CN106379888B - Purification system for improving carbon nano pipe purity - Google Patents

Purification system for improving carbon nano pipe purity Download PDF

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Publication number
CN106379888B
CN106379888B CN201610772156.0A CN201610772156A CN106379888B CN 106379888 B CN106379888 B CN 106379888B CN 201610772156 A CN201610772156 A CN 201610772156A CN 106379888 B CN106379888 B CN 106379888B
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Prior art keywords
acid solution
hydrochloric acid
solution bucket
pipe
connecting tube
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CN201610772156.0A
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CN106379888A (en
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沈宇栋
万仁涛
梁荣皓
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Wuxi Dongheng New Energy Technology Co Ltd
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Wuxi Dongheng New Energy Technology Co Ltd
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Abstract

The present invention relates to a kind of purification systems for improving carbon nano pipe purity,Including hydrochloric acid solution bucket,Agitating device is equipped in hydrochloric acid solution bucket,Hydrochloric acid solution bucket lower end is connect by the first connecting tube with filtering kettle,First connecting tube is equipped with tapping valve,It filters kettle outer wall and is equipped with water inlet pipe,Controller,Water inlet pipe is equipped with inlet valve,It filters kettle inner wall and is equipped with chlorine ion concentration sensor,Ultrasonic washer,Filter the second connecting tube lower end of kettle lower end by three-way connection respectively with drainpipe,Circulation pipe connects,The circulation pipe other end is connect with hydrochloric acid solution bucket,Drainpipe is equipped with drain valve,Circulation pipe is equipped with circulating pump,The chlorine ion concentration sensor,Inlet valve,Drain valve is connect with controller respectively,Agitating device includes motor,Agitating shaft,With several stirring blades of stirring axis connection,One auxiliary agitation blade for being equipped with several holes of vertical connection on each stirring blade,The present invention improves the purity of carbon nanotube,Intelligence degree is high.

Description

Purification system for improving carbon nano pipe purity
Technical field
The present invention relates to a kind of purification systems for improving carbon nano pipe purity, belong to carbon nanotube technology field.
Background technology
Nanotube is also 10,000 times thinner than the hairline of people, and 100 times harder than steel of its hardness.It can be resistant to 6500°F(3593℃)High temperature, and with remarkable heat conductivility.Nanotube both may be used as metallic conductor, than gold Electric conductivity is much higher, is also used as semiconductor necessary to manufacture computer chip.Nanotube also has at very low temperature Superconductivity.
The classification of nanotube has:Nano-tube, single-walled carbon nanotube, double-walled carbon nano-tube, multi-walled carbon nanotube, functionalization Multi-walled carbon nanotube, short MWCNTs, industrial multi-walled carbon nano-tube, graphite multi-walled carbon nano-tube, large diameter thin-walled Carbon nanotube, nickel-plating carbon nanotube.Aerolite carbonaceous crystalline nanometric pipe.
In the development process that nanotube is applied to computer operation, an important milestone is exactly that nanotube is manufactured into Switch or transistor used in computer.1998, a research group in the gloomy research center in the affiliated Witter of IBM Corporation was i.e. with this It is studied for target.Researchers have shown that single nanotube there can be transistor, and improve its crystalline substance The electric conductivity of body.
However, being also that nanotube demonstrates the one side of its superiority applied to computer operation.People can be these Miniature tube is bonded together, and fiber or rope is made, and is used as the superpower reinforcing of superconducting cable or plastics and other advanced materials Agent.If nanotube has extremely strong flexibility, intensity and restoring force, they by can synthesized high-performance sport and aeronautical material. Due to its powerful tension, they have the curved property without rolling over and can restore original form.
In addition, nanotube applies also for needing most the place of heat conductivility.For example, if motor is done using nanotube Cooling fin, plastic components therein would not be melted by high temperature.This Minisize materials, which can be also placed in, to be needed to be resistant to extreme high heat Material among, such as the panel outside aircraft and rocket.American National space flight and Space Agency it is expected nanotube being placed in from anti- Among thermosphere to the various facilities such as suit.
Energy company also regards to nanotube with special esteem.Nanotube can be used for manufacturing smaller, lighter, the higher fuel of efficiency Battery, it can also be used to hydrogen of the storage as the energy.Researcher receives on flat sheet glass or other materials numerous Mitron is lined up, them is allowed to look like the neat wheatland of a piece of harvesting.The NEC of Japan and the Samsung of South Korea prepare will This display screen that television set is made by " field " that nanotube forms, to replace television set used by old-fashioned cathode-ray Pipe.
Currently, carbon nanotube preparation process mainly has arc discharge method, radium-shine ablation and chemical vapour deposition technique.Its In, chemical vapour deposition technique with its simple process, at low cost, nanotube is controllable, length is big, collection rate is high the features such as obtain extensively Research and application.Chemical vapour deposition technique is mainly transition metal or its oxide with nanoscale as catalyst, Carbon containing air source is pyrolyzed at relatively low temperature to prepare carbon nanotube.
In current carbon nanotube preparation process, in addition to some direct current arc methods are without catalyst, other methods are required to There are the participation of catalyst, catalyst mostly to select the transition-metals and their oxides such as iron, cobalt, nickel, manganese.With the life of carbon nanotube Long, metal active constituent can be coated by carbon-coating and lead to catalyst inactivation, inevitable in the carbon nanotube crude product because obtained from Ground remains metallic catalyst.In addition, in large-scale preparation process, while generating carbon nanotube inevitable that The carbon impurities such as the carbon nano-particle of agraphitic carbon, graphite particulate and other forms generate, this largely constrains carbon and receives Application and property research of the mitron in numerous areas.Therefore, in order to obtain high-purity carbon nanotube, it is necessary to carbon nanotube crude product into Row purifying.
The method that 105731417 A of Chinese invention patent specification CN disclose such a purifying carbon nano-tube, the side It is that the oxide of catalyst containing magnetic metal of fluidized state is provided under 1500-3000 DEG C of inert gas atmosphere that method, which includes to temperature, Carbon nanotube crude product;Magnetic metal catalyst oxide in the carbon nanotube crude product is reduced into magnetic metal by carbon Grain;The magnetic metal particle is adsorbed under magnetic fields.It is described the invention also discloses the device for purifying carbon nano-tube Device includes material inlet, inert gas air inlet, high temperature concentration equipment, offgas outlet and material collecting device, the high temperature magnetic separation Device includes hot room and forms the magnet in magnetic field in hot room, and the material collecting device includes material outlet and rewinding tank, institute Material inlet is stated, inert gas air inlet and material outlet are connected to hot room.But this device is to Purification of Carbon Nanotubes Efficiency is low, and intelligence degree is low.
204727614 U of Chinese utility model patent specification CN disclose the process units of such a carbon nanotube, and one Kind automation prepares the device of high-purity carbon nanotube comprising reactant conveying device, chemical reaction equipment, collection device, electricity Raw material, catalyst and reducing gas are transported to chemistry by furnace temperature control system and vacuum pump apparatus, reactant conveying device In reaction unit, carbon nanotube is generated in chemical reaction equipment, carbon nanotube is pushed in collection device;Chemical reaction dress Pre-reactor and main reactor including being cascaded are set, pre-reactor and main reactor are controlled by Furnace Temperature Controlling System Its reaction temperature, the pre-reaction in pre-reactor of raw material, catalyst and reducing gas generates carbon nanotube, then by carbon nanometer Pipe is blown into main reactor that the reaction was continued;The tail gas of pre-reactor, which is passed through in the main reactor, to be continued to convert, while to master Inside reactor is passed through catalyst and raw material.But this device is low to Purification of Carbon Nanotubes efficiency, intelligence degree is low.
Invention content
The technical problem to be solved in the present invention is to provide a kind of purification systems for improving carbon nano pipe purity, this is used for The purification system for improving carbon nano pipe purity improves the purity of carbon nanotube, and intelligence degree is high.
In order to solve the above-mentioned technical problem, of the invention includes that hydrochloric acid is molten for improving the purification system of carbon nano pipe purity Liquid bucket, filtering kettle, hydrochloric acid solution bucket top are equipped with feed pipe, agitating device, hydrochloric acid solution bucket lower end are equipped in hydrochloric acid solution bucket It is connect with filtering kettle by the first connecting tube, the first connecting tube is equipped with tapping valve, and filtering kettle outer wall is equipped with water inlet pipe, control Device, water inlet pipe are equipped with inlet valve, and filtering kettle inner wall is equipped with chlorine ion concentration sensor, ultrasonic washer, filtering kettle lower end The second connecting tube is connected, the second connecting tube lower end is connect with drainpipe, circulation pipe respectively by three-way connection, the circulation pipe other end Connect with hydrochloric acid solution bucket, drainpipe be equipped with drain valve, circulation pipe be equipped with circulating pump, the chlorine ion concentration sensor, Inlet valve, drain valve are connect with controller respectively, the agitating device include motor, agitating shaft, with stirring axis connection it is several A stirring blade, one auxiliary agitation blade for being equipped with several holes of vertical connection on each stirring blade.
The hydrochloric acid solution bucket inner wall is coated with release coating.
The release coating uses teflon material.
The filtering kettle lower end is concave.
The motor is shock-absorbing motor.
Using this Carbon nanotube purification system, has the following advantages:
1, carbon nanotube can be removed metal ion, improve carbon by being reacted with hydrochloric acid solution in hydrochloric acid solution bucket The purity of nanotube;
2, include motor, agitating shaft, several stirring blades with stirring axis connection, each stirring blade due to mixing device One auxiliary agitation blade for being equipped with several holes of upper vertical connection, this agitating device mixing effect is preferable, and reaction is made more to fill Point;
3, it is connect with filtering kettle with by the first connecting tube due to hydrochloric acid solution bucket, filtering kettle inner wall is equipped with chlorine ion concentration Sensor, ultrasonic washer, the second connecting tube lower end are connect with drainpipe, circulation pipe respectively by three-way connection, chlorion Concentration sensor, inlet valve, drain valve are connect with controller respectively, in this way can be to the carbon nanotube with acid solution in filtering kettle It carries out intelligentized be repeated as many times to wash, until obtaining the higher carbon nanotube of purity.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the structural schematic diagram of the present invention.
Wherein have:1. hydrochloric acid solution bucket;2. feed pipe;3. motor;4. agitating shaft;5. stirring blade;6. auxiliary Stirring blade;7. the first connecting tube;8. tapping valve;9. filtering kettle;10. water inlet pipe;11. inlet valve;12. chlorion is dense Spend sensor;13. ultrasonic washer;14. controller;15. the second connecting tube;16. three-way connection;17. drainpipe; 18. drain valve;19. circulation pipe;20. circulating pump.
Specific implementation mode
Purification system shown in Fig. 1 for improving carbon nano pipe purity, including hydrochloric acid solution bucket, filtering kettle, hydrochloric acid solution Bucket top is equipped with feed pipe, and agitating device is equipped in hydrochloric acid solution bucket, and hydrochloric acid solution bucket lower end passes through the first connecting tube and filtering Kettle connects, and the first connecting tube is equipped with tapping valve, and filtering kettle outer wall is equipped with water inlet pipe, controller, and water inlet pipe is equipped with inlet valve, It filters kettle inner wall and is equipped with chlorine ion concentration sensor, ultrasonic washer, filtering kettle lower end connects the second connecting tube, the second connection Pipe lower end is connect with drainpipe, circulation pipe respectively by three-way connection, and the circulation pipe other end is connect with hydrochloric acid solution bucket, drainpipe Be equipped with drain valve, circulation pipe be equipped with circulating pump, the chlorine ion concentration sensor, inlet valve, drain valve respectively with control Device connects, and the agitating device includes motor, agitating shaft, several stirring blades with stirring axis connection, each stirring blade One auxiliary agitation blade for being equipped with several holes of upper vertical connection.
The hydrochloric acid solution bucket inner wall is coated with release coating.
The release coating uses teflon material.
The filtering kettle lower end is concave.
The motor is shock-absorbing motor.
The carbon nanotube obtained by carbon nanotube preparing apparatus, which is entered by feed pipe in hydrochloric acid solution bucket, is reacted, Agitating device stirring further promotes reaction, after carbon nanotube is reacted in hydrochloric acid solution bucket, opens tapping valve, hydrochloric acid solution And carbon nanotube is discharged in filtering kettle, hydrochloric acid solution and carbon nanotube are stayed in through filtering kettle filtering outflow filtering kettle, carbon nanotube In filtering kettle, hydrochloric acid solution is discharged to by circulating pump and circulation pipe that hydrochloric acid solution bucket is secondary to be continuing with again, hydrochloric acid solution Circulating pump is closed after drained.There are remaining acid solutions in carbon nanotube at this time, and due to containing chlorion in acid solution, chlorine ion concentration passes Sensor detects the chlorion in remaining acid solution in carbon nanotube, and signal is transmitted to controller, controller control open inlet valve, Drain valve, water inlet pipe injection deionized water into filtering kettle clean carbon nanotube, and ultrasonic washer can promote carbon nanometer The separation of pipe and chlorion, after being repeated several times and cleaning, when chlorine ion concentration sensor detects chlorine residual in carbon nanotube When ion concentration is less than chlorine ion concentration sensor setting value, signal is transmitted to controller, controller by chlorine ion concentration sensor Inlet valve, drain valve are closed in control, and carbon nanotube taking-up after purification, which is finally put into drying and crushing device dry, crushing, is in Powder.
It is the prior art not have the technical characteristic being described in detail in the application.The application is only illustrated in above-described embodiment Principles and effects, not for limitation the application.Any person skilled in the art all can be in the essence without prejudice to the application God and under the scope of, carry out modifications and changes to above-described embodiment.Therefore, those of ordinary skill in the art is not taking off It, should be by the right of the application from all equivalent modifications or change completed under spirit and technological thought disclosed herein It is required that being covered.

Claims (3)

1. a kind of purification system for improving carbon nano pipe purity, it is characterised in that:Including hydrochloric acid solution bucket, filtering kettle, salt It is equipped with feed pipe above acid solution bucket, is equipped with agitating device in hydrochloric acid solution bucket, hydrochloric acid solution bucket lower end passes through the first connecting tube It is connect with filtering kettle, the first connecting tube is equipped with tapping valve, and filtering kettle outer wall is equipped with water inlet pipe, controller, and water inlet pipe is equipped with Inlet valve, filtering kettle inner wall are equipped with chlorine ion concentration sensor, ultrasonic washer, and filtering kettle lower end connects the second connecting tube, Second connecting tube lower end is connect with drainpipe, circulation pipe respectively by three-way connection, and the circulation pipe other end connects with hydrochloric acid solution bucket It connects, drainpipe is equipped with drain valve, and circulation pipe is equipped with circulating pump, the chlorine ion concentration sensor, inlet valve, drain valve point It is not connect with controller, the agitating device includes several stirring blades of motor, agitating shaft and stirring axis connection, each One auxiliary agitation blade for being equipped with several holes of vertical connection, the hydrochloric acid solution bucket inner wall are coated with anti-snearing on stirring blade Material, the filtering kettle lower end are concave.
2. the purification system described in accordance with the claim 1 for improving carbon nano pipe purity, it is characterised in that:The anti-snearing Material uses teflon material.
3. the purification system described in accordance with the claim 1 for improving carbon nano pipe purity, it is characterised in that:The motor is Shock-absorbing motor.
CN201610772156.0A 2016-08-31 2016-08-31 Purification system for improving carbon nano pipe purity Active CN106379888B (en)

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NO345003B1 (en) 2018-05-31 2020-08-17 Bergen Carbon Solutions As Apparatus and method for purification of carbon nanomaterial

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CN1277146A (en) * 1999-06-15 2000-12-20 李铁真 Method for purifying carbon nanometre tube in large scale
JP2002177702A (en) * 2000-12-08 2002-06-25 Sony Corp Ultrasonic reflux system for single step refining of carbon nano structure
KR101147259B1 (en) * 2008-09-30 2012-05-21 한화케미칼 주식회사 Continuous method and apparatus of purifying Carbon Nanotube
WO2010079981A2 (en) * 2009-01-09 2010-07-15 세종대학교산학협력단 Method for purification and distribution of carbon nano tubes
CN101591795B (en) * 2009-06-18 2011-06-29 广东韶配动力机械有限公司 Pickling unit for carbon nanotubes in composite coating and using method thereof
CN101780951B (en) * 2010-03-09 2011-10-19 北京大学 Purification method for obtaining high-purity carbon nano tube
TW201410597A (en) * 2012-04-27 2014-03-16 Showa Denko Kk Method for purifying multi-wall carbon nanotube
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