CN105174242A - Vertical reaction furnace for continuous production of carbon nanotubes with preset catalyst - Google Patents
Vertical reaction furnace for continuous production of carbon nanotubes with preset catalyst Download PDFInfo
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- CN105174242A CN105174242A CN201510124301.XA CN201510124301A CN105174242A CN 105174242 A CN105174242 A CN 105174242A CN 201510124301 A CN201510124301 A CN 201510124301A CN 105174242 A CN105174242 A CN 105174242A
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Abstract
The invention relates to a vertical reaction furnace for continuous production of carbon nanotubes with a preset catalyst. The reaction furnace comprises a heating furnace, a reaction chamber, a collecting chamber, a carbon nanotube growth plate, a growth plate support column, a growth plate push rod, and a pneumatic push rod valve, etc. The reaction chamber is located in the heating furnace, and the carbon nanotube growth plate is located at the center of the reaction chamber. The carbon nanotube growth plate and the growth plate support column are in hinged connection, and the growth plate support column is vertically fixed at the center of the collecting chamber base plate. One end of the growth plate motion push rod is in hinged connection with the carbon nanotube growth plate, and the other end is in hinged connection with the pneumatic push rod valve. The reaction furnace provided by the invention can realize continuous production of carbon nanotubes, and can effectively and fully exert the catalytic efficiency of the catalyst in a carbon nanotube deposition process. The tail gas of carbon nanotube deposition is utilized, the energy consumption for production of unit weight carbon nanotube can be reduced, the carbon nanotube production cost is lowered, and the equipment structure is simpler.
Description
Technical field
The invention belongs to chemical vapor deposition method manufacturing field of equipment, relate to nano material producing apparatus.
Background technology
Carbon nanotube is One-dimensional nanocrystal novel material, has many excellent properties, and commercial applications has developed some frontiers, has also started to replace carbon black and graphite, become the additive product that downstream manufacturers is specified in traditional a lot of Application Areass.
Catalyst chemical gas phase deposition technique is the main method of industrialization scale operation carbon nanotube.The main process feature of the preset catalyst chemical gas phase deposition technique contacted with the present invention is: 1 adopts carbon-source gas as the growth carbon source of carbon nanotube.2, reaction chamber is in high temperature, anoxic, provides carbon source gas checking solution environment.3 preset solid catalysts, impel cracking carbon to be self-assembled into carbon nanotube according to carbon nanotube one dimension shape.
The equipment of preset solid catalyst chemical vapor carbon deposition nanotube is all horizontal gaseous phase deposition stove at present, and the technique of producing carbon nanotube has discontinuous to produce, continuous seepage.Major equipment has the horizontal gas phase of carrier bar delivering to sink stove and fluidized-bed gaseous phase deposition stove.The former device structure is complicated, and carbon nanotube prepared by the latter is agglomerating spherical, bad dispersibility.Generally use horizontal interruption chemical vapor deposition stove at present.
The main drawback that horizontal interruption chemical vapor deposition stove produces carbon nanotube is: 1, during workman's operate continuously, needs to face to open fire door taking-up product, places raw catalyst, so working conditions is arduous simultaneously; 2, production efficiency is low.Open fire door, take out product, placing raw catalyst needs to expend dead time, closes after fire door, emptying furnace gas again, and this all consumes effective growth time of carbon nanotube, reduces production efficiency.3, electricity can not be closed within the interval time of producing carbon nanotube, so improve the energy consumption of producing carbon nanotube.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, design the Reaktionsofen of the preset Catalyst Production carbon nanotube of a kind of vertical continuous.
The present invention is achieved by the following technical solutions.
The present invention includes process furnace (15), reaction chamber (13), collecting chamber (12), catalyzer charging machine (1), carbon nano tube growth plate (3), growth plate pillar stiffener (4), growth plate push rod (5), liquid packing (9), air-leg valve (7), movable sealing valve (10), carbon nanotube transfer roller (11), annular gas nozzle (6), carbon potential monitoring probe (14).
Reaction chamber (13) is arranged in process furnace (15), and reaction chamber (13) outer side wall and process furnace (15) thorax wall leave gap.Reaction chamber (13) is connected with collecting chamber (12) by tongued and grooved flanges.
Carbon nano tube growth plate (3) is positioned at reaction chamber (13) middle part, the furnace height position of corresponding 2/5.Carbon nano tube growth plate (3) and growth plate pillar stiffener (4) chain connection, can move around falling hinger axle vertical rotation.Growth plate pillar stiffener (4) is vertically fixed on collecting chamber (12) base plate center position.Growth plate motion push rod (5) one end and carbon nano tube growth plate (3) chain connection, the other end and air-leg valve (7) chain connection.Air-leg valve (7) sealing is fixed on collecting chamber (12) bottom, and at collecting chamber (12) outward, a part is in collecting chamber (12) for a part.
Movable sealing valve (10) is loaded in the outlet of collecting chamber (12) bottom barrel, can rotate around Horizontal-shaft vertical.
Carbon nanotube transfer roller (11) is positioned at collecting chamber (12) outlet below, is tightly connected with collecting chamber (12) discharge flange.
Liquid packing (9) admission piece is connected by pipeline with the outlet nozzle (8) being arranged on collecting chamber (12), and liquid packing outlet nozzle (8) is connected with annular gas nozzle (6).Annular gas nozzle (6) is positioned at above collecting chamber (12) shell, below reaction chamber (13) shell, faces reaction chamber (12) outer side wall and process furnace (15) inwall interstitial site.
Catalyzer charging machine (1) is enclosed construction, and its horizontal discharge port and reaction chamber (13) top bell sidewall are tightly connected.Carbon potential monitoring probe (14) is installed on interior carbon nano tube growth plate (3) top of reaction chamber (13) 1/2 growth plate diametrical position.
Catalyzer charging machine (1) of the present invention can be helical screw feeder, electric and magnetic oscillation feeder or belt feeder.
The horizontally disposed high-temperature zone at reaction chamber of carbon nano tube growth plate (3) of the present invention, temperature distribution is at 645 DEG C-1000 DEG C.The horizontal rotational shaft 90 degree of diameter walked around by carbon nano tube growth plate (3), and on it, the long carbon nanotube had just all can fall into collecting chamber (12).
Carbon nano tube growth plate (3) top and bottom of the present invention all cover nonmetal high temperature material, as silica glass, aluminium sesquioxide porcelain plate, stupalith plate, magnesium oxide porcelain plate, fireclay plate, silicon-dioxide porcelain plate or silicate material porcelain plate.
Carbon nano tube growth plate (3) of the present invention adopts Mo and Mo alloys, tungsten and alloy thereof or tantalum and alloy thereof.
The coating that the stainless steel push rod (5) of the carbon nano tube growth plate in reaction chamber of the present invention (13), stainless steel pillar stiffener (4) all adopt nonmetal high temperature material to make or casing protection.
The waste gas that the present invention discharges from reaction chamber (13) enters process furnace (15) burner hearth through the ring jet pipe (8) being positioned at vertical heater (15) bottom, burning.Realize exhaust gas utilization, effective save energy.
Carbon potential detection probe (14) of the present invention employing detects iron wire or iron alloy silk is made, and is installed in reaction chamber (13), and the carbon potential change in monitoring reaction chamber (13), judges the upgrowth situation of carbon nanotube.
Working process of the present invention is as follows: process furnace (15) starts, reaction chamber (13) temperature rises, rare gas element is sent into from admission piece (2), emptying reaction chamber (13) and collection room air, when in reaction chamber (13), temperature reaches 400 degree, catalyzer charging machine (1) works, and quantitatively sends into catalyzer, under gravity, catalyst sedimentation is on carbon nano tube growth plate (3).Send into hydrogen again by admission piece (2), reducing catalyst makes catalyzer have activity.When reaction chamber (13) temperature reaches carbon nanotube formation temperature, carbon source gas is sent into from admission piece (2), close hydrogen, the interior carbon potential of reaction chamber (13) raises, carbon nanotube starts growth on growth plate (3), after certain hour, carbon nanotube coated carbon nanotube growth plate (3) and thickening, catalyst failure, start catalyzer charging machine (1), quantitative feeding catalyzer, catalyzer is deposited in the carbon nanotube layer surface that carbon nano tube growth plate (3) has grown under gravity, by the hydrogen reducing in reaction chamber (13), play the effect of catalyzing carbon nanotube growth.Circulation like this, the thickness of the carbon nanotube layer on growth plate constantly increases.When the carbon nanotube layer thickness on carbon nano tube growth plate (3) reach a certain height, open air-leg valve (7), growth plate push rod (5) promotes carbon nano tube growth plate (3) around horizontal axis, carbon nano tube growth plate (3) plane is in close to vertical position, and the carbon nanotube on carbon nano tube growth plate (3) drops into collecting chamber (12) under gravity.The carbon nanotube stored in the collecting chamber (12) reach a certain amount of after, the movable sealing valve (10) of collecting chamber bottom is opened, and carbon nanotube transfer roller (11) works, and the carbon nanotube in collecting chamber (12) is transferred to reaction chamber (13) outward.Movable sealing valve (10) cuts out subsequently.Achieve the working cycle of first time self-feeding-deposition-discharging.
Gas return path working process: when carbon nano-tube, from admission piece (2) input carbon source gas and hydrogen carrier gas.At carbon nano tube growth plate (3), upper and catalyst chemical reacts and grows carbon nanotube carbon source gas, waste gas enters collecting chamber (12) and leaves reaction chamber (13) from reaction chamber outlet nozzle (8), enter liquid packing (9), flow out liquid packing (9) again to enter into annular gas jet pipe and enter into vertical heater thorax, in stove combustion, realize exhaust gas utilization.
Growth plate pillar stiffener (4) of the present invention also can be another design: namely pillar stiffener (4) can be designed to the structure that can move up and down, when carbon nano tube growth plate (3) covers with carbon nanotube, pillar stiffener (4) moves downward, carbon nano tube growth plate (3) is along with decline, enter collecting chamber (12), the now horizontal push pedal of collecting chamber (12) sidewall design one, can shift collecting chamber (12) onto the carbon nanotube on carbon nano tube growth plate (3).
Advantage performance of the present invention is as follows.
1, under use preformed catalyst condition, non-discontinuity can be realized and produce carbon nanotube, catalyzer can join in reaction chamber under uninterrupted deposition of carbon nanotubes condition, and carbon nanotube product also can not to stop under deposition process condition safe transport to outside reaction chamber.Another one workman can manage more equipment, increases substantially production efficiency and improves working conditions.The technique that present employing preformed catalyst produces carbon nanotube is generally horizontal chemical vapor deposition stove, after adding catalyzer, when deposition of carbon nanotubes one section, catalyst failure, now need to take out carbon nanotube, add raw catalyst, will deposition process be stopped for this reason, and blow-on lid, at high temperature take out carbon nanotube.Consume effective production time like this, reduce productivity, workman's production efficiency is low, and labor condition is arduous.
2, the catalytic efficiency of catalyzer can be played effectively fully in deposition of carbon nanotubes process.In deposition of carbon nanotubes process of the present invention, catalyzer is also that discontinuity joins reaction chamber, the carbon nanotube of growth is also that discontinuity is transported to outside reaction chamber, but minimumly within each break time sequentially to add more than 3 times catalyzer, the catalyzer that such first time and second time add also remains on carbon nano tube growth plate after catalyzing carbon nanotube growth, and the catalyzer added with third time plays the effect that catalyzing carbon nanotube grows jointly.So catalyst action can be played to greatest extent.
3, make use of the tail gas of deposition of carbon nanotubes.The energy consumption of production unit wt carbon nanotube can be reduced, reduce carbon nanotube production cost.
4, to realize the device structure of the relatively horizontal continuous seepage carbon nanotube of carbon nanotube quantity-produced equipment simpler in the present invention.
Accompanying drawing explanation
Accompanying drawing 1 is structural representation of the present invention.Wherein, 1 is catalyzer charging machine, and 2 is admission piece, 3 is carbon nano tube growth plate, and 4 is growth plate pillar stiffener, and 5 is growth plate push rod, 6 is annular gas nozzle, and 7 is air-leg valve, 8 reaction chamber outlet nozzles, 9 is liquid packing, and 10 is movable sealing valve, and 11 is carbon nanotube transfer roller, 12 is collecting chamber, 13 is reaction chamber, and 14 is carbon potential monitoring probe, and 15 is process furnace.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
1, working process is as follows: process furnace 15 starts, reaction chamber 12 temperature rises, enter rare gas element from admission piece 2, air in emptying reaction chamber 13, when in reaction chamber 13, temperature reaches 400 degree, conveying catalyzer charging machine 1 works, quantitative feeding catalyzer, under gravity, catalyst sedimentation is on carbon nano tube growth plate 3, now send into hydrogen again as reducing gas by admission piece 2, reducing catalyst is become the nanometer sized metal particles with catalytic activity by oxidized metal.Continue heating, when reaction chamber 13 temperature reaches carbon nanotube formation temperature, enter carbon source gas from admission piece 2, close hydrogen or rare gas element, now carbon source gas checking solution, in reaction chamber 13, carbon potential raises, carbon atom crystallization under catalyst action goes out carbon nanotube, continues insulation, carbon nano tube growth.After certain hour, catalyst failure, catalyzer charging machine 1 starts, quantitative feeding catalyzer, catalyzer is deposited in the carbon nanotube accumulation horizon surface grown under gravity, by the hydrogen reducing in reaction chamber 13, performance catalyzing carbon nanotube is formed, the effect of growth.Circulation like this, the thickness of the carbon nanotube accumulation horizon on growth plate 3 constantly increases.When the carbon nanotube accumulation horizon thickness on growth plate 3 reach a certain height, open air-leg valve 7, growth plate push rod 5 promotes carbon nano tube growth plate 3 and rotates around growth plate pillar stiffener 4, when carbon nano tube growth plate 3 planar tilt to a certain extent time, carbon nanotube on it drops into collecting chamber 12, and growth plate 3 resets under push rod 5 acts on subsequently.After this flow process of carbon nano-tube proceeds, and the carbon nanotube by volume of collecting chamber 12 increases, and the movable sealing valve 10 of collecting chamber 12 lower part outlet is opened, and carbon nanotube transfer roller 11 works, and the carbon nanotube in reaction chamber 13 is transferred to outside reaction chamber 13.Movable sealing valve 10 cuts out subsequently.More than achieve first time self-feeding--deposition---working cycle of discharging.
2, gas return path working process.When carbon nano-tube, input carbon source gas and hydrogen carrier gas from admission piece 2.Gas enters reaction chamber 13 from reaction chamber 13 top, skims over carbon nano tube growth plate 3, discharges from the outlet nozzle 8 being positioned at collecting chamber 12, enter liquid packing 9, out, enter into again annular gas nozzle 6, spirt vertical heater thorax 15, in stove combustion, realizes exhaust gas utilization.
Claims (7)
1. a Reaktionsofen for the preset Catalyst Production carbon nanotube of vertical continuous, is characterized in that comprising process furnace (15), reaction chamber (13), collecting chamber (12), catalyzer charging machine (1), carbon nano tube growth plate (3), growth plate pillar stiffener (4), growth plate push rod (5), liquid packing (9), air-leg valve (7), movable sealing valve (10), carbon nanotube transfer roller (11), annular gas nozzle (6), carbon potential monitoring probe (14);
Reaction chamber (13) is arranged in process furnace (15), and reaction chamber (13) outer side wall and process furnace (15) thorax wall leave gap, and reaction chamber (13) is connected with collecting chamber (12) by tongued and grooved flanges;
Carbon nano tube growth plate (3) is positioned at reaction chamber (13) middle part, the furnace height position of corresponding 2/5; Carbon nano tube growth plate (3) and growth plate pillar stiffener (4) chain connection, can move around falling hinger axle vertical rotation; Growth plate pillar stiffener (4) is vertically fixed on collecting chamber (12) base plate center position; Growth plate motion push rod (5) one end and carbon nano tube growth plate (3) chain connection, the other end and air-leg valve (7) chain connection; Air-leg valve (7) sealing is fixed on collecting chamber (12) bottom, and at collecting chamber (12) outward, a part is in collecting chamber (12) for a part;
Movable sealing valve (10) is loaded in the outlet of collecting chamber (12) bottom barrel, can rotate around Horizontal-shaft vertical;
Carbon nanotube transfer roller (11) is positioned at collecting chamber (12) outlet below, is tightly connected with collecting chamber (12) discharge flange;
Liquid packing (9) admission piece is connected by pipeline with the outlet nozzle (8) being arranged on collecting chamber (12), and liquid packing outlet nozzle (8) is connected with annular gas nozzle (6); Annular gas nozzle (6) is positioned at above collecting chamber (12) shell, below reaction chamber (13) shell, faces reaction chamber (12) outer side wall and process furnace (15) inwall interstitial site;
Catalyzer charging machine (1) is enclosed construction, and its horizontal discharge port and reaction chamber (13) top bell sidewall are tightly connected; Carbon potential monitoring probe (14) is installed on interior carbon nano tube growth plate (3) top of reaction chamber (13) 1/2 growth plate diametrical position.
2. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that described catalyzer charging machine (1) can be helical screw feeder, electric and magnetic oscillation feeder or belt feeder.
3. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that described carbon nano tube growth plate (3) top and bottom all cover silica glass, aluminium sesquioxide porcelain plate, stupalith plate, magnesium oxide porcelain plate, fireclay plate, silicon-dioxide porcelain plate or silicate material porcelain plate.
4. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that described carbon nano tube growth plate (3) adopts Mo and Mo alloys, tungsten and alloy thereof or tantalum and alloy thereof.
5. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that the stainless steel push rod (5) of the carbon nano tube growth plate in described reaction chamber (13), coating that stainless steel pillar stiffener (4) all adopts nonmetal high temperature material to make or casing protection.
6. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that described carbon potential detection probe (14) adopts detection iron wire or iron alloy silk to make.
7. the Reaktionsofen of the preset Catalyst Production carbon nanotube of vertical continuous according to claim 1, is characterized in that described growth plate pillar stiffener (4) is the structure that moves up and down, the horizontal push pedal of collecting chamber (12) sidewall design one.
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| CN201510124301.XA CN105174242B (en) | 2015-03-23 | 2015-03-23 | A kind of reacting furnace of the preset Catalyst Production CNT of vertical continuous |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381540A (en) * | 2017-07-21 | 2017-11-24 | 南昌大学 | A kind of horizontal kiln for reinforcing body catalyst continuous production CNT |
| CN109437158A (en) * | 2018-11-14 | 2019-03-08 | 江西晶纳新材料有限公司 | A kind of horizontal carbon nanotube cvd furnace of tubular |
| CN111115614A (en) * | 2019-10-12 | 2020-05-08 | 成都科汇机电技术有限公司 | Carbon nano tube prepared by catalytic cracking of hydrocarbon by rotary method, device and method |
| CN112657432A (en) * | 2020-12-15 | 2021-04-16 | 焦作集越纳米材料技术有限公司 | Reaction furnace for producing carbon nano tube |
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| CN102515139A (en) * | 2011-11-10 | 2012-06-27 | 青岛科技大学 | Two-chamber vertical vacuum controllable atmosphere furnace for continuously preparing nano materials through gas-phase method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381540A (en) * | 2017-07-21 | 2017-11-24 | 南昌大学 | A kind of horizontal kiln for reinforcing body catalyst continuous production CNT |
| CN109437158A (en) * | 2018-11-14 | 2019-03-08 | 江西晶纳新材料有限公司 | A kind of horizontal carbon nanotube cvd furnace of tubular |
| CN109437158B (en) * | 2018-11-14 | 2022-03-15 | 江西晶纳新材料有限公司 | Cylindrical horizontal carbon nanotube deposition furnace |
| CN111115614A (en) * | 2019-10-12 | 2020-05-08 | 成都科汇机电技术有限公司 | Carbon nano tube prepared by catalytic cracking of hydrocarbon by rotary method, device and method |
| CN112657432A (en) * | 2020-12-15 | 2021-04-16 | 焦作集越纳米材料技术有限公司 | Reaction furnace for producing carbon nano tube |
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