CN106276846A - A kind of system and method preparing CNT - Google Patents
A kind of system and method preparing CNT Download PDFInfo
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- CN106276846A CN106276846A CN201610561905.5A CN201610561905A CN106276846A CN 106276846 A CN106276846 A CN 106276846A CN 201610561905 A CN201610561905 A CN 201610561905A CN 106276846 A CN106276846 A CN 106276846A
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Abstract
The invention belongs to carbon nanotube preparation technology field, be specifically related to a kind of system and method preparing CNT.Described system is nine grids flame reactor, and the agent structure of reactor is symmetrical, and shape of cross section is nine grids；Be positioned at centre grid is flame of centre passage, and be positioned on four angles is four external flame passages that are identical and that be centrosymmetric；Between every two adjacent external flame passages, be disposed with four identical and be centrosymmetric prepare reaction channel.The flame reactor that the present invention provides with continuous producing carbon nano-tube, and can have low cost, yield height, equipment and the simple advantage of operational approach.
Description
Technical field
The invention belongs to carbon nanotube preparation technology field, be specifically related to a kind of system and method preparing CNT.
Background technology
CNT is described as " king of nanometer ", shows the most surprising characteristic, such as its strength modulus and diamond
Almost identical, have fabulous flexibility；Can non-resistance ground conveying electric current under room temperature；Nano electron device etc. can be constructed.Therefore, more
Carrying out the most scholars and begin one's study it, CNT has become one of research topic the most popular in the world.CNT has
Having typical cannulated structure, tube wall is the hexagon carbocyclic ring structure being combined by the carbon atom of class graphite crystal and being formed
Become.The radial dimension of CNT is less, and caliber is typically about several nanometers to several tens of nanometers, but the length of pipe can reach
Micron dimension, has the biggest draw ratio, and therefore, CNT is considered as a kind of typical monodimension nanometer material.
For many years, the technology of preparing of CNT is constantly subjected to the concern of domestic and international scientist.At present, the system of CNT
Preparation Method mainly has four kinds: arc discharge method, laser evaporization method, chemical vapour deposition technique and flame method.Wherein, first three methods
Research work carry out more, comparative maturity the most, but this several method at aspects such as cost, equipment, operations by relatively
Big restriction.And although the flame method preparing CNT existed achieves the target that cost is relatively low, easy to operate, but
Most of yield are the highest, and the utilization rate of carbon source is relatively low, and equipment is the simplest, does not possess a large amount of quantity-produced condition.
Therefore, it is necessary to seek more effective preparation method of carbon nano-tube so that the preparation process of CNT continuously, batch
Amount, controlled, low cost, equipment are simple and convenient to operate.
Summary of the invention
The invention provides a kind of system and method preparing CNT, concrete technical scheme is as follows:
A kind of system preparing CNT, described system is nine grids flame reactor, the agent structure pair of reactor
Claiming, shape of cross section is nine grids；Be positioned at centre grid is flame of centre passage, be positioned on four angles be four completely
External flame passage that is identical and that be centrosymmetric；Between every two adjacent external flame passages, it is disposed with four complete phases
With and be centrosymmetric prepare reaction channel.
Preferably, it is respectively positioned at the upper end outlet of flame of centre passage and external flame passage and prepares reaction channel height
In place of 5%～50%, and passage of flame and the relative altitude prepared between reaction channel can be adjusted as required.
Preferably, four angles of reactor top are respectively provided with a piece of fin.
Utilize the method that system as above prepares CNT: fuel gas and air are from flame of centre passage and four
The lower end input of bar external flame passage, is ignited at upper end outlet, forms flame of centre straight up and external flame,
Thus for preparing the heat energy needed for CNT provides；Reacting gas is from four lower end inputs preparing reaction channel, the most completely
Remaining carbon-source gas and other flammable reacting gas of reaction are ignited at upper end outlet；At flame of centre and external flame
Dual-heated effect under, there is chemical reaction in the carbon-source gas in reacting gas within preparing reaction channel, decomposited before this
Substantial amounts of carbon atom, after then carbon atom experiences the process of a succession of complexity, separates out and stone on the surface of active catalyst particles
Mo Hua, and then nucleating growth is CNT；Carbon-source gas decomposites the process of substantial amounts of carbon atom and is preparing reaction channel
Lower half is carried out, and carbon atom is combined into the process of CNT to be carried out at the first half preparing reaction channel.
Preferably, described fuel gas is the acetylene that flame is concentrated, caloric value is high.
Preferably, described reacting gas is CO, H2And He, wherein CO is described carbon-source gas, H2For flammable reaction gas
Body.
Preferably, use contactless thermometer to measure carbon atom dissociation reaction district and prepare reaction zone with CNT
Temperature.
Preferably, described contactless thermometer is thermocouple.
Preferably, gas mass flow controller is used the mass flow of gas to be measured and controls, and by joining
The mass flow of gas is observed and recorded to the read out instrument of set.
Preferably for the CNT prepared, sampling mode is: by sampling substrate from the upper end preparing reaction channel
Near exit samples, or sample probe stretches into the inside sampling preparing reaction channel.
Be respectively positioned at the upper end outlet of flame of centre passage and external flame passage prepare reaction channel height 5%～
In place of 50%, and passage of flame and the relative altitude prepared between reaction channel can be adjusted as required.This structure
Mode is naturally enough separated the generation process of the dissociation process of carbon atom with CNT, beneficially the control of preparation condition
System, sampling mode also becomes simple and flexible.
Prepare reaction channel the most simultaneously by the dual and Bidirectional heating effect of flame of centre Yu external flame, make for each
The heats of flame becomes apparent from, prepare being uniformly heated of gas in reaction channel, be conducive to improving heating-up temperature,
Eliminate temperature deviation.
Article four, prepare reaction channel identical and be centrosymmetric, just the same with heating condition by hot mode, each bar
In passage, the composition of gas and flow do not have difference, i.e. these four physical and chemical conditions prepared in reaction channel complete one yet
Cause, it is ensured that the CNT prepared all does not has bigger difference in terms of form, quality.So, only need to be these four systems
Standby reaction channel samples, by contrasting the form of four groups of samples, quality simultaneously, it is possible to eliminate the occasionality of experimental result, increases
The credibility of strong experiment and cogency；The position gone wrong in reactor can also be rapidly found out when breaking down；In addition
Also a saving the sampling waiting time of repeated experiment, drastically increase efficiency.
Owing to external flame passage is in atmospheric environment, therefore when the flame temperature required is not the highest, it is not necessary to
Wherein input air, the flow of the fuel gas that only need to fix or change input can maintain outside burning or the regulation of external flame
Enclose the temperature of flame.Although the surrounding of flame of centre passage is all produced reaction channel and is surrounded, but remain complete above it
Open wide, have enough air can maintain the burning of flame of centre, to regulate the temperature of flame of centre, can be to central flame
The air that the input of flame passage is appropriate.
External flame passage is not fixed together with preparing reaction channel, and the relative altitude between them can be random
Change, is so conducive to controlling and regulate the dissociation temperature of carbon atom and the generation temperature of CNT.Dissociating carbon atom
React the reaction of formation with CNT to be controlled by respectively, the generation process of CNT can be controlled more preferably, quickly, with
Time be conducive to experimental result being analyzed and discussing.
Meanwhile, it is respectively positioned at the upper end outlet of flame of centre passage and external flame passage and prepares reaction channel height
In place of 5%～50%, and the relative altitude between them can be adjusted as required, is conducive to controlling respectively carbon atom solution
Temperature from reaction zone Yu CNT reaction of formation district.
In the present invention, preparing the reacting gas in reaction channel is CO, H2And He.CO provides carbon source, and it can be by competing
Striving active site stops catalyst surface to be covered by amorphous carbon, and makes oarse-grained ferrum crush, and produces more active surface.H2
Make CO hydrogenation separate out carbon, and promote that the carbon of dissociation is by ferrum granular absorption, beneficially carbon nano tube growth, moreover it is possible to keep catalyst
Activity.He primarily serves the effect of partial dilution and cooling, carries vaporific catalyst and enters the helium of reactor and also affect and urge
The supply rate of agent.It addition, H2Also have carbon nano tube surface purging and the effect of purification with He, simultaneously also can be effectively
Maintain the activity of catalyst.
In a particular embodiment, CO can be substituted by other carbon source.
Respectively being provided with a piece of fin on four angles of nine grids type reactor top, on the one hand they can cause periphery
Produced CO after flame combustion2Streaming of gas, in order to produced CO after burning with flame of centre2Gas converges, and makes a large amount of
CO2Reaction channel top is prepared in gas encirclement, hinders the entrance of oxygen, thus forms the environment of relatively hypoxia, reduces preparation anti-
Answer the flame temperature on passage top, prevent the CNT of preparation to be burned off, be favorably improved the yield of CNT；The opposing party
Face promotes external flame backflow, with overheavy firing, improves the utilization rate of fuel gas, saves fuel.
In the present invention, carbon atom dissociation reaction district is the highest with the temperature that CNT is prepared needed for reaction zone, it is impossible to make
Measure with general thermometer.Simultaneously, it is contemplated that the factor of accuracy of measurement, thus select high-precision thermocouple non-with other
Contact tehermometer measures temperature.
The flame reactor that the present invention provides can with continuous producing carbon nano-tube, and have that low cost, yield is high, equipment with
The simple advantage of operational approach.
Accompanying drawing explanation
Fig. 1 is the top view of nine grids type reactor；
Fig. 2 is the 3D schematic diagram (laterally overlooking) of nine grids type reactor；
Fig. 3 is the 3D schematic diagram (laterally looking up) of nine grids type reactor；
Label in figure: 1-external flame passage, 2-flame of centre passage, 3-prepares reaction channel, 4-fin, 5-nine grids
Flame reactor, 6-reacting gas inputs, and 7-flame fuel inputs.
Detailed description of the invention
The present invention is described further with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 show a kind of nine grids flame reactor preparing CNT, and the agent structure of reactor is symmetrical, transversal
Face is shaped as nine grids；Be positioned at centre grid is flame of centre passage, be positioned on four angles be four identical and
The external flame passage being centrosymmetric；Between every two adjacent external flame passages, be disposed with four identical and in
Centrosymmetric prepare reaction channel.
Preparation reaction it is respectively positioned on logical at upper end outlet from Fig. 2, Fig. 3, flame of centre passage and external flame passage
In place of the 5%～50% of road height, and passage of flame and the relative altitude prepared between reaction channel can be carried out as required
Adjust.And on four angles of reactor top, a piece of fin is respectively installed.
Utilize the method that system as above prepares CNT: acetylene and air are from flame of centre passage and four
Enclose the lower end input of passage of flame, be ignited at upper end outlet, form flame of centre straight up and external flame；CO、
H2With He from four lower end inputs preparing reaction channel, H2And the remaining CO reacted the most completely is ignited at upper end outlet；
Under the flame of centre dual-heated effect with external flame, there is chemical reaction in CO within preparing reaction channel, decomposed before this
Go out substantial amounts of carbon atom, after then carbon atom experiences the process of a succession of complexity, separate out also on the surface of active catalyst particles
Graphitization, and then nucleating growth is CNT；Carbon-source gas decomposites the process of substantial amounts of carbon atom and is preparing reaction channel
Lower half carry out, carbon atom is combined into the process of CNT to be carried out at the first half preparing reaction channel.
Use contactless thermometer to measure carbon atom dissociation reaction district and CNT and prepare the temperature of reaction zone.Adopt
With gas mass flow controller the mass flow of gas measured and control, and being come by supporting read out instrument
Observe and the mass flow of record gas.For the CNT prepared, sampling mode is: by sampling substrate from preparation reaction
Sampling near the upper end outlet of passage, or sample probe is stretched into the inside sampling preparing reaction channel.
Claims (10)
1. the system preparing CNT, it is characterised in that described system is nine grids flame reactor (5), reactor
Agent structure symmetrical, shape of cross section is nine grids；Be positioned at centre grid is flame of centre passage (2), is positioned at four
On angle is four external flame passages (1) that are identical and that be centrosymmetric；Every two adjacent external flame passages (1)
Between, be disposed with four identical and be centrosymmetric prepare reaction channel (3).
Nine grids flame reactor the most according to claim 1, it is characterised in that flame of centre passage (2) and periphery fire
Be respectively positioned at the upper end outlet of flame passage (1) prepare reaction channel (3) height 5%～50% in place of, and passage of flame with
The relative altitude prepared between reaction channel (3) can be adjusted as required.
Nine grids flame reactor the most according to claim 1, it is characterised in that each on four angles of reactor top
A piece of fin (4) is installed.
4. utilize the method that the system described in any one of claim 1-3 prepares CNT, it is characterised in that fuel gas with
Air inputs from the lower end of flame of centre passage (2) and four external flame passages (1), is ignited at upper end outlet, is formed
Flame of centre straight up and external flame；
Reacting gas from four lower ends inputs preparing reaction channel (3), the remaining carbon-source gas reacted the most completely and other can
The reacting gas of combustion is ignited at upper end outlet；Under the flame of centre dual-heated effect with external flame, reacting gas
In carbon-source gas within preparing reaction channel (3), there is chemical reaction, decomposited substantial amounts of carbon atom, then carbon atom before this
After experiencing the process of a succession of complexity, separate out and graphitization on the surface of active catalyst particles, and then nucleating growth is that carbon is received
Mitron；
Carbon-source gas decomposites the process of substantial amounts of carbon atom to be carried out in the lower half preparing reaction channel (3), and carbon atom combines
Process for CNT is carried out at the first half preparing reaction channel (3).
Method the most according to claim 4, it is characterised in that described fuel gas is acetylene.
Method the most according to claim 4, it is characterised in that described reacting gas is CO, H2And He, wherein CO is described
Carbon-source gas, H2For flammable reacting gas.
Method the most according to claim 4, it is characterised in that use contactless thermometer to measure carbon atom and dissociate instead
District and CNT is answered to prepare the temperature of reaction zone.
Method the most according to claim 5, it is characterised in that described contactless thermometer is thermocouple.
Method the most according to claim 4, it is characterised in that use the gas mass flow controller quality stream to gas
Amount measures and controls, and is observed and recorded the mass flow of gas by supporting read out instrument.
Method the most according to claim 4, it is characterised in that for the CNT prepared, sampling mode is: by
Sampling substrate is from preparing sampling near the upper end outlet of reaction channel (3), or is stretched into by sample probe and prepare reaction channel (3)
Internal sampling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610561905.5A CN106276846B (en) | 2016-07-15 | 2016-07-15 | A kind of system and method for preparing CNT |
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| CN201610561905.5A CN106276846B (en) | 2016-07-15 | 2016-07-15 | A kind of system and method for preparing CNT |
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| CN106276846A true CN106276846A (en) | 2017-01-04 |
| CN106276846B CN106276846B (en) | 2018-02-23 |
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Citations (10)
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|---|---|---|---|---|
| CN1297218A (en) * | 1999-11-05 | 2001-05-30 | 李铁真 | Field-emission display device using vertically arranged nanometer carbon tubes and its mfg. method |
| CN1328958A (en) * | 2001-07-22 | 2002-01-02 | 太原理工大学 | Preparation of carbon nanometer pipe material and its equipment |
| CN1454838A (en) * | 2002-04-29 | 2003-11-12 | 中国科学院成都有机化学研究所 | Reaction unit and process of continuous preparation of carbon nano-tube |
| CN2632063Y (en) * | 2003-07-04 | 2004-08-11 | 上海扬泽纳米新材料有限公司 | Electrode device for producing carbon nanometer tube by arc process |
| CN2666887Y (en) * | 2003-10-28 | 2004-12-29 | 黄德欢 | Apparatus for continuous producing carbon nano-tube |
| CN1830766A (en) * | 2005-02-19 | 2006-09-13 | 三星Sdi株式会社 | Carbon nanotube structure and method of manufacturing the same, field emission device and method of manufacturing the same |
| CN1837034A (en) * | 2005-03-25 | 2006-09-27 | 清华大学 | Carbon nanotube array growing device |
| CN1850594A (en) * | 2005-04-22 | 2006-10-25 | 清华大学 | Apparatus for preparing carbon nano tube array structure |
| CN1915805A (en) * | 2005-08-19 | 2007-02-21 | 清华大学 | Device and method for preparing array of Nano carbon tube |
| CN1951804A (en) * | 2005-10-21 | 2007-04-25 | 鸿富锦精密工业（深圳）有限公司 | Carbon nanotube preparation apparatus |
-
2016
- 2016-07-15 CN CN201610561905.5A patent/CN106276846B/en not_active Expired - Fee Related
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297218A (en) * | 1999-11-05 | 2001-05-30 | 李铁真 | Field-emission display device using vertically arranged nanometer carbon tubes and its mfg. method |
| CN1328958A (en) * | 2001-07-22 | 2002-01-02 | 太原理工大学 | Preparation of carbon nanometer pipe material and its equipment |
| CN1454838A (en) * | 2002-04-29 | 2003-11-12 | 中国科学院成都有机化学研究所 | Reaction unit and process of continuous preparation of carbon nano-tube |
| CN2632063Y (en) * | 2003-07-04 | 2004-08-11 | 上海扬泽纳米新材料有限公司 | Electrode device for producing carbon nanometer tube by arc process |
| CN2666887Y (en) * | 2003-10-28 | 2004-12-29 | 黄德欢 | Apparatus for continuous producing carbon nano-tube |
| CN1830766A (en) * | 2005-02-19 | 2006-09-13 | 三星Sdi株式会社 | Carbon nanotube structure and method of manufacturing the same, field emission device and method of manufacturing the same |
| CN1837034A (en) * | 2005-03-25 | 2006-09-27 | 清华大学 | Carbon nanotube array growing device |
| CN1850594A (en) * | 2005-04-22 | 2006-10-25 | 清华大学 | Apparatus for preparing carbon nano tube array structure |
| CN1915805A (en) * | 2005-08-19 | 2007-02-21 | 清华大学 | Device and method for preparing array of Nano carbon tube |
| CN1951804A (en) * | 2005-10-21 | 2007-04-25 | 鸿富锦精密工业（深圳）有限公司 | Carbon nanotube preparation apparatus |
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| CN106276846B (en) | 2018-02-23 |
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