CN102115075A - Prismoid type flame combustor and synthesis method of carbon nanotube thereof - Google Patents
Prismoid type flame combustor and synthesis method of carbon nanotube thereof Download PDFInfo
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- CN102115075A CN102115075A CN 201110021510 CN201110021510A CN102115075A CN 102115075 A CN102115075 A CN 102115075A CN 201110021510 CN201110021510 CN 201110021510 CN 201110021510 A CN201110021510 A CN 201110021510A CN 102115075 A CN102115075 A CN 102115075A
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Abstract
The invention discloses a prismoid type flame combustor and a synthesis method of a carbon nanotube thereof, belonging to the technical field of a carbon nanotube. The combustor consists of a synthesis region, a pyrolytic reaction region, a combustion tube, a premixing room and a center premixing room; a stable flame surface is formed by the combustion of the combustible gas at two sides of the combustor to pack the pyrolytic reaction region and the synthesis region so as to offer a high-temperature heat source; reaction mixture, metal catalyst nanoparticle and inert gas of the center premixing room can be used for offering a carbon source and a catalyst; and the pyrolytic reaction region is heated to be decomposed into carbon atoms and metal catalyst atoms, the carbon atoms are gradually aggregated into carbon atom clusters when the carbon atoms upwards flow, the metal catalyst atoms are gradually grown into catalyst particles when the metal catalyst atoms upwards flow, and the carbon atoms clusters and the catalyst particles reach the synthesis region to be synthesized into the carbon nanotube. After the method is used, the pyrolysis process of the carbon-containing chemical compound is separated from the synthesis process of the carbon nanotube, so that the carbon nanotube can be prepared under a controllable way, continuously, in bulk, on a large scale, and at a low cost.
Description
Technical field
The invention belongs to the carbon nanotube synthesis technical field, be specifically related to the method for a kind of prismoid shaped flame burner and synthesizing carbon nanotubes thereof.
Background technology
(Carbon Nanotubes is a kind of novel one-dimensional carbon nano material CNTs) to carbon nanotube, is to be found during at the observation transmission electron microscope in 1991 by the Iijima doctor of Japan.Because features such as its unique graphite-structure, high surperficial ratio and minor diameters, attracted a large amount of investigators to be devoted to the research of aspects such as its structure, synthetic, application.Potential is used and is comprised nanoelectronic equipment, probe, inductor block, absorption agent, catalysis, matrix material toughener etc.The synthetic method of carbon current nanotube mainly contains arc discharge method (arc discharge), laser evaporation method (laser vaporization) and chemical Vapor deposition process (chemical vapor deposition, CVD), these methods all are mature methods, and scholar's brainstrust of being engaged in these method researchs has obtained the carbon nanotube of better performances.But these methods comprise its improvement or epitaxy method and are subject to cost high or discontinuous being combined in batches mostly.Realize low-cost, equipment is simple, processing ease, preparation continuously, commercialization is synthetic is pursuing one's goal of present nearly all carbon nanotube study on the synthesis person.Flame synthesis method (flame synthesis) does not need special environment, in normal atmosphere, just can carry out, and flame method equipment simple, easy to operate, can realize continuously syntheticly, have the potentiality that large-scale commercial applications is combined to.The representational research of flame method synthesizing carbon nanotubes at present mainly contains:
The people such as Liming Yuan of Kentucky, United States university " Liming Yuan; Kozo Saito; Chunxu Pan; et al.Nanotubes from methane flames[J] .Chemical Physics Letters; 2001, V340 (3-4): 237-241 " what adopt is the laminar flow diffusion flame synthesizing multi-wall carbon nanotube of big pipe box tubule.Diameter be effusive in the stainless steel tube tubule of 11mm be methane and assist gas, tubule and diameter are that what carry between the bassoon of 50mm is air, metals such as cadmium, nickel, iron are attached to makes catalyzer on the sample probe.
The Vander of NASA wal etc. document " Vander wal RL.Fe-catalyzed single-walled carbon nanotubes synthesis within a flame environment[J] .Combustion and Flame; 2002, V130 (1-2): 37-47 " in adopt McKenna burner synthesizing carbon nanotubes.The annular burner of external diameter 50mm, outer shroud are set up rich fuel premix flat flame as thermal source, and middle 11mm diameter pipe core outlet is concordant with the outer shroud outlet, and the reaction gas mixtures of the logical containing metal catalyzer of pipe core adds thinner and reduces temperature.Be arranged vertically a diameter 25mm thin-wall circular tube as stable cover near the burner top, utilize the thief carbon pin to collect Single Walled Carbon Nanotube in stable cover outlet.
3. Japan's celebrating answers the people " Shunpei Nakazawa; Takeshi Yokomori; Masahiko Mizomoto.Flame synthesis of carbon nanotubes in a wall stagnation flow.Chemical physics letters; 2005, V403 (1-3): 158-162 " such as Shunpei Nakazawa of university of private school charging no tuition to adopt in allocating the synthetic of plate burner research multi-walled carbon nano-tubes.Ethene, air and nitrogen mix in the stainless steel tube burner of a long 1000mm, internal diameter 10mm, and at the jet combustion of pipe end, ethene provides the carbon source and the thermal source of synthesizing carbon nanotubes.Apart from pipe end burner noz(zle) 8mm place is that a diameter 76mm allocates plate with staying of catalyzer nickel, and carbon nanotube is generating in allocating the plate surface.What this mode was burnt formation is premixed flame, but because whole burning is all leaked in atmosphere cruelly, therefore the outside of premixed flame has the composition of diffusion flame simultaneously, this is bell mouth shape with regard to having caused the carbon content in the flame, oxygen content is lower in the middle of allocating plate simultaneously, outside oxygen oxygen level is higher, obtains multi-walled carbon nano-tubes on the suitable endless belt of combustion oxygen ratio.
4. Korea S becomes the people " Sang Kil Woo; Young Taek Hong; Oh Chae Kwon.Flame synthesis of carbon nanotubes using a double-faced wall stagnation flow burner.Carbon; 2009,47 (3): 912-916 " such as Sang Kil Woo of equal shop university to adopt two-sided staying to allocate plate burner synthesizing carbon nanotubes.Burner allocates plate and two nozzle (internal diameter 3mm up and down thereof by staying of applying of nickel, length-to-diameter ratio is 100) form, the mixture of ethene, air and nitrogen is from two nozzle ejection burnings up and down and impact and stay the upper and lower surface that allocates plate, stays to allocate to obtain carbon nanotube on the plate.
The people such as Yu Xiaoli of Tsing-Hua University " Yu Xiaoli; Yang Xiaoyong, Ye Ping is etc. the experimental study [J] of acetylene air pre-mixing flame method synthesizing multi-wall carbon nanotube. Engineering Thermophysics journal; 2009,30 (1): 165-168 " adopt acetylene air pre-mixing flame synthesizing multi-wall carbon nanotube.Burner is made up of two different concentric pipes of diameter.Pipe feeds acetylene and air pre-mixing gas in the stainless steel, lights in the exit to form the laminar flow premixed flame, and outer tube is made up of metal tube and plexiglass tent two portions, bubbling air or shielding gas nitrogen.Utilize the probe that applies nickelous nitrate or ferrocene catalyzer to obtain carbon nanotube in the sampling of flame different heights.
Up to the present, in the whole bag of tricks with the flame method synthesizing carbon nanotubes, if expect that a large amount of output must have time enough, efficient is lower, simultaneously of long duration only can obtain multi-walled carbon nano-tubes and can not get Single Walled Carbon Nanotube.Existing flame method do not reach ideal a large amount of, continuously, can operate, extensive synthesizing carbon nanotubes.
Summary of the invention
The object of the present invention is to provide a kind of prismoid shaped flame burner.
The present invention also aims to provide a kind of method of prismoid shaped flame burner synthesizing carbon nanotubes.
A kind of prismoid shaped flame burner is characterized in that, described burner is made up of synthetic district 1, pyrolysis reaction region 2, incendiary pencil 3, premixer 4, premixer, center 5; Synthetic district 1 is positioned at pyrolysis reaction region 2 tops, both ends open; Synthetic district 1 and pyrolysis reaction region 2 are joined with premixer, center 5; Premixer 4 links to each other with incendiary pencil 3.
Described synthetic district 1 and pyrolysis reaction region 2 are down the prismoid shaped structure that end cross-sectional area is big, upper end cross sectional is little.
A kind of method of prismoid shaped flame burner synthesizing carbon nanotubes is characterized in that, may further comprise the steps:
Inflammable gas and ignition dope at the premixer of both sides 4 premixs, are derived by incendiary pencil 3, and igniting makes gas fuel burning, forms stable flame front, with pyrolysis reaction region 2 with syntheticly distinguish 1 and wrap, provides synthesizing carbon nanotubes necessary thermal source;
With 5 mixing of reaction mixture, metal-catalyst nanoparticles and rare gas element in the premixer, center, enter pyrolysis reaction region 2 and synthetic district 1 then, reaction mixture provides synthesizing carbon nanotubes necessary carbon source, metal-catalyst nanoparticles provides synthesizing carbon nanotubes necessary catalyzer, makes pyrolysis reaction region 2 and synthetic district 1 possess the necessary three elements of synthesizing carbon nanotubes;
Described inflammable gas is the liquid fuel of geseous fuel, atomizing or the solid particulate that is carried by air, and described ignition dope is an air or oxygen.
Described reaction mixture is the mixture of carbon monoxide and hydrogen, perhaps one or more components in the carbonaceous liquid of acetylene, ethene, atomizing and the mixture of hydrogen.
Described metal-catalyst nanoparticles is the compound or the simple substance of iron content, cobalt, nickel, molybdenum and aluminium.
Described rare gas element is nitrogen, helium or argon gas.
The volume ratio that described inflammable gas and ignition dope feed is 1-2.2, and flow is 0.05-0.2L/s; By the volume ratio of adjustment inflammable gas and ignition dope and the variation of flow realization pyrolysis temperature and synthesis temperature; Volume by adjusting distance between incendiary pencil 3 and the synthetic district 1 and inflammable gas and ignition dope when flow can realize the temperature-resistant temperature that only changes pyrolysis reaction region 2 in synthetic district 1 or pyrolysis reaction region 2 temperature-resistant only change to synthesize distinguish 1 temperature.
Beneficial effect of the present invention: can adopt the structure serial sampling of similar travelling belt, therefore can accomplish that continuous batch is synthetic, the pyrolysis flame and the synthetic separately control of carbon nanotube that will participate in the carbon nanotube generation simultaneously can realize controlled, extensive, the low-cost carbon nanotube for preparing; Adopt the structure that following end cross-sectional area is big, upper end cross sectional is little of prismoid shaped to participate in that combustiblecomponents fully burns in the carbon nanotube synthetic reaction mixture in the middle of can avoiding; Can realize carrying out pyrolysis and synthesizing under the temperature condition of the best of carbon nanotube of carbon source by the distance of adjusting between incendiary pencil 3 and the synthetic district 1 in addition.
Description of drawings
Fig. 1 is a prismoid shaped pyrolysis flame burner synoptic diagram;
Wherein, the synthetic district of 1-, 2-pyrolysis reaction region, 3-incendiary pencil, 4-premixer, premixer, 5-center.
Embodiment
The present invention will be further described below in conjunction with the drawings and specific embodiments:
Embodiment 1
Figure 1 shows that present embodiment prismoid shaped pyrolysis flame burner synoptic diagram, form by synthetic district 1, pyrolysis reaction region 2, incendiary pencil 3, premixer 4, premixer, center 5; Synthetic district 1 is positioned at pyrolysis reaction region 2 tops; Synthetic district 1 and pyrolysis reaction region 2 are joined with premixer, center 5; Premixer 4 links to each other with incendiary pencil 3; Synthetic district 1 and pyrolysis reaction region 2 are down the prismoid shaped structure that end cross-sectional area is big, upper end cross sectional is little; Synthetic district 1 is a both ends open, is convenient to the sample probe sampling; Premixer's 5 logical reaction mixture, metal-catalyst nanoparticles and rare gas elementes; The mixture of incendiary pencil 3 logical inflammable gass and ignition dope.
The concrete steps of prismoid shaped flame method synthesizing carbon nanotubes are:
With acetylene and air in the premixer 4 premixs, at the stable flame of the end burning formation of incendiary pencil 3 pyrolysis reaction region 2 and synthetic district 1 are encased then, derive by incendiary pencil 3, igniting makes gas fuel burning, form stable flame front, pyrolysis reaction region 2 and synthetic district 1 are wrapped, provide synthesizing carbon nanotubes necessary thermal source; The volume ratio of acetylene and air and flow mainly influence the temperature of pyrolysis flame, and selecting the volume ratio of acetylene and air according to the pyrolysis temperature (600 ℃～1300 ℃) of synthesizing carbon nanotubes needs is 1-2.2, and flow is 0.05-0.2L/s.
With carbon monoxide (or acetylene, ethene, the carbonaceous liquid of atomizing) with the mixture of hydrogen, iron (or cobalt, nickel, molybdenum, aluminium) catalyst nano particle and argon gas (or helium, nitrogen) being mixed in chamber 5 in advance at the center mixes, enter pyrolysis reaction region 2 and synthetic district 1 then, carbon monoxide (or acetylene, ethene, the carbonaceous liquid of atomizing) provide synthesizing carbon nanotubes necessary carbon source, iron (or cobalt, nickel, molybdenum, aluminium) provide synthesizing carbon nanotubes necessary catalyzer, so pyrolysis reaction region 2 and synthetic district 1 have possessed the necessary three elements of synthesizing carbon nanotubes, can synthesizing carbon nanotubes.
The prismoid shaped flame method of present embodiment the carbon compound that thermal source and carbon source are provided separately also will participate in simultaneously the pyrolysis of the carbon compound that carbon nanotube generates and the building-up process of carbon nanotube and separate.Reaction mixture can be the mixture of carbon monoxide (carbonaceous liquid of hydrocarbon polymer such as acetylene, ethene or atomizing) and hydrogen, and carbon monoxide is separated out carbon by hydrogenization carbon source is provided; The catalyst nano particle can be the compound or the simple substance of iron content, cobalt, nickel, molybdenum, aluminium, introduces by the method that atomizes, sprays into or apply; Rare gas element can be argon gas, helium, nitrogen.To adopting iron is the situation of catalyzer, and reactivity ratio's acetylene of carbon monoxide is much better than, and carbon monoxide can cause the fragmentation of macrobead iron, and reaction surface is increased, and the iron particle promotes that carbon monoxide at high temperature decomposes simultaneously.Hydrogen Energy promotes dissociative carbon to be absorbed by the iron particle, promotes the growth of carbon nanotube, and hydrogen can clean the carbon atom bunch that accumulates in carbon nano tube surface in addition, can also the deactivated catalyst particle, keep activity of such catalysts.Rare gas element is as thinner, but attemperation reaches carbon nanotube synthetic temperature range (600 ℃～1300 ℃); Rare gas element also can clean the carbon atom bunch and the granules of catalyst of carbon nano tube surface, plays the effect of smooth carbon nanotube; Work to keep catalyst activity in addition.The introducing of metal catalyst adopts the effect of atomizing better, liquid catalyst or the solid catalyst atomizing of dissolving in liquid can be less, the uniform small droplets of particle diameter by atomizing, the grain diameter that generates after the pyrolysis at high temperature of these small dropletss further reduces, and it is synthetic to be more suitable for carbon nanotube.
Claims (8)
1. a prismoid shaped flame burner is characterized in that, described burner is made up of synthetic district (1), pyrolysis reaction region (2), incendiary pencil (3), premixer (4), premixer, center (5); Synthetic district (1) is positioned at pyrolysis reaction region (2) top, both ends open; Synthetic district (1) and pyrolysis reaction region (2) are joined with premixer, center (5); Premixer (4) links to each other with incendiary pencil (3).
2. according to the described a kind of prismoid shaped flame burner of claim 1, it is characterized in that described synthetic district (1) and pyrolysis reaction region (2) are down the prismoid shaped structure that end cross-sectional area is big, upper end cross sectional is little.
3. the method for a prismoid shaped flame burner synthesizing carbon nanotubes is characterized in that, may further comprise the steps:
With inflammable gas and ignition dope at the premixer (4) of both sides premix, derive by incendiary pencil (3), igniting makes gas fuel burning, forms stable flame front, pyrolysis reaction region (2) and synthetic district (1) are wrapped, provide synthesizing carbon nanotubes necessary thermal source;
Reaction mixture, metal-catalyst nanoparticles and rare gas element are mixed in premixer, center (5), enter pyrolysis reaction region (2) and synthetic district (1) then, reaction mixture provides synthesizing carbon nanotubes necessary carbon source, metal-catalyst nanoparticles provides synthesizing carbon nanotubes necessary catalyzer, makes pyrolysis reaction region (2) and synthetic district (1) possess the necessary three elements of synthesizing carbon nanotubes;
Pyrolysis reaction region (2) decomposes generates carbon atom and metal catalyst atoms, carbon atom is gathered into carbon atom bunch gradually in process of flowing upwards, metal catalyst atoms is upwards growing up to metal catalyst particles in the process of flowing gradually, and carbon atom bunch and metal catalyst particles arrive back, synthetic district (1) synthesizing carbon nanotubes.
4. according to the method for the described a kind of prismoid shaped flame burner synthesizing carbon nanotubes of claim 3, it is characterized in that described inflammable gas is the liquid fuel of geseous fuel, atomizing or the solid particulate that is carried by air, described ignition dope is an air or oxygen.
5. according to the method for the described a kind of prismoid shaped flame burner synthesizing carbon nanotubes of claim 3, it is characterized in that, described reaction mixture is the mixture of carbon monoxide and hydrogen, perhaps one or more components in the carbonaceous liquid of acetylene, ethene, atomizing and the mixture of hydrogen.
6. according to the method for the described a kind of prismoid shaped flame burner synthesizing carbon nanotubes of claim 3, it is characterized in that described metal-catalyst nanoparticles is the compound or the simple substance of iron content, cobalt, nickel, molybdenum and aluminium.
7. according to the method for the described a kind of prismoid shaped flame burner synthesizing carbon nanotubes of claim 3, it is characterized in that described rare gas element is nitrogen, helium or argon gas.
8. according to the method for the described a kind of prismoid shaped flame burner synthesizing carbon nanotubes of claim 3, it is characterized in that the volume ratio that described inflammable gas and ignition dope feed is 1-2.2, flow is 0.05-0.2L/s; By the volume ratio of adjustment inflammable gas and ignition dope and the variation of flow realization pyrolysis temperature and synthesis temperature; Volume by adjusting distance between incendiary pencil (3) and the synthetic district (1) and inflammable gas and ignition dope when flow can realize that temperature-resistant temperature or temperature-resistant only change of pyrolysis reaction region (2) that only changes pyrolysis reaction region (2) in synthetic district (1) synthesize temperature of distinguishing (1).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10087077B2 (en) * | 2013-09-17 | 2018-10-02 | Fgv Cambridge Nanosystems Limited | Method, system and injection subsystem for producing nanotubes |
| CN108892122B (en) * | 2018-08-31 | 2020-10-27 | 北京化工大学 | Method for preparing carbon nano tube by solution combustion |
| CN115744877A (en) * | 2022-10-24 | 2023-03-07 | 国家能源集团新能源技术研究院有限公司 | Preparation device of carbon nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1830770A (en) * | 2006-04-21 | 2006-09-13 | 华北电力大学（北京） | Burner for synthesizing nanometer carbon pipe by V type and conical type pyrolytic flame and its synthesizing method |
| CN201952234U (en) * | 2011-01-19 | 2011-08-31 | 华北电力大学 | Truncated pyramid type flame burner |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830770A (en) * | 2006-04-21 | 2006-09-13 | 华北电力大学（北京） | Burner for synthesizing nanometer carbon pipe by V type and conical type pyrolytic flame and its synthesizing method |
| CN201952234U (en) * | 2011-01-19 | 2011-08-31 | 华北电力大学 | Truncated pyramid type flame burner |
Non-Patent Citations (1)
| Title |
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| 《人工晶体学报》 20100831 孙保民等 五羰基铁催化热解合成碳纳米管 936-940 1-8 第39卷, 第4期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10087077B2 (en) * | 2013-09-17 | 2018-10-02 | Fgv Cambridge Nanosystems Limited | Method, system and injection subsystem for producing nanotubes |
| CN108892122B (en) * | 2018-08-31 | 2020-10-27 | 北京化工大学 | Method for preparing carbon nano tube by solution combustion |
| CN115744877A (en) * | 2022-10-24 | 2023-03-07 | 国家能源集团新能源技术研究院有限公司 | Preparation device of carbon nano material |
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Application publication date: 20110706 |