CN1547225A - Technology and equipment for preparing magnetic carbon nanometer tube by plasma - Google Patents
Technology and equipment for preparing magnetic carbon nanometer tube by plasma Download PDFInfo
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- CN1547225A CN1547225A CNA2003101097010A CN200310109701A CN1547225A CN 1547225 A CN1547225 A CN 1547225A CN A2003101097010 A CNA2003101097010 A CN A2003101097010A CN 200310109701 A CN200310109701 A CN 200310109701A CN 1547225 A CN1547225 A CN 1547225A
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Abstract
The invention is a technology for using plasma to produce the magnetic carbon nano pipe. The argon is blown into the plasma generator, there forms the plasma efflux under the effect of the current; the methane is blended with the plasma in condition without oxygen, it is ionized and decomposed into nano grade active carbon particles, and enters the reactor whose magnetism intensity if 70-200G, and uses the nickel sieve carrying load iron powder or ferric oxide powder to generate the magnetic carbon nano pipe. The structure is simple, the device is cheap, and it can avoid the structure deficiencies.
Description
Technical field:
The invention belongs to a kind of technology for preparing carbon nano-tube, relate in particular to a kind of technology and device for preparing magnetic carbon nano-tube with plasma.
Background technology:
At present, the preparation method to carbon nano-tube is a lot of in the world, such as: ion or laser splash method, pyrolyzed-polymer method, solid-phase pyrolysis etc. also have the solar energy that utilizes of up-to-date report to prepare the method for carbon pipe.But ripe relatively at present process chemistry vapour deposition process, the tubular structure proportion of products is not high in the thick product of the carbon nano-tube of this prepared, and caliber is irregular, has more crystal defect.People also utilize DC arc plasma method to prepare carbon nano-tube (as " Massproduction of single-wall carbon nanotubes by the arc plasma jetmethod " Chem.Phys.Lett.323 (2000) 580-585) simultaneously, obtain containing the deposit of carbon nano-tube on negative electrode.But because the arc temperature height, the CNT (carbon nano-tube) that is produced is sintered into one, causes more defective.And its adopts graphite rod as electrode, will constantly regulate distance between electrodes in experimentation, has hindered the stable of reaction system and has carried out.
Summary of the invention:
The objective of the invention is to utilize a kind of practicality of feature development, inexpensive of plasma, the technology of the magnetic carbon nano-tube that yield is high and device.
The object of the present invention is achieved like this:
(1) cooling water, argon gas being fed plasma generator, is 70-90A at electric current, and power is 3.5-5.0kW, and operating pressure is under the atmospheric condition, and plasma generator makes the gas continuous discharge form plasma jet;
(2) give and to feed methane in the plasma generator, it is mixed and be ionized being decomposed into nano level active charcoal particle under oxygen-free environment with the high-temperature plasma jet, the feeding amount of methane is 15-30 with the ratio of the volume of argon gas: 1;
(3) the nano level active charcoal that resolves into enters the reactor that magnetic field intensity is 70-200 G, and the nickel system screen cloth by load iron powder or di-iron trioxide powder, generates magnetic carbon nano-tube, and wherein the mass ratio of nickel and iron is 2-5: 1.
In order to reach the foregoing invention purpose, designed the plasma generator isolated plant, it is to connect by insulating flange between negative electrode and the anode; Cooling water pipe and hydrocarbon feed ingress pipe link to each other with anode with welding manner.Be to be threaded between water collar and anode, the reactor, install magnetic coil additional around the reactor, inside adds puts screen cloth, argon gas inlet and anode welding.
The present invention compared with prior art has following advantage:
Plasma provides high enthalpy thermal source and active particle source, catalyst in flow regime easily and the hydrocarbon cracking product fully mix, help the growth of carbon pipe.Externally-applied magnetic field has the effect of stable arc, prevents too early knot charcoal.Make the nanometer iron in the product have suitable magnetic simultaneously.The hydrogen that generates can be used as fuel and uses, and entire reaction can be carried out and the technical process environmental friendliness no NO under normal pressure
x, CO
xDischarging.
1. because the carbon nano-tube itself of not purifying contains catalyst granules, and this catalyst is some nano level magnetic inorganic particles, existing good wave absorbtion has the good absorption ultrared performance that dissipates again.
2. accessory substance hydrogen promptly can act as a fuel and reclaim, and it also provides the reducing atmosphere of reaction system necessity really simultaneously.
3. compare the method that other prepare carbon nano-tube, the equipment cheapness, and avoid fault of construction.
Embodiment:
Fig. 1 is the structural representation of plasma reactor of the present invention
As shown in the figure: connect by insulating flange 3 between negative electrode 1 and the anode 4; Cooling water pipe 2 and hydrocarbon feed ingress pipe 8 link to each other with anode 4 with welding manner.Between water collar 7 and anode 4, the reactor 9 is to be threaded.Install magnetic coil 10 additional around the reactor 9, inside adds puts screen cloth 11.Argon gas inlet 12 and anode 4 welding.
Embodiment 1
At first the cooling water pipe 2 of cooling water from the plasma reactor top fed, the cooling jacket 7 of flowing through is discharged from the cooling water pipe 2 of plasma reactor lower end at last.Argon gas is introduced plasma reactor from inlet tube 12.Reactor 9 outer additional magnetic coils 10, its magnetic field intensity remains 70G.Opening power is regulated electric current to 70A, and discharge will feed the argon gas puncture of plasma reactor between negative electrode 1 and the anode 4, produce plasma jet.Plasma jet was tied and was extended in the reactor 9 after ceramic ring 5 is retrained by discharge channel 6.Methane is introduced reactor 9 from hydrocarbon feed ingress pipe 8, and the volume ratio of argon gas and methane feeds in 16: 1 ratio.Under the oxygen-free environment of methane in reactor 9 with reactor 9 in plasma jet fully contact, be ionized and generate nano active charcoal particle.Active carbon wherein is attached to the nickel system screen cloth 11 in the reactor 9, and reacts with iron powder on the screen cloth, and the mass ratio of nickel and iron is 5: 1.Grow carbon nano-tube at catalyst surface at last.Power work stops reaction after 20 minutes.Finish back gas chromatographic analysis product gas component, and collect the solid product carbon nano-tube, with transmission electron microscope observing granular size and shape, its surface topography of scanning electron microscopic observation, its result is written in the table 1 in the lump.
Embodiment 2
Adopt aforementioned manufacturing installation, at first the cooling water pipe 2 of cooling water from the plasma reactor top fed, the cooling jacket 7 of flowing through is discharged from the cooling water pipe 2 of plasma reactor lower end at last.Argon gas is introduced plasma reactor from inlet tube 12.Reactor 9 outer additional magnetic coils 10, its magnetic field intensity remains 100G.Opening power is regulated electric current to 85A, and discharge will feed the argon gas puncture of plasma reactor between negative electrode 1 and the anode 4, produce plasma jet.Plasma jet was tied and was extended in the reactor 9 after ceramic ring 5 is retrained by discharge channel 6.Methane is introduced reactor 9 from hydrocarbon feed ingress pipe 8, and the volume ratio of argon gas and methane feeds in 25: 1 ratio.Under the oxygen-free environment of methane in reactor with reactor 9 in plasma jet fully contact, be ionized and generate nano active charcoal particle.Active carbon wherein is attached to the nickel system screen cloth 11 in the reactor 9, and reacts with iron powder on the screen cloth, and the mass ratio of nickel and iron is 3: 1.Grow carbon nano-tube at catalyst surface at last.Power work stops reaction after 40 minutes.Finish back gas chromatographic analysis product gas component, and collect the solid product carbon nano-tube, with transmission electron microscope observing granular size and shape, its surface topography of scanning electron microscopic observation, its result is written in the table 1 in the lump.
Embodiment 3
Adopt aforementioned manufacturing installation, at first the cooling water pipe 2 of cooling water from the plasma reactor top fed, the cooling jacket 7 of flowing through is discharged from the cooling water pipe 2 of plasma reactor lower end at last.Argon gas is introduced plasma reactor from inlet tube 12.Reactor 9 outer additional magnetic coils 10, its magnetic field intensity remains 150G.Opening power is regulated electric current to 90A, and discharge will feed the argon gas puncture of plasma reactor between negative electrode 1 and the anode 4, produce plasma jet.Plasma jet was tied and was extended in the reactor 9 after ceramic ring 5 is retrained by discharge channel 6.Methane is introduced reactor 9 from hydrocarbon feed ingress pipe 8, and the volume ratio of argon gas and methane feeds in 30: 1 ratio.Under the oxygen-free environment of methane in reactor with reactor 9 in plasma jet fully contact, be ionized and generate nano active charcoal particle.Active carbon wherein is attached to the nickel system screen cloth 11 in the reactor 9, and reacts with iron powder on the screen cloth, and the mass ratio of nickel and iron is 2: 1.Grow carbon nano-tube at catalyst surface at last.Power work stops reaction after 40 minutes.Finish back gas chromatographic analysis product gas component, isolate hydrogen with transformation absorption (number of patent application 00108935.8), and collect the solid product carbon nano-tube, with transmission electron microscope observing granular size and shape, its surface topography of scanning electron microscopic observation, its result is written in the table 1 in the lump.
Table one
Claims (2)
1. a plasma prepares the technology of magnetic carbon nano-tube, it is characterized in that comprising the steps:
(1) cooling water, argon gas being fed plasma generator, is 70-90A at electric current, and power is 3.5-5.0kW, and operating pressure is under the atmospheric condition, and plasma generator makes the gas continuous discharge form plasma jet;
(2) give and to feed methane in the plasma generator, it is mixed and be ionized being decomposed into nano level active charcoal particle under oxygen-free environment with the high-temperature plasma jet, the feeding amount of methane is 15-30 with the ratio of the volume of argon gas: 1;
(3) the nano level active charcoal that resolves into enters the reactor that magnetic field intensity is 70-200G, and the nickel system screen cloth by load iron powder or di-iron trioxide powder, generates magnetic carbon nano-tube, and wherein the mass ratio of nickel and iron is 2-5: 1.
2. one kind is used for the device that plasma prepares the technology of magnetic carbon nano-tube, it is characterized in that connecting by insulating flange (3) between negative electrode (1) and the anode (4); Cooling water pipe (2) and hydrocarbon feed ingress pipe (8) link to each other with anode (4) with welding manner.Water collar (7) and anode (4), reactor are to be threaded between (9).Reactor (9) installs magnetic coil (10) on every side additional, and inside adds puts screen cloth (11).Argon gas inlet (12) and anode (4) welding.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200310109701 CN1248248C (en) | 2003-12-11 | 2003-12-11 | Technology and equipment for preparing magnetic carbon nanometer tube by plasma |
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| CN 200310109701 CN1248248C (en) | 2003-12-11 | 2003-12-11 | Technology and equipment for preparing magnetic carbon nanometer tube by plasma |
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| CN1547225A true CN1547225A (en) | 2004-11-17 |
| CN1248248C CN1248248C (en) | 2006-03-29 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102548176A (en) * | 2012-01-12 | 2012-07-04 | 北京交通大学 | Discharge electrode and plasma generating device using same |
| CN103200758A (en) * | 2010-10-04 | 2013-07-10 | 衢州市广源生活垃圾液化技术研究所 | Arc plasma device |
| CN103200757B (en) * | 2010-10-04 | 2015-06-24 | 衢州昀睿工业设计有限公司 | Arc plasma torch |
| CN104787749B (en) * | 2015-04-30 | 2016-07-06 | 西安科技大学 | A kind of preparation method of aligned carbon nanotube |
| CN109012059A (en) * | 2018-08-22 | 2018-12-18 | 浙江理工大学 | A kind of preparation method of the Modified Iron dried bean noodles drying prescription based on multilayer carbon nanotube |
| CN112191857A (en) * | 2020-12-04 | 2021-01-08 | 西安欧中材料科技有限公司 | Method for preparing iron-based powder by using high-energy-density plasma rotating electrode |
| CN115057431A (en) * | 2022-06-24 | 2022-09-16 | 中山烯利来设备科技有限公司 | Method for manufacturing carbon nano tube |
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| US9550694B2 (en) | 2014-03-31 | 2017-01-24 | Corning Incorporated | Methods and apparatus for material processing using plasma thermal source |
| US9533909B2 (en) | 2014-03-31 | 2017-01-03 | Corning Incorporated | Methods and apparatus for material processing using atmospheric thermal plasma reactor |
| US20160200618A1 (en) | 2015-01-08 | 2016-07-14 | Corning Incorporated | Method and apparatus for adding thermal energy to a glass melt |
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2003
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103200758A (en) * | 2010-10-04 | 2013-07-10 | 衢州市广源生活垃圾液化技术研究所 | Arc plasma device |
| CN103200758B (en) * | 2010-10-04 | 2015-03-18 | 衢州市广源生活垃圾液化技术研究所 | Arc plasma device |
| CN103200757B (en) * | 2010-10-04 | 2015-06-24 | 衢州昀睿工业设计有限公司 | Arc plasma torch |
| CN102548176A (en) * | 2012-01-12 | 2012-07-04 | 北京交通大学 | Discharge electrode and plasma generating device using same |
| CN104787749B (en) * | 2015-04-30 | 2016-07-06 | 西安科技大学 | A kind of preparation method of aligned carbon nanotube |
| CN109012059A (en) * | 2018-08-22 | 2018-12-18 | 浙江理工大学 | A kind of preparation method of the Modified Iron dried bean noodles drying prescription based on multilayer carbon nanotube |
| CN112191857A (en) * | 2020-12-04 | 2021-01-08 | 西安欧中材料科技有限公司 | Method for preparing iron-based powder by using high-energy-density plasma rotating electrode |
| CN112191857B (en) * | 2020-12-04 | 2021-07-06 | 西安欧中材料科技有限公司 | Method for preparing iron-based powder by using high-energy-density plasma rotating electrode |
| CN115057431A (en) * | 2022-06-24 | 2022-09-16 | 中山烯利来设备科技有限公司 | Method for manufacturing carbon nano tube |
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| Publication number | Publication date |
|---|---|
| CN1248248C (en) | 2006-03-29 |
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