CN103435029A - Device and method for preparing continuous carbon nanotube aggregate by assistance of ultrasonic atomization - Google Patents

Device and method for preparing continuous carbon nanotube aggregate by assistance of ultrasonic atomization Download PDF

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Publication number
CN103435029A
CN103435029A CN2013104000453A CN201310400045A CN103435029A CN 103435029 A CN103435029 A CN 103435029A CN 2013104000453 A CN2013104000453 A CN 2013104000453A CN 201310400045 A CN201310400045 A CN 201310400045A CN 103435029 A CN103435029 A CN 103435029A
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reactor
aggregate
tube
carbon nano
preparing
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蒋雅雅
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WUHAN BOLIXIN NANO SCIENCE & TECHNOLOGY Co Ltd
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WUHAN BOLIXIN NANO SCIENCE & TECHNOLOGY Co Ltd
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Abstract

The invention relates to a device and a method for preparing continuous carbon nanotube aggregate by the assistance of ultrasonic atomization. The device comprises a high temperature reactor and an ultrasonic atomizer connected with the high temperature reactor, the high temperature reactor comprises a reactor and a high temperature heating furnace for heating the reactor, and the ultrasonic atomizer comprises an ultrasonic generator connected with an infusion device which is used for providing reaction liquid for ultrasonically atomizing the reaction liquid into vapor and an ultrasonic atomizer nozzle which is connected with the high temperature reactor and used for inputting the vapor into the reactor. The method for preparing the continuous carbon nanotube aggregate by the assistance of ultrasonic atomization comprises the following steps that the reaction liquid is input into the ultrasonic generator and ultrasonically atomized into the vapor, the vapor enters into the high temperature reactor under the action of carrier gas to generate the carbon nanotubes by catalytic pyrolysis, the carbon nanotubes are freely assembled into the aggregate in the carrier gas, and then the aggregate moves to the other end of the reactor along with the carrier gas so as to form the continuous carbon nanotube aggregate. So that the device and the method for preparing the continuous carbon nanotube aggregate by the assistance of ultrasonic atomization are conducive to the evenness and continuity of the high temperature catalytic pyrolysis.

Description

The auxiliary device and method for preparing the continuous carbon nano-tube aggregate of ultrasonic atomizatio
Technical field
The present invention relates to the nano material preparing technical field, relate in particular to a kind of device and method for preparing the continuous carbon nano-tube aggregate.
Background technology
Carbon nanotube has excellent mechanics, electricity, calorifics and multi-functional characteristic, in fields such as matrix material, technical fiber, bio-sensing, electromagnetic shieldings, extensive potential application foreground is arranged.It is the important step that realizes the carbon nanotube application that carbon nanotube is assembled into to macroscopical fiber.Chemical gas phase reaction can prepare continuous carbon nano-tube fibre.It is by reactant being input in a high temperature gas flow that chemical gas phase reaction prepares carbon nano-tube fibre, reactant is the catalyse pyrolysis carbon nano-tube under catalyst action, carbon nanotube forms aggregate in the air-flow assembling, aggregate moves and forms continuous carbon nanotube agglomerate with air-flow, to the spinning of continuous carbon nano-tube aggregate, then make continuous carbon nano-tube fibre.
The homogeneity of gas-phase reaction is relevant with the mode that continuity and reaction liquid enter reactor.Chinese invention patent is announced and disclosed that a kind of reactant is input in high-temperature reactor for No. CN100552105C is the mode by syringe connecting needle direct injection.It is that mode dropwise enters reactor that the mode of this injection is inputted reaction liquid, drop size is grade, millimetre-sized liquid particle enters into the homogeneity that the high-temperature reactor pyrolysis is unfavorable for reaction, then the even carbon nanotube that makes to react synthetic is influenced, even causes reaction discontinuous.
Therefore, improve chemical gas phase reaction synthesizing carbon nanotubes homogeneity and improve the carbon nano-tube fibre continuity, need to improve reactant input high-temperature reactor mode.
Summary of the invention
The object of the present invention is to provide a kind of in order to improve the auxiliary device and method for preparing the continuous carbon nano-tube aggregate of carbon nanotube agglomerate homogeneity and successional ultrasonic atomizatio.
For achieving the above object, the invention provides the auxiliary device for preparing the continuous carbon nano-tube aggregate of a kind of ultrasonic atomizatio, the auxiliary device for preparing the continuous carbon nano-tube aggregate of described ultrasonic atomizatio comprises high-temperature reactor and the ultrasonic atomizer be connected with high-temperature reactor, described high-temperature reactor comprises reactor and in order to heat the high-temperature heater of described reactor, described ultrasonic atomizer comprise in order to the infusion set with reaction liquid is provided, be connected for the ultra-sonic generator that the reaction liquid ultrasonic atomizatio become to fog with high-temperature reactor, be connected for fog being input to the ultrasonic atomizer nozzle of reactor.
As the present invention, further improve, described high-temperature reactor is vertical, horizontal or has certain pitch angle to place, and it is parallel, vertical with the reactor direction or become arbitrarily angled that fog enters the direction of high-temperature reactor.
As the present invention, further improve, described infusion set comprise infusion pump and be connected in infusion pump and ultra-sonic generator between in order in ultra-sonic generator the input reaction liquid syringe.
As the present invention, further improve, described ultrasonic atomizer comprise with infusion set, be connected in order to the infusion pipeline of carrying reaction liquid in ultra-sonic generator and in order to carry the conveying gas pipeline of conveying gas in ultra-sonic generator.
The present invention also can adopt following technical scheme to realize purpose of the present invention:
A kind of auxiliary method for preparing the continuous carbon nano-tube aggregate of ultrasonic atomizatio, comprise the following steps: provide ultrasonic atomizatio the auxiliary device for preparing the continuous carbon nano-tube aggregate, this device comprises high-temperature reactor and the ultrasonic atomizer be connected with high-temperature reactor, described high-temperature reactor comprises reactor and in order to heat the high-temperature heater of described reactor, described ultrasonic atomizer comprises the ultra-sonic generator be connected in order to the infusion set with reaction liquid is provided and is embedded in the ultrasonic atomizer nozzle in high-temperature reactor, described reaction liquid is atomized into fog through ultrasonic atomizer, fog enters high-temperature reactor catalyse pyrolysis reaction carbon nano-tube under the conveying gas airflow function, carbon nanotube is assembled and is formed aggregate in air-flow, aggregate moves to the reactor the other end with the carrier gas air-flow, form the continuous carbon nano-tube aggregate.
As the present invention, further improve, in the ultrasonic atomizatio process, to be input to the flow in reactor be 6-600ml/h to reaction liquid, and described ultrasonic atomizer conveying gas air flow rate is 0-2000ml/min.
As the present invention, further improve, described is 100-5000ml/min for the carrier gas air-flow velocity that fog is loaded into to high-temperature reactor.
As the present invention, further improve, described pyroreaction actuator temperature is at 800-1600 ℃.
As the present invention, further improve, described reaction liquid comprises liquid carbon source, catalyzer and additive, carbon source is one or more in the small molecules liquid such as ethylene glycol, methyl alcohol, ethanol, acetone, normal hexane, stupid class, catalyzer is one or more in the metal-salts such as ferrocene, nickel acetate, iron(ic) chloride, and additive is one or more in water, thiophene, molybdate.
As the present invention, further improve, described continuous carbon nano-tube aggregate is cylindric, carbon nanotube is distributed in three dimensions in aggregate, and the carbon nanotube diameter in aggregate is 2-20nm, and carbon nanotube is few-wall carbon nanotube, the tube wall number is less than 10, carbon nanotube exists with the tube bank form, tube bank diameter 10-300nm, and tube bank distributes along the aggregate length direction, the tube bank of part minor diameter rides between larger tube bank, forms the three dimensional network structure.
The present invention is by increasing the ultrasonic atomizatio utility appliance in the device preparing the continuous carbon nano-tube aggregate, be that described reaction liquid is input in ultrasonic atomizer, atomization enters into the high-temperature reactor catalytic cracking reaction after forming fog under the delivery air effect, and prepares the continuous carbon nano-tube aggregate under the carrier gas airflow function.The auxiliary method for preparing the continuous carbon nano-tube aggregate of described ultrasonic atomizatio is atomized into micron order by drop from grade, and the method input reactor to spray, improve the even performance that reaction liquid enters reactor, then realized that gas-phase reaction prepares the carbon nanotube of uniform texture, and improved the continuity of carbon nanotube agglomerate.
The accompanying drawing explanation
Fig. 1 is the auxiliary device schematic diagram for preparing carbon nanotube agglomerate of the ultrasonic atomizatio in the specific embodiment of the invention 1;
Fig. 2 is the auxiliary device schematic diagram for preparing carbon nanotube agglomerate of the ultrasonic atomizatio in the specific embodiment of the invention 3;
Fig. 3 is the sweep electron microscope photo on the carbon nanotube agglomerate surface that is prepared from of the present invention;
Fig. 4 is the transmission electron microscope photo of the carbon nanotube agglomerate that is prepared from of the present invention.
Embodiment
Below with reference to specific embodiment shown in the drawings, describe the present invention.What deserves to be explained is, the embodiment that hereinafter put down in writing does not limit the present invention, and the conversion on the structure that those of ordinary skill in the art makes according to these embodiment, method or function all is included in protection scope of the present invention.
The ultrasonic atomizer 3 that the auxiliary device for preparing the continuous carbon nano-tube aggregate of ultrasonic atomizatio of the present invention comprises high-temperature reactor and is connected with high-temperature reactor.Described high-temperature reactor comprises high-temperature heater 1 and is inserted in the reactor 2 in high-temperature heater 1.Described ultrasonic atomizer 3 is fixed in described reactor 2 one ends.Described ultrasonic atomizer 3 comprises ultra-sonic generator 32 and ultrasonic atomizer nozzle 31.Described ultra-sonic generator 32 is connected with infusion set, and ultrasonic atomizer nozzle 31 is connected with reactor 2, and the reaction liquid 7 of infusion set input enters into reactor 2 after ultrasonic atomizer 3 ultrasonic atomizatios.
Described high-temperature heater 1 is for pyrochemistry gas-phase reaction high temperature, for vertical, horizontal or have a high-temperature reactor at certain pitch angle.
Described reactor 2 is for the chemical gas phase reaction space, is silica glass, metal titanium pipe or carbon tube etc.
Described infusion set is that reaction liquid 7 is input to the device in ultrasonic atomizer 3, comprise infusion pump and syringe 4, described syringe 4 be connected between infusion pump and ultra-sonic generator 32 in order to the interior input reaction liquid 7 of ultra-sonic generator 32, described infusion set can be syringe pump etc. in other embodiments.
Described ultrasonic atomizer 3 is by 7 equipment that are atomized into fog of reaction liquid.
Described ultrasonic atomizer 3 has two pipelines, one tunnel is in order to the infusion pipeline 35 to the interior conveying reaction liquid 7 of ultra-sonic generator 32, described infusion pipeline 35 is connected with infusion set, and infusion set 3 is atomized into fog by reaction liquid 7 by described infusion pipeline 35 input ultrasonic atomizers.Another road is in order to the conveying gas pipeline 34 to the interior conveying conveying gas 5 of ultra-sonic generator 32, and under the effect of conveying gas 5, described ultrasonic atomizer nozzle 31 dispels the fog after atomization, after formation taper fog, is input in high-temperature reactor.Described ultrasonic atomizer 3 also comprises to control the ultrasonic controller 33 of ultra-sonic generator 32 and ultrasonic atomizer nozzle 31.It is parallel, vertical with reactor 2 directions or become any direction that the reactant of described ultrasonic atomizer 3 atomizations enters the direction of reactor 2, depends on reactor 2 designs.
Described ultrasonic atomizer 3 is that ultrasonic atomizing nozzle is embedded on reactor 2 front end flange dishes or is placed in reactor 2 with the high-temperature reactor mode of connection, and preferably mode is to be embedded in the ring flange central position.
The method that described ultrasonic atomizatio prepares the continuous carbon nano-tube aggregate is, reaction liquid 7 is expelled in ultra-sonic generator 32 according to certain flow by infusion set, reaction liquid 7 is become fog by ultrasonic atomizatio, and fog forms taper fog by ultrasonic atomizer nozzle 31 and enters high-temperature reactor under the airflow function of conveying gas 5.Described fog can also be other shapes, depends on the design of ultrasonic atomizer nozzle 31 spray patterns.Described fog enters high-temperature reactor catalyse pyrolysis reaction carbon nano-tube under conveying gas 5 airflow functions, carbon nanotube is freely assembled and is formed aggregate in carrier gas 6 air-flows, carbon nanotube agglomerate moves to reactor 2 the other ends with carrier gas 6 air-flows, then forms the continuous carbon nano-tube aggregate.The fog formed by ultrasonic atomizatio contributes to homogeneity and the continuity of high-temperature catalytic scission reaction.
Described reaction liquid 7 is 6-600ml/h by infusion set to reaction liquid 7 flows of input in ultrasonic atomizer 3, and preferably flow is 20-200ml/h.
The air flow rate of described conveying gas 5 is 0-2000ml/min.
Described carrier gas 6 air flow rates are 100-5000ml/min.
Described high-temperature reactor temperature of reaction is 800-1600 ℃, and preferably temperature is 1000-1300 ℃.
Described reaction liquid 7 carbonaceous sources, catalyzer and additive, carbon source is one or more in the small molecules liquid such as ethylene glycol, methyl alcohol, ethanol, acetone, normal hexane, stupid class; Catalyzer is one or more in the metal-salts such as ferrocene, nickel acetate, iron(ic) chloride; Additive is one or more in water, thiophene, molybdate etc.
In described reaction liquid 7, carbon source content is 80-99wt.%, and catalyst content is 0.1-10wt.%, and additive level is 0-20wt.%.
The carbon nanotube agglomerate of the auxiliary preparation of described ultrasonic atomizatio is shaped as cylindric, and it is thicker that aggregate forms end, arrives reactor 2 rear ends and slightly attenuates, and is distributed in three dimensions, and color is black.Carbon nanotube in aggregate exists with the tube bank form, the tube bank diameter Distribution is at 20-300nm, concentrate and be distributed in 30-100nm, tube bank is mainly arranged along air flow line, the tube bank of part minor diameter rides between larger tube bank, tube bank that will be larger connects, and forms the carbon nanotube web frame with certain orientation of the three-dimensional in space.
Described tube bank is containing the multi-walled pipes of few wall, and the few-wall carbon nanotube diameter is 2-15nm.
Embodiment is as follows:
Specific embodiment 1
Please refer to shown in Fig. 1, the auxiliary device for preparing the continuous carbon nano-tube aggregate of described ultrasonic atomizatio is horizontal.In the middle of described horizontal-type high temperature reactor, quartz tube reactor 2 is arranged, reactor 2 one ends have ultrasonic atomizer 3 and infusion set.Quartz tube reactor 2 two ends are by flangeseal reactor 2, and ring flange one end is ultrasonic atomizer nozzle 31 and gas-carrier pipeline 21 fixedly, and the other end has air outlet 22.
In the present embodiment, described infusion set is infusion pump and is connected in the syringe 4 on infusion pump.Described infusion pipeline 35 is connected with syringe 4, and described reaction liquid 7 is input in ultrasonic atomizer 3 by syringe 4 approach infusion pipelines 35 under the dynamic action of infusion pump.In other embodiments, described infusion set can for syringe pump etc., other can provide reaction liquid 7 to be input to the power set in ultrasonic atomizer 3.Concrete, syringe 4 on infusion set is connected with ultrasonic atomizer 3 by infusion pipeline 35, reaction liquid 7 is loaded in syringe 4, reaction liquid 7 in emitter 4 is made a bet in the infusion pump effect pushes atomization in ultrasonic atomizer 3, and the fog after atomization enters reactor 2 under the airflow function of conveying gas 5.Auxiliary continuous carbon nano-tube aggregate reaction liquid 7 formulas that prepare of ultrasonic atomizatio are: contain 2.3g ferrocene catalyzer, 0.3g thiophene, 97.4g acetone in the reaction liquid 7 of 100g.The air-flow of conveying gas 5 is hydrogen, and flow is 600ml/min.Carrier gas 6 is hydrogen, and flow is 2400ml/min.Pass into the argon gas air-discharging in the high-temperature reactor temperature-rise period in reactor 2, question response device 2 changes argon gas into hydrogen stream after rising to 1350 ℃, and the hydrogen stream flow is 2400ml/min.
Syringe 4 injection reaction liquid 7 flow velocitys are 50ml/h, and reaction liquid 7 enters into ultrasonic atomizer 3, by ultrasonic atomizatio, is become fog, and fog enters reactor 2 under the airflow function of conveying gas 5.The high temperature reaction zone catalytic cracking reaction carbon nano-tube of fog enter high-temperature reactor under conveying gas 5 airflow functions in, the carbon nanotube of growing in the high temperature vapor phase stream is freely assembled the macroscopic smog of formation group, smog group moves to reactor 2 the other ends with carrier gas 6 air-flows, smog group forms cylindrical shape, and move body diameter with air-flow to reactor 2 rear ends and be tapered, then formed the continuous carbon nano-tube aggregate.
Please refer to shown in Fig. 3, for the carbon nanotube agglomerate surface carbon nanotube distribution photo prepared by scanning electron-microscopic observation the present invention, carbon nanotube distributes along the aggregate length direction, and the tube bank of part minor diameter rides between larger tube bank, and carbon nanotube is connected into to the three dimensional network structure.Please refer to shown in Fig. 4, for passing through the aggregate photo of transmission electron microscope observation gained, described aggregate is comprised of double-walled carbon nano-tube, and the double-walled carbon nano-tube diameter is mainly at 8-10nm, and double-walled carbon nano-tube exists with the tube bank form.
Specific embodiment 2
Ultrasonic atomizatio is auxiliary, and to prepare reaction unit and the method for continuous carbon nano-tube aggregate similar with embodiment, and different is that reactor 2 is vertical, makes the continuous carbon nano-tube aggregate.
Specific embodiment 3
Please refer to shown in Fig. 2, ultrasonic atomizatio assists the reaction unit for preparing the continuous carbon nano-tube aggregate similar to Example 1, high-temperature reactor is inserted with the quartz tube reactor 2 with sidewall, ultrasonic atomizer 3 is installed on quartz tube reactor 2 sidewalls, it is vertical with reactor 2 that the reaction liquid 7 of ultrasonic atomizatio enters reactor 2 directions, so arrange, when fog enters reactor 2 under the airflow function of conveying gas 5, described fog initial velocity on the direction towards reactor 2 the other ends is zero, then contributes to the homogeneity of high-temperature catalytic scission reaction.Make the continuous carbon nano-tube aggregate.
Specific embodiment 4
Ultrasonic atomizatio assists the reaction unit for preparing the continuous carbon nano-tube aggregate similar to Example 1, different is in the process for preparing the continuous carbon nano-tube aggregate, reaction liquid 7 input high-temperature reactor flows are 100ml/h, form the larger carbon nanotube agglomerate of concentration in the visible reactor 2 of naked eyes, aggregate is assembled in reactor 2 rear end depositions, forms the continuous carbon nano-tube aggregate.
Specific embodiment 5
Ultrasonic atomizatio assists the reaction unit for preparing the continuous carbon nano-tube aggregate similar to Example 1, different is in the process for preparing the continuous carbon nano-tube aggregate, the air flow rate of conveying gas 5 is 1000ml/min, and carrier gas 6 air flow rates are 1000ml/min, make the continuous carbon nano-tube aggregate.
Specific embodiment 6
Ultrasonic atomizatio assists the reaction unit for preparing the continuous carbon nano-tube aggregate similar to Example 1, and different is in the process for preparing the continuous carbon nano-tube aggregate, and the pyroreaction actuator temperature is 950 ℃, forms the continuous carbon nano-tube aggregate.
Specific embodiment 7
Ultrasonic atomizatio assists the reaction unit for preparing the continuous carbon nano-tube aggregate similar to Example 1, different is in the process for preparing the continuous carbon nano-tube aggregate, reaction carbon source is normal hexane, catalyst aid is thiophene and ammonium molybdate, ammonium molybdate content is 0.05g, reactor 2 is observed and is formed the continuous carbon nano-tube aggregate, and aggregate concentration is lower.In the transmission electron microscope observation carbon nanotube agglomerate, carbon nanotube is containing Single Walled Carbon Nanotube, and diameter of single-wall carbon nano tube is 2nm.
Be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, technical scheme in each embodiment also can, through appropriate combination, form other embodiments that it will be appreciated by those skilled in the art that.
Above listed a series of detailed description is only illustrating for feasibility embodiment of the present invention; they are not in order to limit the scope of the invention, all disengaging within equivalent embodiment that skill spirit of the present invention does or change all should be included in protection scope of the present invention.

Claims (10)

1. a ultrasonic atomizatio is assisted the device for preparing the continuous carbon nano-tube aggregate, it is characterized in that: the auxiliary device for preparing the continuous carbon nano-tube aggregate of described ultrasonic atomizatio comprises high-temperature reactor and the ultrasonic atomizer be connected with high-temperature reactor, described high-temperature reactor comprises reactor and in order to heat the high-temperature heater of described reactor, described ultrasonic atomizer comprise in order to the infusion set with reaction liquid is provided, be connected for the ultra-sonic generator that the reaction liquid ultrasonic atomizatio become to fog with high-temperature reactor, be connected for fog being input to the ultrasonic atomizer nozzle of reactor.
2. ultrasonic atomizatio according to claim 1 is assisted the device for preparing the continuous carbon nano-tube aggregate, it is characterized in that: described high-temperature reactor is vertical, horizontal or has certain pitch angle to place, and it is parallel, vertical with the reactor direction or become arbitrarily angled that fog enters the direction of high-temperature reactor.
3. the auxiliary device for preparing the continuous carbon nano-tube aggregate of ultrasonic atomizatio according to claim 1 is characterized in that: described infusion set comprise infusion pump and be connected in infusion pump and ultra-sonic generator between the syringe in order to input reaction liquid in ultra-sonic generator.
4. the auxiliary device for preparing the continuous carbon nano-tube aggregate of ultrasonic atomizatio according to claim 1 is characterized in that: described ultrasonic atomizer comprise with infusion set, be connected in order to the infusion pipeline of carrying reaction liquid in ultra-sonic generator and in order to carry the conveying gas pipeline of conveying gas in ultra-sonic generator.
5. a ultrasonic atomizatio is assisted the method for preparing the continuous carbon nano-tube aggregate, it is characterized in that: the method comprises the following steps: provide ultrasonic atomizatio the auxiliary device for preparing the continuous carbon nano-tube aggregate, this device comprises high-temperature reactor and the ultrasonic atomizer be connected with high-temperature reactor, described high-temperature reactor comprises reactor and in order to heat the high-temperature heater of described reactor, described ultrasonic atomizer comprises the ultra-sonic generator be connected in order to the infusion set with reaction liquid is provided and is embedded in the ultrasonic atomizer nozzle in high-temperature reactor, described reaction liquid is atomized into fog through ultrasonic atomizer, fog enters high-temperature reactor catalyse pyrolysis reaction carbon nano-tube under the conveying gas airflow function, carbon nanotube is assembled and is formed aggregate in air-flow, aggregate moves to the reactor the other end with the carrier gas air-flow, form the continuous carbon nano-tube aggregate.
6. ultrasonic atomizatio according to claim 5 is assisted the method for preparing the continuous carbon nano-tube aggregate, it is characterized in that: in the ultrasonic atomizatio process, to be input to the flow in reactor be 6-600ml/h to reaction liquid, and described ultrasonic atomizer conveying gas air flow rate is 0-2000ml/min.
7. ultrasonic atomizatio according to claim 5 is assisted the method for preparing the continuous carbon nano-tube aggregate, and it is characterized in that: described is 100-5000ml/min for the carrier gas air-flow velocity that fog is loaded into to high-temperature reactor.
8. ultrasonic atomizatio according to claim 5 is assisted the method for preparing the continuous carbon nano-tube aggregate, and it is characterized in that: described pyroreaction actuator temperature is at 800-1600 ℃.
9. ultrasonic atomizatio according to claim 5 is assisted the method for preparing the continuous carbon nano-tube aggregate, it is characterized in that: described reaction liquid comprises liquid carbon source, catalyzer and additive, carbon source is one or more in the small molecules liquid such as ethylene glycol, methyl alcohol, ethanol, acetone, normal hexane, stupid class, catalyzer is one or more in the metal-salts such as ferrocene, nickel acetate, iron(ic) chloride, and additive is one or more in water, thiophene, molybdate.
10. ultrasonic atomizatio according to claim 5 is assisted the method for preparing the continuous carbon nano-tube aggregate, it is characterized in that: described continuous carbon nano-tube aggregate is cylindric, carbon nanotube is distributed in three dimensions in aggregate, carbon nanotube diameter in aggregate is 2-20nm, carbon nanotube is few-wall carbon nanotube, the tube wall number is less than 10, carbon nanotube exists with the tube bank form, tube bank diameter 10-300nm, tube bank distributes along the aggregate length direction, the tube bank of part minor diameter rides between larger tube bank, forms the three dimensional network structure.
CN2013104000453A 2013-09-05 2013-09-05 Device and method for preparing continuous carbon nanotube aggregate by assistance of ultrasonic atomization Pending CN103435029A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105329882A (en) * 2015-12-08 2016-02-17 赵屹坤 Preparation method of carbon nano-tube
CN105439118A (en) * 2014-09-28 2016-03-30 中国科学院大连化学物理研究所 Method for preparation of bamboo-shaped carbon nanotube by ultrasonic atomization
CN106395796A (en) * 2016-07-01 2017-02-15 赵春田 A carbon nanotube wire rod, a preparing method thereof, a preparing device and applications
CN108408716A (en) * 2018-03-26 2018-08-17 苏州捷迪纳米科技有限公司 System for manufacturing carbon nm tube
CN113490638A (en) * 2019-02-22 2021-10-08 住友电气工业株式会社 Method for producing carbon nanotube, method for producing carbon nanotube assembly line bundle, carbon nanotube production apparatus, carbon nanotube assembly line production apparatus, and carbon nanotube assembly line bundle production apparatus
CN115180614A (en) * 2022-08-02 2022-10-14 武汉市碳翁科技有限公司 Continuous carbon nanotube aggregate synthesis device and use method
CN116332159A (en) * 2023-03-28 2023-06-27 北京科技大学 Method and device for preparing carbon nano tube by catalytically cracking hydrocarbon under assistance of ultrasound

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101153413A (en) * 2007-09-04 2008-04-02 天津大学 Apparatus and method for producing continuous carbon nano-tube fibre by liquid sealed vapor-phase flow catalytic reaction
CN101613895A (en) * 2009-06-04 2009-12-30 天津大学 Process based on preparation carbon nano-tube fibre in the chemical vapor flow spinning method inert atmosphere
CN101817522A (en) * 2010-06-04 2010-09-01 温州大学 Method for preparing carbon nanometer tubes by using soluble metallic salt as catalyst
CN203558855U (en) * 2013-09-05 2014-04-23 武汉博力信纳米科技有限公司 Device for preparing continuous carbon nano tube aggregate under assistance of ultrasonic atomization

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101153413A (en) * 2007-09-04 2008-04-02 天津大学 Apparatus and method for producing continuous carbon nano-tube fibre by liquid sealed vapor-phase flow catalytic reaction
CN101613895A (en) * 2009-06-04 2009-12-30 天津大学 Process based on preparation carbon nano-tube fibre in the chemical vapor flow spinning method inert atmosphere
CN101817522A (en) * 2010-06-04 2010-09-01 温州大学 Method for preparing carbon nanometer tubes by using soluble metallic salt as catalyst
CN203558855U (en) * 2013-09-05 2014-04-23 武汉博力信纳米科技有限公司 Device for preparing continuous carbon nano tube aggregate under assistance of ultrasonic atomization

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105439118A (en) * 2014-09-28 2016-03-30 中国科学院大连化学物理研究所 Method for preparation of bamboo-shaped carbon nanotube by ultrasonic atomization
CN105329882A (en) * 2015-12-08 2016-02-17 赵屹坤 Preparation method of carbon nano-tube
CN105329882B (en) * 2015-12-08 2017-05-10 赵屹坤 Preparation method of carbon nano-tube
CN106395796A (en) * 2016-07-01 2017-02-15 赵春田 A carbon nanotube wire rod, a preparing method thereof, a preparing device and applications
CN108408716A (en) * 2018-03-26 2018-08-17 苏州捷迪纳米科技有限公司 System for manufacturing carbon nm tube
CN113490638A (en) * 2019-02-22 2021-10-08 住友电气工业株式会社 Method for producing carbon nanotube, method for producing carbon nanotube assembly line bundle, carbon nanotube production apparatus, carbon nanotube assembly line production apparatus, and carbon nanotube assembly line bundle production apparatus
CN113490638B (en) * 2019-02-22 2024-03-29 住友电气工业株式会社 Carbon nanotube, method for producing integrated wire thereof, method for producing integrated wire bundle, and apparatus for producing the same
CN115180614A (en) * 2022-08-02 2022-10-14 武汉市碳翁科技有限公司 Continuous carbon nanotube aggregate synthesis device and use method
CN116332159A (en) * 2023-03-28 2023-06-27 北京科技大学 Method and device for preparing carbon nano tube by catalytically cracking hydrocarbon under assistance of ultrasound

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Application publication date: 20131211