CN106379888A - Purification system for improving purity of carbon nanotubes - Google Patents

Purification system for improving purity of carbon nanotubes Download PDF

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Publication number
CN106379888A
CN106379888A CN201610772156.0A CN201610772156A CN106379888A CN 106379888 A CN106379888 A CN 106379888A CN 201610772156 A CN201610772156 A CN 201610772156A CN 106379888 A CN106379888 A CN 106379888A
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pipe
acid solution
hydrochloric acid
purification system
kettle
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CN201610772156.0A
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CN106379888B (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 invention relates to a purification system for improving the purity of carbon nanotubes. The purification system comprises a hydrochloric acid solution barrel, a stirring device is arranged in the hydrochloric acid solution barrel, the lower end of the hydrochloric acid solution barrel is connected to a filter kettle through a first connection pipe, a liquid discharge valve is arranged on the first connection pipe; the external wall of the filter kettle is provided with a water inlet pipe and a controller, a water inlet valve is arranged on the water inlet pipe; a chlorine ion concentration sensor and an ultrasonic washer are arranged on the internal wall of the filter kettle; the lower end of a second connection pipe on the lower end of the filter kettle is connected to a drain pipe and a circulation pipe through a T-junction, the other end of the circulation pipe is connected to the hydrochloric acid solution barrel, a drain valve is arranged on the drain pipe, a circulation pump is arranged on the circulation pipe; the chlorine ion concentration sensor, the water inlet pipe, and the drain valve are individually connected to the controller; the stirring device comprises a motor, a stirring shaft, and a plurality of stirring blades, which are connected to the stirring shaft, and each stirring blade is vertically connected to an auxiliary stirring blade provided with a plurality of holes. The provided purification system improves the carbon nanotube purity and the intellectualization degree is high.

Description

For improving the purification system of carbon nano pipe purity
Technical field
The present invention relates to a kind of purification system for improving carbon nano pipe purity, belong to carbon nanotube technology field.
Background technology
Nanotube is also thinner 10,000 times than the hairline of people, and its hardness is hard 100 times than steel.It can tolerate 6500°F(3593℃)High temperature, and have brilliance heat conductivility.Nanotube both can serve as metallic conductor, than golden Electric conductivity much higher it is also possible to as manufacture computer chip necessary to semiconductor.Nanotube also has at very low temperature Superconductivity.
The classification of nanotube has:Nano-tube, SWCN, double-walled carbon nano-tube, multi-walled carbon nano-tubes, functionalization Multi-walled carbon nano-tubes, short MWCNTs, industrial multi-walled carbon nano-tube, graphite multi-walled carbon nano-tube, large diameter thin-walled CNT, nickel-plating carbon nanotube.Aerolite carbonaceous crystalline nanometric pipe.
It is applied in the development process of computer computing in nanotube, an important milestone is exactly that nanotube is manufactured into Switch used or transistor in computer.1998, a research group in the gloomy research center in the affiliated Witter of IBM Corporation was i.e. with this Studied for target.Researcher proves that single nanotube can have the effect of transistor, and it is brilliant to improve it The electric conductivity of body.
However, being applied to computer computing is also the one side that nanotube demonstrates its superiority.People can be these Miniature tube is bonded together, and makes fiber or rope, as superconducting cable, or the superpower reinforcing of plastics and other advanced materials Agent.If nanotube possesses extremely strong flexibility, intensity and restoring force, they are by can the physical culture of synthesized high-performance and aeronautical material. Due to its powerful tension force, they have property that is curved and not rolling over and can recover original form.
Additionally, nanotube applies also for needing most the place of heat conductivility.For example, if motor is done using nanotube Fin, plastic components therein would not be melted by high temperature.This Minisize materials also can be inserted to be needed to tolerate extreme high heat Material among, such as aircraft and the panel outside rocket etc..American National space flight and NASA's expectation insert nanotube from anti- Thermosphere is among the various facilities such as suit.
Energy company also regards with special esteem to nanotube.Nanotube can be used to manufacture fuel less, that lighter, efficiency is higher Battery, it can also be used to store the hydrogen as the energy.Researcher receives numerous on flat sheet glass or other materials Mitron is lined up, and allows them look like the neat wheatland of a piece of harvesting.The Samsung of the NEC of Japan and Korea S prepares will This display screen being made television set by " field " that nanotube forms, to replace the old-fashioned cathode-ray that television set is adopted Pipe.
At present, CNT preparation technology mainly has arc discharge method, radium-shine ablation and chemical vapour deposition technique.Its In, chemical vapour deposition technique with its simple process, low cost, nanotube is controlled, length is big, collection rate is high the features such as obtain extensively Research and application.Chemical vapour deposition technique mainly uses the transition metal of nanoscale or its oxide as catalyst, It is pyrolyzed the source of the gas of carbon containing preparing CNT at a temperature of relatively low.
In current CNT preparation technology, in addition to some direct current arc methods are without catalyst, additive method is required to There is the participation of catalyst, the transition-metals and their oxides such as iron, cobalt, nickel, manganese mostly selected by catalyst.Life with CNT Long, metal active constituent can be led to catalyst to inactivate by carbon-coating cladding, because obtained from CNT crude product unavoidably Remain metallic catalyst.Additionally, in large-scale preparation process, generate while CNT inevitable that The carbon impurities such as the carbon nano-particle of agraphitic carbon, graphite particulate and other forms generate, and this constrains carbon to a great extent and receives Mitron is in the application of numerous areas and property research.Therefore, in order to obtain high-purity CNT it is necessary to enter to CNT crude product Row purifies.
The method of the open such a purifying carbon nano-tube of Chinese invention patent specification CN 105731417 A, described side Method is included to temperature for providing the oxide of catalyst containing magnetic metal of fluidized state under 1500-3000 DEG C of inert gas atmosphere CNT crude product;Magnetic metal catalyst oxide in described CNT crude product is reduced into magnetic metal by carbon Grain;Described magnetic metal particle is adsorbed under magnetic fields.The invention also discloses for the device of purifying carbon nano-tube, described Device includes material inlet, inert gas air inlet, high temperature concentration equipment, offgas outlet and material collecting device, described high temperature magnetic separation Device includes hot room and the magnet in high temperature interior formation magnetic field, and described material collecting device includes material outlet and rewinding tank, institute State material inlet, inert gas air inlet is all connected with hot room with material outlet.But this device is to Purification of Carbon Nanotubes Efficiency is low, and intelligence degree is low.
The process units of the open such a CNT of Chinese utility model patent specification CN 204727614 U, one Plant the device that high-purity CNT is prepared in automation, it includes reactant conveying device, chemical reaction equipment, collection device, electricity Furnace temperature control system and vacuum pump apparatus, raw material, catalyst and reducing gas are transported to chemistry by reactant conveying device In reaction unit, chemical reaction equipment generates CNT, CNT is pushed in collection device;Chemical reaction fills Put including the pre-reactor being cascaded and main reactor, pre-reactor and main reactor are by Furnace Temperature Controlling System control Its reaction temperature, the pre-reaction in pre-reactor of raw material, catalyst and reducing gas generates CNT, then by carbon nanometer Pipe is blown in main reactor and continues reaction;The tail gas of pre-reactor is passed through in described main reactor and continues conversion, simultaneously 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.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of purification system for improving carbon nano pipe purity, and this is used for The purification system improving carbon nano pipe purity improves the purity of CNT, and intelligence degree is high.
In order to solve above-mentioned technical problem, it is molten that the purification system for improving carbon nano pipe purity of the present invention includes hydrochloric acid Liquid bucket, filtration kettle, are provided with feed pipe, are provided with agitating device, hydrochloric acid solution bucket lower end in hydrochloric acid solution bucket above hydrochloric acid solution bucket It is connected with filtering kettle by the first connecting tube, the first connecting tube is provided with tapping valve, filter kettle outer wall and be provided with water inlet pipe, control Device, water inlet pipe is provided with water intaking valve, filters kettle inwall and is provided with chlorine ion concentration sensor, ultrasonic washer, filters kettle lower end Connect the second connecting tube, the second connecting tube lower end is connected with drainpipe, circulation pipe respectively by three-way connection, the circulation pipe other end It is connected with hydrochloric acid solution bucket, drainpipe is provided with draining valve, circulation pipe is provided with circulating pump, described chlorine ion concentration sensor, Water intaking valve, draining valve are connected with controller respectively, and it is some that described agitating device includes motor, shaft is connected with shaft Individual stirring vane, each stirring vane vertically connects an auxiliary agitation blade being provided with some holes.
Described hydrochloric acid solution bucket inwall scribbles release coating.
Described release coating adopts Teflon material.
Described filtration kettle lower end is concave.
Described motor is shock-absorbing motor.
Using this Carbon nanotube purification system, there is advantages below:
1st, CNT can be removed metal ion, improve carbon nanometer by being reacted with hydrochloric acid solution in hydrochloric acid solution bucket The purity of pipe;
2nd, due to mixing several stirring vanes that device includes motor, shaft is connected with shaft, each stirring vane hangs down Direct-connected connect an auxiliary agitation blade being provided with some holes, this agitating device mixing effect preferably, makes reaction more abundant;
3rd, because hydrochloric acid solution bucket is connected with filtering kettle with by the first connecting tube, filter kettle inwall and be provided with chlorine ion concentration sensing Device, ultrasonic washer, the second connecting tube lower end is connected with drainpipe, circulation pipe respectively by three-way connection, chlorine ion concentration Sensor, water intaking valve, draining valve are connected with controller respectively, so can carry out to filtering the CNT with acid solution in kettle Intelligentized repeatedly wash, until obtain the higher CNT of purity.
Brief description
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the structural representation of the present invention.
Wherein have:1. hydrochloric acid solution bucket;2. feed pipe;3. motor;4. shaft;5. stirring vane;6. assist Stirring vane;7. the first connecting tube;8. tapping valve;9. filter kettle;10. water inlet pipe;11. water intaking valves;12. chlorions are dense Degree sensor;13. ultrasonic washers;14. controllers;15. second connecting tubes;16. three-way connections;17. drainpipes; 18. draining valves;19. circulation pipes;20. circulating pumps.
Specific embodiment
For improving the purification system of carbon nano pipe purity shown in Fig. 1, including hydrochloric acid solution bucket, filter kettle, hydrochloric acid solution It is provided with feed pipe above bucket, in hydrochloric acid solution bucket, is provided with agitating device, the first connecting tube and filtration are passed through in hydrochloric acid solution bucket lower end Kettle connects, and the first connecting tube is provided with tapping valve, filters kettle outer wall and is provided with water inlet pipe, controller, water inlet pipe is provided with water intaking valve, Filter kettle inwall and be provided with chlorine ion concentration sensor, ultrasonic washer, filter kettle lower end and connect the second connecting tube, the second connection Pipe lower end is connected with drainpipe, circulation pipe respectively by three-way connection, and the circulation pipe other end is connected with hydrochloric acid solution bucket, drainpipe Be provided with draining valve, circulation pipe is provided with circulating pump, described chlorine ion concentration sensor, water intaking valve, draining valve respectively with control Device connects, several stirring vanes that described agitating device includes motor, shaft is connected with shaft, each stirring vane Upper vertically one auxiliary agitation blade being provided with some holes of connection.
Described hydrochloric acid solution bucket inwall scribbles release coating.
Described release coating adopts Teflon material.
Described filtration kettle lower end is concave.
Described motor is shock-absorbing motor.
The CNT being obtained by carbon nanotube preparing apparatus is entered in hydrochloric acid solution bucket by feed pipe and is reacted, Agitating device stirring promotes reaction further, after CNT reacts in hydrochloric acid solution bucket, opens tapping valve, hydrochloric acid solution And CNT is discharged in filtration kettle, hydrochloric acid solution and CNT filter outflow filter kettle through filtering kettle, and CNT is stayed In filtration kettle, hydrochloric acid solution passes through circulating pump and circulation pipe is discharged to that hydrochloric acid solution bucket is secondary is continuing with again, hydrochloric acid solution Circulating pump is closed after drained.Now leave remaining acid solution on CNT, due to containing chlorion in acid solution, chlorine ion concentration passes Sensor detects the chlorion in remaining acid solution on CNT, and signal is passed to controller, controller control open water intaking valve, Draining valve, water inlet pipe cleans toward filtering injection deionized water in kettle to CNT, and ultrasonic washer can promote carbon nanometer Pipe is separated with chlorion, after cleaning is repeated several times, when chlorine ion concentration sensor detects residual chlorine on CNT When ion concentration is less than chlorine ion concentration sensor setting value, signal is passed to controller, controller by chlorine ion concentration sensor Control close water intaking valve, draining valve, finally by after purification CNT take out be put in drying and crushing device be dried, pulverize be in Powder.
The technical characteristic describing in detail is not had to be prior art in the application.Above-described embodiment only illustrative the application Principle and its effect, not for limit 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, modifications and changes are carried out to above-described embodiment.Therefore, those of ordinary skill in the art is not taking off All equivalent modifications being completed under spirit disclosed herein with technological thought or change, must be by the right of the application Require to be covered.

Claims (5)

1. a kind of purification system for improving carbon nano pipe purity it is characterised in that:Including hydrochloric acid solution bucket, filter kettle, salt It is provided with feed pipe above acid solution bucket, in hydrochloric acid solution bucket, is provided with agitating device, the first connecting tube is passed through in hydrochloric acid solution bucket lower end It is connected with filtering kettle, the first connecting tube is provided with tapping valve, filter kettle outer wall and be provided with water inlet pipe, controller, water inlet pipe is provided with Water intaking valve, filters kettle inwall and is provided with chlorine ion concentration sensor, ultrasonic washer, filters kettle lower end and connects the second connecting tube, Second connecting tube lower end is connected with drainpipe, circulation pipe respectively by three-way connection, and the circulation pipe other end is with hydrochloric acid solution bucket even Connect, drainpipe is provided with draining valve, circulation pipe is provided with circulating pump, described chlorine ion concentration sensor, water intaking valve, draining valve divide It is not connected with controller, several stirring vanes that described agitating device includes motor, shaft is connected with shaft, each One auxiliary agitation blade being provided with some holes is vertically connected on stirring vane.
2. according to described in claim 1 for improve carbon nano pipe purity purification system it is characterised in that:Described hydrochloric acid is molten Liquid bucket inwall scribbles release coating.
3. according to described in claim 2 for improve carbon nano pipe purity purification system it is characterised in that:Described anti-snearing Material adopts Teflon material.
4. according to described in claim 1 for improve carbon nano pipe purity purification system it is characterised in that:Described filtration kettle Lower end is concave.
5. according to described in claim 1 for improve carbon nano pipe purity purification system it is characterised in that:Described motor is Shock-absorbing motor.
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NO20180759A1 (en) * 2018-05-31 2019-12-02 Bergen Carbon Solutions As Apparatus and method for purification of carbon nanomaterial
WO2019231334A1 (en) 2018-05-31 2019-12-05 Bergen Carbon Solutions As Apparatus and method for purification of carbon nanomaterial
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