of gas, and the electrode being electrically connected with plasma power supply, base part are provided with inner nozzle and outer nozzle.
Above-mentioned gas-solid separator structure is the gas-solid separator with cooling jacket, is provided in gas-solid separator lateral
Gas-solid separator is divided into epicoele and cavity of resorption by partition.Under intracavitary be alternatively arranged metal filtration pipe or/and Bag filter pipe, mistake
Chimney filter lower end closed, upper end are connected through a screw thread, and pass through diaphragm plate after-opening in epicoele.It is all provided in upper intracavitary each connecting tube
It is equipped with the solenoid valve of blowback air, is connected with by Y-pipe in the connecting tube between solenoid valve and partition and to be connected to air accumulator
Air supply pipe, the cavity of resorption of the connecting pipe connection gas-solid separator of cooling container, the gas outlet setting of gas-solid separator is in gas-solid point
Epicoele from device, gas-solid separator cavity of resorption lower part are provided at material collection.
The present invention having the beneficial effect that compared with the existing technology:
1, the present invention is bonded after being ionized and thermally decomposed using hydrocarbon gas through high growth temperature controller again, in the band of air-flow
Dynamic lower generation carbon nanocoils pipe or/and carbon nanopowder particle, realize the control of carbon nano shape.And pass through control growth control
Temperature, the mixed gas of device enter the internal channel of the flow of growth controller, the charging rate of hydrocarbon gas and growth controller
Length, the final form of product is controlled, to realize the preparation of the carbon nanocoils pipe or/and carbon nanopowder particle of various specifications.
2, hydrocarbon gas and inert gas are input in plasma gun by the present invention, are ionized out first in plasma chamber
Carbon ion and hydrogen ion, while there is the hydrocarbon gas for not yet ionizing chemical bond to go successively to catalytic behavior of materials rifle or straight
Ultrahigh-temperature (6000-18000 DEG C) the plasma arc region that galvanic electricity source non-transferred arc plasma rifle generates, hydrocarbon gas high warm
Decompose and generate carbon ion and hydrogen ion so that hydrocarbon gas more thoroughly dissociates, greatly improve hydrocarbon gas it is effective into
Tolerance reaches the purpose of magnanimity preparation.
3, a large amount of cooling gas forms continuous circulating cooling system, is greatly saved through electricity after heat exchanger is cooling
High-temperature mixed gas and material from rear generation need the cooling required gas cost of a large amount of cooling gas, to considerably reduce
Material manufacturing cost.
4, plasma gun, gas-solid separator, heat exchanger, heater, air blower, vacuum pump that the present invention uses etc. is equal
For conventional equipment, purchase and easy to assembly, it is low in cost.
5, the magnanimity preparation of carbon nanomaterial especially carbon nanocoils pipe may be implemented in method and apparatus provided by the invention,
It prepares speed and reaches as high as 32000g/h.
Detailed description of the invention
Fig. 1 is the device of the invention connection figure；
Fig. 2 is the structure chart of growth controller of the present invention；
Fig. 3 is the structure chart of plasma apparatus of the present invention；
Detailed description of the invention: 1, plasma power supply；2, plasma gun；3, inertial gas tank；4, hydrocarbon gas storage tank；5, raw
Long controller；6, cooling container；7, gas cooling ring；8, gas-solid separator；9, getter device；10, heat exchanger；11, it mixes
Gas reservoir；12, high-temperature resistant tube；13, heater；14, insulating layer；15, water cooling protects shell；16, vacuum intake storage barrel；
17, vacuum pump；18, input channel；19, electrode；20, inner nozzle；21, outer nozzle；22, partition；23, epicoele；24, cavity of resorption.
Specific embodiment
With specific embodiment, the invention will be further described with reference to the accompanying drawing, referring to Fig. 1-3.
A kind of continuous circulating cooling magnanimity prepares the device of carbon nanomaterial, the plasma controlled including plasma power supply 1
Body rifle 2, the inner cavity of plasma gun 2 are connected with inertial gas tank 3, hydrocarbon gas storage tank 4, and the lower end of plasma gun 2 is set
It is equipped with growth controller 5, the lower end of growth controller 5 is provided with cooling container 6, is provided with gas cooling ring in cooling container 6
7, the cooling container 6 connects gas-solid separator 8 and is provided with getter device 9, and the gas vent of the gas-solid separator 8 is successively
Connection heat exchanger 10 and mixed gas storage tank 11, mixed gas storage tank 11 are connected after cooling to export with gas cooling ring 7
Mixed gas.
Above-mentioned mixed gas storage tank 11 is connected by pipeline with growth controller 5, and gas flow control is arranged on pipeline
Device processed, for mixed gas to be input in growth controller 5.
Attached drawing 2 is compareed, above-mentioned growth controller 5 includes cylindrical high-temperature resistant tube 12, is provided with high temperature outside high-temperature resistant tube 12
Heater 13, heater 13 are provided with heat-insulated carbon felt insulation 14 outside, the cold protection shell of stainless steel water are provided with outside insulating layer 14
15.The diameter and length ratio of 12 inner cylinder high temperature channel of high-temperature resistant tube are 1:5-200.
Above-mentioned getter device 9 is air blower or vacuum pump, and 8 lower end of gas-solid separator is provided at solid collection, Gu
Vacuum intake storage barrel 16 is connected at body collection, vacuum intake storage barrel 16 connects vacuum pump 17.
Attached drawing 3 is compareed, above-mentioned plasma gun 2 is DC power supply non-transferred arc plasma rifle, is respectively set in cavity
There is the input channel 18 of inert gas, hydrocarbon gas, and the electrode 19 being electrically connected with plasma power supply, is provided with below electrode 19
Inner nozzle 20 and outer nozzle 21.Above-mentioned DC power supply non-transferred arc plasma rifle can also be substituted for catalytic behavior of materials
Rifle.
Above-mentioned gas-solid separator 8 is the gas-solid separator 8 with cooling jacket, is provided in gas-solid separator 8 lateral
Gas-solid separator 8 is divided into epicoele 23 and cavity of resorption 24 by partition 22.Metal filtration pipe or/and cloth bag have been alternatively arranged in cavity of resorption 24
Screen pipe, screen pipe lower end closed, upper end are connected through a screw thread, and pass through 22 after-opening of diaphragm plate in epicoele 23.In epicoele 23
It is provided with the solenoid valve of blowback air in each connecting tube, is connected in the connecting tube between solenoid valve and partition 22 by Y-pipe
It is connected to the air supply pipe being connected to air accumulator, the cavity of resorption 24 of the connecting pipe connection gas-solid separator 9 of cooling container 7, gas solid separation
The epicoele 23 of gas-solid separator 8 is arranged in the gas outlet of device 8, and 8 cavity of resorption of gas-solid separator, 24 lower part is provided at material collection.
Above-mentioned apparatus is equipped with various control air valves, water valve, various instruments, instrument, gas flowmeter and peace in corresponding site
Complete anti-exposure valve is with the trouble-free operation of control device.
The present invention is by the method that above-mentioned apparatus prepares carbon nanomaterial:
It opens getter device 9 and uses inert gas replacement to oxygen content 5000PPm hereinafter, defeated again the oxygen content in system
Entering inert gas makes the pressure in system reach 50kpa-200kpa, preferably 106kpa-150kpa.
Opening plasma power supply 1 will be in the hydrocarbon gas such as methane and inertial gas tank 3 in hydrocarbon gas storage tank 4
Inert gas such as argon gas are input among the inner cavity of plasma gun 2 through gas flow controller.
The hydrocarbon gas of input the intracavitary speed ionization and thermal decomposition with Millisecond of plasma gun 2 open carbon ion and
Hydrogen ion combine chemical bond, ionized and thermally decomposed open after carbon ion and hydrogen ion enter high growth temperature controller 5 into
And high temperature generates carbon nanocoils pipe or/and carbon nanopowder particle again, the specific form of generation passes through the temperature of growth controller 5
Degree, into the gas flow of growth controller 5, the charging rate of hydrocarbon gas and growth controller 5 internal channel length into
Row is adjusted, and the mixture of the two also can be generated.
Carbon nanomaterial enters in cooling container 6, then the combination cooling gas largely released through cooling gas ring 7 is to height
Winner rice noodles or/and high temperature carbon nanopowder high efficiency particulate are quickly cooled down stable formation, then will cool down the carbon nanocoils pipe in container 6
Or/and carbon nanopowder particle and the ionization hydrogen ion hydrogen reconfigured the and mixed gas largely released through cooling ring, lead to
The suction for crossing getter device 9 enters gas-solid separator 8 through connecting pipe, to carbon nanocoils pipe or/and carbon nanopowder particle and mixes
It closes gas and carries out gas solid separation.
By separation, carbon nanocoils pipe or/and carbon nanopowder granular materials are retained in into 8 intracavity bottom of gas-solid separator,
Mixed gas after separation enters in heat exchanger 10 after getter device 9 to exchange heat, and hot mixing gas is rapidly cooled
To 90 degrees Celsius hereinafter, being sent into mixed gas storage tank 11 through pipeline, then will be cooled down by connecting pipe through gas flow controller
Mixed gas formation afterwards, which moves in circles, to be sent into gas cooling ring 7.
The high temperature carbon nanocoils pipe or/and carbon nanopowder particles that ejected by high growth temperature controller be quickly cooled down stablize at
After shape, it is gathered at the solid collection of 8 lower end of gas-solid separator, starting vacuum pump 17 vacuumizes vacuum intake storage barrel 16,
To 50kpa-80kpa, 8 bottom valve of gas-solid separator is opened by the material vacuum in gas-solid separator 8 and is pumped to vacuum intake
In storage barrel 16, non-stop-machine continuous production is formed.
Above-described embodiment is only presently preferred embodiments of the present invention, is not limited the scope of the invention according to this, therefore: it is all according to
The equivalence changes that structure of the invention, shape, principle are done, should all be covered by within protection scope of the present invention.
Claims (10)
1. a kind of method that magnanimity prepares carbon nanomaterial, which comprises the steps of:
(1) hydrocarbon gas and inert gas are input in plasma gun, carbon is ionized and thermally decomposed out in plasma gun
Ion and hydrogen ion；
(2) make to enter in growth controller by ionizing and thermally decomposing open carbon ion and hydrogen ion, regenerate carbon nanometer
Spool or/and carbon nanopowder particle；
(3) the carbon nanocoils pipe or/and carbon nanopowder particle regenerated enters in cooling container, releases through cooling gas ring
Cooling gas be quickly cooled down stable molding.
2. the method that a kind of magnanimity according to claim 1 prepares carbon nanomaterial, which is characterized in that the step is also wrapped
It includes: the carbon nanocoils pipe or/and carbon nanopowder particle that regenerate, cooling gas and reconfiguring the hydrogen of generation and enter gas-solid
Separator carries out gas solid separation, and carbon nanocoils pipe or/and carbon nanopowder particle are deposited in gas-solid separator bottom, and gas enters pipe
Road enters circulation after heat exchanger is quickly cooled down.
3. the method that a kind of magnanimity according to claim 1 prepares carbon nanomaterial, which is characterized in that the hydrocarbon gas
Selected from one of methane, ethane, ethylene, acetylene, styrene, benzene, toluene or a variety of, preferably methane, the inert gas
Selected from one of argon gas, neon, xenon, helium or a variety of, preferably argon gas.
4. the method that a kind of magnanimity according to claim 1 prepares carbon nanomaterial, which is characterized in that the hydrocarbon gas
Entering the intracavitary ratio of plasma with inert gas is 1:5-0.
5. the method that a kind of magnanimity according to claim 1 prepares carbon nanomaterial, which is characterized in that the growth control
Temperature control in device is 2500 DEG C or less.
6. the method that a kind of magnanimity according to claim 1 prepares carbon nanomaterial, which is characterized in that the hydrocarbon gas
Conveying speed be the mark side 3-35/hour, the line footpath of carbon nanocoils pipe is 35-280nm, length 300-3000nm, carbon nanometer
The diameter D50 of powder particles is 50-500nm.
7. the device that a kind of magnanimity prepares carbon nanomaterial, which is characterized in that the plasma gun including plasma power supply control,
The inner cavity of plasma gun is connected with inertial gas tank, hydrocarbon gas storage tank, and the lower end of plasma gun is provided with growth control
Device processed, the lower end of growth controller are provided with cooling container, and gas cooling ring is provided in cooling container, and the cooling container connects
It connects gas-solid separator and is provided with getter device, the gas vent of the gas-solid separator is sequentially connected heat exchanger and gaseous mixture
Body storage tank, mixed gas storage tank are connected to export mixed gas after cooling with gas cooling ring.
8. the device that a kind of magnanimity according to claim 7 prepares carbon nanomaterial, which is characterized in that the growth control
Device includes cylindrical high-temperature resistant tube, and high temperature heater (HTH) is provided with outside high-temperature resistant tube, is provided with insulating outside heater, is kept the temperature
Layer is outer to be provided with the cold protection shell of stainless steel water.
9. the device that a kind of magnanimity according to claim 8 prepares carbon nanomaterial, which is characterized in that the high-temperature resistant tube
The diameter and length ratio of inner cylinder high temperature channel are 1:5-200.
10. the device that a kind of magnanimity according to claim 7 prepares carbon nanomaterial, which is characterized in that the air-breathing dress
It is set to air blower or vacuum pump, the gas-solid separator lower end is provided at solid collection, and vacuum intake is connected at solid collection
Storage barrel, vacuum intake storage barrel connect vacuum pump.
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Cited By (2)
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| CN111470488A (en) * | 2019-10-16 | 2020-07-31 | 中山大学 | Growth method of one-dimensional carbon chain |
| CN117483772A (en) * | 2023-12-29 | 2024-02-02 | 西安赛隆增材技术股份有限公司 | Powder preparation method of plasma atomization powder preparation equipment |
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| CN206635042U (en) * | 2017-03-27 | 2017-11-14 | 江永斌 | A kind of continuous volume production silicon nanowires group or the device of silicon flocculence cluster of grains |
| CN108746652A (en) * | 2018-06-22 | 2018-11-06 | 上海硕余精密机械设备有限公司 | A kind of preparation facilities of metal powder and preparation method thereof |
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| CN1537808A (en) * | 2004-04-07 | 2004-10-20 | 太原理工大学 | Aggregation-state fuller carbon nanometer micro-crystal and its preparation method |
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