CN100484869C - Method for preparing carbon nano tube using high power plasma generator - Google Patents
Method for preparing carbon nano tube using high power plasma generator Download PDFInfo
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- CN100484869C CN100484869C CNB2006100409362A CN200610040936A CN100484869C CN 100484869 C CN100484869 C CN 100484869C CN B2006100409362 A CNB2006100409362 A CN B2006100409362A CN 200610040936 A CN200610040936 A CN 200610040936A CN 100484869 C CN100484869 C CN 100484869C
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- coal dust
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Abstract
The great power plasma generator process of preparing carbon nanotube includes the following steps: introducing work gas hydrogen, nitrogen or argon to the plasma generator; initiating the power source of the plasma generator to ionize hydrogen into hydrogen plasma and to form hydrogen plasma jet at 1,800-30,000 K; and conveying coal powder of 120 micron below size with hydrogen to the high temperature plasma jet to react for 10-40 ms so as to form carbon nanotube in the mixing reaction area and the below inner wall. The plasma generator has output power adjustable in 200 KW to 2 MW, and has work gas of hydrogen, nitrogen, argon or their mixture. The power of the plasma generator and the sort and flow rate of the work gas may be regulated for producing carbon nanotube and acetylene.
Description
Technical field
The invention belongs to plasma body and nanometer material science research field.Be specifically related to prepare the method for carbon nanotube, used equipment configuration and processing condition with plasma generator.
Background technology
Carbon nanotube is a kind of novel carbon nanomaterial, and typical carbon nanotube is the hollow tubule that the coaxial circles cylinder by a plurality of carbon atom hexagonal lattices constitutes, the only several nanometers to tens of a diameter nanometer, and length can reach micron dimension, is the ideal one-dimensional material.Up to the present Single Walled Carbon Nanotube and multi-walled carbon nano-tubes two big class carbon nanotubes have been prepared.The carbon nanotube particular structure has determined its physicochemical property and potential Application Areas thereof.Carbon nanotube has the unique electrical performance of an emission characteristic and double electrical property, and the electric property of these two uniquenesses makes carbon nanotube be used as the aspect such as probe, Field Emission Display of Scanning Probe Microscopy.Carbon nanotube is because the class graphite linings space between its nano level pipeline configuration and the multi-walled carbon nano-tubes makes it can be used as the hydrogen storage material of hydrogen fuel cell.Carbon nanotube can also be as the electrode materials of ultracapacitor because size is little, specific surface area is big, the adsorption activation ability can be used for making chemical sensor and catalyzer by force.Carbon nanotube has advantages such as the strong and good stability of stronger wide-band microwave absorptive character, high-temperature oxidation resistance, can be used for making stealth material, electromagnetic shielding material.
Since lijima found carbon nanotube in 1991 first in the cathode deposit of arc discharge method production soccerballene since, people had developed the multiple method for preparing carbon nanotube, mainly contain arc process, laser evaporation method, chemical Vapor deposition process.The required graphite rod of arc process costs an arm and a leg, electrode materials consumption is many; Production unit power is less, is generally tens kilowatts, and impurity such as the carbon nanotube of preparation and decolorizing carbon are sintered in one, are unfavorable for carbon nanotube separation and purification.But laser evaporation method manufacture order wall carbon nano tube, the equipment complexity of this method involves great expense, and promotes the use of to have difficulties.There is crystal defect in the carbon nanotube of chemical Vapor deposition process preparation, degree of graphitization is poor, influence the mechanical property and the physicals of carbon nanotube, therefore be necessary carbon nanotube is carried out aftertreatment, the carbon nanotube degree of graphitization is uprised as The high temperature anneal.
Summary of the invention
Weak point at above-mentioned preparation carbon nanotube technology, the invention provides a method of utilizing high power plasma generator to prepare carbon nanotube, adopt the present invention can realize that cracking in plasma jet prepares carbon nanotube by coal dust and other carbonaceous materials, outstanding feature of the present invention is that the output rating of plasma generator is big, can reach MW class.And when producing carbon nano-tube material, can produce industrial chemicals such as acetylene.
Utilize high power plasma generator to prepare the method for carbon nanotube, it is characterized in that included following steps: logical working gas hydrogen in plasma generator, nitrogen or argon gas, start the power supply of plasma generator, hydrogen gas ionizes becomes hydrogen plasma, form the plasma jet of 1800K～15000K, with hydrogen coal dust is quickened to be transported in the pyritous plasma jet to react, the particle diameter of used coal dust is no more than 120 microns, reaction time is 10～40ms, the mixing zone of plasma jet and coal dust and below inwall on form carbon nanotube.
The pressure of coal dust and plasma jet mixing zone is 0.02～0.09MPa in the described plasma generator.
The confession powder speed of coal dust is 5Kg/cm
2H～20Kg/cm
2H, hydrogen flowing quantity are 200～800m
3/ h, the output rating of plasma generator can be regulated, and regulation range is between 200KW～2MW.
Described coal dust substitutes with other carbonaceous material.
The present invention can be by multilayer coal feeding pipe pulverized coal conveying respectively, coal dust is transported in the high temperature of plasma jet to react.
The technological process of preparation carbon nanotube is as follows: logical working gas hydrogen, nitrogen or argon gas in plasma generator, and the power supply of startup plasma generator, hydrogen gas ionizes becomes hydrogen plasma, forms the plasma jet of 1800K～15000K.With hydrogen coal dust is quickened to be transported in the pyritous plasma jet, the confession powder speed of coal dust is 5Kg/cm
2H～20Kg/cm
2H, hydrogen flowing quantity are 200～800m
3/ h, the output rating of regulating plasma generator is between 200KW～2MW, and the particle diameter of used coal dust is under 120 microns, and the working pressure of plasma reactor is 0.02～0.09MPa, and the residence time of reaction is 10～40ms.On the mixing section copper inwall of the mixing zone of plasma jet and coal dust, form carbon nanotube, on reactor siliconize graphite inwall, also form carbon nanotube.
The present invention is the catalyzer of added metal or nonmetallic compound not, only utilizes high temperature of plasma body and chemically reactive to prepare carbon nanotube.
The output rating of used plasma generator can be regulated, and can reach 2 megawatts.The plasma body core temperature that produces is about 15000K, and the medial temperature of whole plasma jet is 3000K～6000K, is the effectively instrument of gasification of carbonaceous material.
Outstanding advantage of the present invention is:
1, the output rating of plasma generator can be regulated between 200KW～2MW continuously, and the working gas of plasma generator is hydrogen, argon gas, nitrogen or its gaseous mixture.The power of plasma generator and the kind and the flow of working gas be can regulate as required and carbon nanotube and acetylene produced.
2, can prepare the carbon nanotube of variform in the primary first-order equation.
3, do carrier gas with hydrogen the coal dust of pulverizing is transported in the hydrogen plasma jet, in the pyritous plasma jet, fugitive constituent volatilizees rapidly in the coal dust, thereby and with plasma jet complicated chemical reaction takes place and can prepare carbon nanotube.
Description of drawings
Fig. 1 is the device synoptic diagram that high power plasma generator of the present invention prepares the method and the technology of carbon nanotube.
Fig. 2 is plasma jet and coal dust mixing section and structure of reactor synoptic diagram.
Fig. 3, Fig. 6 are the photos that utilizes the prepared carbon nanotube of the present invention that transmission electron microscope is taken.
Fig. 4, Fig. 5, Fig. 7 are the photos that utilizes the prepared carbon nanotube of the present invention that scanning electronic microscope is taken.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.
The major equipment of realizing the preparation of carbon nanotube is: coal supply powder system 1, power supply and airing system 2, plasma generator 3, plasma jet and coal dust mixing section 4, reactor 5, quencher 6, solid-liquid separator 7, gas-liquid separator 8, water seal spark arrester 9, exhaust gas processing device 10.Description of equipment is as follows: plasma generator 3 is a V-type, and the coal powder entrance of coal supply powder system 1 is plasma generator 3 times.The plasma jet high speed that plasma generator 3 produces enters plasma jet and coal dust mixing section 4, quickens coal dust with hydrogen, and it is ejected in the plasma jet, and both are thorough mixing in plasma jet and coal dust mixing section 4.Reactor 5 is plasma jet and coal dust mixing section 4 times, and reactor is a tubular reactor, and internal diameter is 90mm, and length is 1000mm.Reactor is for 5 times a quencher 6, the high temperature material that produces through the high pressure water quenching enter into solid-liquid separator 7 successively, gas-liquid separator 8 separates, solid product is purified and can be got the part carbon nanotube, gas enters in the exhaust treatment system 10 through water seal spark arrester 9, and necessity is to light discharging through torch.
Operation steps is as follows: at first lead to working gas hydrogen, nitrogen or argon gas in plasma generator, start the power supply of plasma generator, hydrogen gas ionizes becomes hydrogen plasma, forms the plasma jet of 1800K～15000K.Then coal dust is quickened to be transported in the pyritous plasma jet with hydrogen, the output rating of re-adjustment plasma generator is between 200KW～2MW, keeping the working pressure of plasma reactor is 0.02～0.09Mpa, and the residence time of reaction is 10～40ms.On the mixing section copper inwall of plasma jet and coal dust, form carbon nanotube, on reactor siliconize graphite inwall, also form carbon nanotube.Part carbon nanotube and reaction residue mix, and carry out aftertreatment and just can isolate carbon nanotube.
Embodiment 1
With the Xinjiang long-flame coal is raw material, and the median size of coal dust is about 120 microns.Adopt the hydrogen plasma jet, the power of plasma generator is 1.8MW, and the confession powder speed of coal dust is 6Kg/cm
2H, hydrogen flowing quantity are 340m
3/ h reacted after 20 minutes, had found to have a large amount of carbon nanotubes to be deposited on (see figure 3) on the mixing section copper inwall of plasma jet and coal dust by the captured photo of scanning electronic microscope.
With Huainan bituminous coal is raw material, and the median size of coal dust is about 120 microns.Adopt the hydrogen plasma jet, the power of plasma generator is 1.6MW, and the confession powder speed of coal dust is 5Kg/cm
2H, hydrogen flowing quantity are 300m
3/ h reacted after 40 minutes, had found to have the carbon nanotube that comes in every shape to be deposited on (see figure 4) on the reactor siliconize graphite inwall by the captured photo of transmission electron microscope.
With the Xinjiang long-flame coal is raw material, and the median size of coal dust is about 120 microns.Adopt the hydrogen plasma jet, the power of plasma generator is 2.0MW, and coal feeding pipe is divided into multilayer pulverized coal conveying respectively, is example with two-layer coal supply.For powder speed is 20Kg/cm
2H, hydrogen flowing quantity are 560m
3/ h reacted after 55 minutes, had found to have a large amount of carbon nanotubes to be deposited on (see figure 5) on the mixing section copper inwall of plasma jet and coal dust and the reactor siliconize graphite inwall by the captured photo of scanning electronic microscope.
With the Xinjiang long-flame coal is raw material, and the median size of coal dust is about 120 microns.Adopt the nitrogen plasma jet, the power of plasma generator is 1.6MW, is 5.5Kg/cm for powder speed
2H, nitrogen flow are 280m
3/ h reacted after 70 minutes, had found that by the captured photo of transmission electron microscope carbon nanotube is deposited on (see figure 6) on the mixing section copper inwall of plasma jet and coal dust.
Embodiment 5
With Huainan bituminous coal is raw material, and the median size of coal dust is about 120 microns.Adopt the hydrogen plasma jet, the power of plasma generator is 0.90MW, and coal feeding pipe is divided into two-layer up and down pulverized coal conveying respectively, is 5Kg/cm for powder speed
2H, hydrogen flowing quantity are 160m
3/ h reacted after 30 minutes, had found to have the carbon nanotube that comes in every shape to be deposited on (see figure 7) on the reactor siliconize graphite inwall by the captured photo of scanning electronic microscope.
Claims (6)
1, utilize high power plasma generator to prepare the method for carbon nanotube, it is characterized in that may further comprise the steps: logical working gas hydrogen in plasma generator, nitrogen or argon gas, start the power supply of plasma generator, hydrogen gas ionizes becomes hydrogen plasma, form the plasma jet of 1800K-15000K, with hydrogen coal dust is quickened to be transported in the pyritous plasma jet to react, the particle diameter of used coal dust is no more than 120 microns, reaction time is 10-40ms, the mixing zone of plasma jet and coal dust and below inwall on form carbon nanotube; The output rating of plasma generator can be regulated, and regulation range is between 200KW-2MW.
2, method according to claim 1 is characterized in that the pressure of coal dust and plasma jet mixing zone is 0.02-0.09MPa in the described plasma generator.
3, method according to claim 1 is characterized in that described plasma body core temperature is about 15000K, and the medial temperature of whole plasma jet is 3000K-6000K.
4, method according to claim 1, what it is characterized in that coal dust is 5Kg/cm for powder speed
2H-20Kg/cm
2H, hydrogen flowing quantity are 200-800m
3/ h.
5, method according to claim 1 is characterized in that described coal dust substitutes with other carbonaceous material.
6, method according to claim 1 is characterized in that by multilayer coal feeding pipe pulverized coal conveying respectively, coal dust is transported in the high temperature of plasma jet to react.
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| CN100484869C true CN100484869C (en) | 2009-05-06 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447076C (en) * | 2007-04-20 | 2008-12-31 | 北京交通大学 | Method of preparing multi-wall carbon nano-tube from coal |
| JP5660804B2 (en) * | 2010-04-30 | 2015-01-28 | 東京エレクトロン株式会社 | Carbon nanotube formation method and carbon nanotube film forming apparatus |
| US20130192979A1 (en) * | 2011-01-17 | 2013-08-01 | Greenville Envirotech Co Ltd | Apparatus for plasmatizing solid-fuel combustion additive and method for using the same |
| CN103022514B (en) * | 2012-12-06 | 2016-04-06 | 中国科学院等离子体物理研究所 | A kind of preparation method of high density herring-bone form carbon nano-carrier |
| CN103843822B (en) * | 2014-03-21 | 2016-03-30 | 西安科技大学 | A kind of preparation method of CNT silver composite antibacterial material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328958A (en) * | 2001-07-22 | 2002-01-02 | 太原理工大学 | Preparation of carbon nanometer pipe material and its equipment |
| CN1398781A (en) * | 2002-08-30 | 2003-02-26 | 太原理工大学 | Acetylene and carbon nanotube preparing plant |
| EP1414744A1 (en) * | 2001-07-27 | 2004-05-06 | University Of Surrey | Production of carbon nanotubes |
| WO2004039723A1 (en) * | 2002-10-30 | 2004-05-13 | Fuji Xerox Co., Ltd. | Production system and production method of carbon nanotube |
| CN1541938A (en) * | 2003-11-06 | 2004-11-03 | 大连理工大学 | Method and apparatus for continuous preparation of carbon nanometer tube material from coal |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328958A (en) * | 2001-07-22 | 2002-01-02 | 太原理工大学 | Preparation of carbon nanometer pipe material and its equipment |
| EP1414744A1 (en) * | 2001-07-27 | 2004-05-06 | University Of Surrey | Production of carbon nanotubes |
| CN1398781A (en) * | 2002-08-30 | 2003-02-26 | 太原理工大学 | Acetylene and carbon nanotube preparing plant |
| WO2004039723A1 (en) * | 2002-10-30 | 2004-05-13 | Fuji Xerox Co., Ltd. | Production system and production method of carbon nanotube |
| CN1541938A (en) * | 2003-11-06 | 2004-11-03 | 大连理工大学 | Method and apparatus for continuous preparation of carbon nanometer tube material from coal |
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