CN106395797B - Remove the carbon nanotubes purification system of metal ion - Google Patents
Remove the carbon nanotubes purification system of metal ion Download PDFInfo
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- CN106395797B CN106395797B CN201610768180.7A CN201610768180A CN106395797B CN 106395797 B CN106395797 B CN 106395797B CN 201610768180 A CN201610768180 A CN 201610768180A CN 106395797 B CN106395797 B CN 106395797B
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- carbon nanotubes
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- acid
- storage tank
- heat exchanger
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
Remove the carbon nanotubes purification system of metal ion, including fluid reaction bed, heat exchanger, acid storage tank, two grinders and two filter presses, the acid vapors of the fluid reaction bed discharge are passed through heat exchanger, the acid coolant of the heat exchanger discharge is passed through acid storage tank, the carbon nanotubes crude product of the fluid reaction bed discharge is passed through filter press, the acid solution of the filter press discharge is passed through acid storage tank, the carbon nanotubes crude product of the filter press discharge is passed through grinder, carbon nanotubes crude product after the grinder grinding passes through a grinder again, then pass to next filter press, obtain finished product carbon nanotubes.The present invention, carbon nanotubes crude product pass through the continuous grinder of twice, and removal impurity effect is good, and energy consumption is low.
Description
Technical field
The present invention relates to the carbon nanotubes purification system for removing metal ion, belong to carbon nanotubes production technical field.
Background technology
Carbon nanotubes is a kind of tubular nanometer material being made of carbon atom.Tube wall contains multilayer carbon atom and is referred to as multi wall
Carbon nanotubes（MWNT）, it is referred to as single-walled carbon nanotube containing single layer of carbon atom（SWNT）.Carbon nanotubes is since being found, and one
It is directly of interest as researcher using its unique structure and excellent performance.Novel conductive/high-strength meet material, electronic device,
Catalyst carrier material etc. has potential application prospect.
The preparation process of carbon nanotubes mainly has：Arc discharge method, laser ablation method, chemical vapour deposition technique, solid-phase thermal
Solution, flame synthesis, electric glow discharge method and polymerisation synthetic method etc..Wherein, the application of chemical vapour deposition technique (CVD)
The most extensively, this method is to allow gaseous alkanes by being attached with the template of catalyst granules, under conditions of 600~1200 DEG C,
Gaseous hydrocarbon decomposes generation carbon nanotubes.One outstanding advantages of this method are that Residual reactants are gas, may exit off reaction
System, obtains the higher carbon nanotubes of purity, while temperature also need not be very high, in contrast saves energy.However, CVD
Method need to use transition-metal catalyst, and such as Fe, Co, Ni and its alloy are as catalyst.This causes prepared carbon nanometer
Often the metal impurities containing high level, the presence of metal impurities can directly affect performance and the application of carbon nanotubes in pipe.
The technique that metal impurities are removed from carbon nanotubes is known as purifying.Carbon nanotubes can produce during purification reaction
Acid mist and spent acid.At present, acid mist and spent acid not only cause problem of environmental pollution, but also increase all without by recycling
Production cost.
Inventor has found by retrieval：Application No. 201510466039.7, entitled carbon nanotubes method of purification,
The patent discloses a kind of carbon nanotubes method of purification, and the carbon nanotubes method of purification mainly includes the following steps that：A, in fixation
During bed or fluid unit preparation carbon nanotubes or after the completion of preparation, reducing gas and/or inert gas are passed through, is specially
Hydrogen and/or carbon dioxide, the temperature of reaction for 100 DEG C -800 DEG C it
Between, the reaction time is 3-60 minutes, and gas flow rate is between 0.06m3/h-1000m3/h；B, stop being passed through
Reducing gas, drops to room temperature in the protection of inert gas, and inert gas is nitrogen and/or argon gas, that is, obtains purity as 99.5%
Carbon nanotubes above.Carbon nanotubes method of purification of the present invention can remove impurity on the premise of carbon pipe is not injured, and have
The advantages that technique is simple, easy to operate, and purification efficiency is high and cost is relatively low, is adapted to the carbon nanotubes purification of industrial mass.
But in the patent, can not be fully whole by the oxidizing gas in fixed bed or fluid unit after being passed through inert gas
Exclude, in fact, it is difficult to accomplish that carbon nanotubes can be cooled down in reducing gas and/or inert gas without by autoxidation,
The purity of carbon nanotubes is caused not reach more than 99.5%.
Inventor also found by retrieval：Application No. 201210476918.4, a kind of entitled purified carbon nanometer
The method of pipe, the invention discloses a kind of method of purifying carbon nano-tube, it includes the following steps：Extracted using soxhlet extraction
Impurity in carbon nanotubes crude product：First extracted with acid with strong oxidizing property, then extracted with deionized water.The purifying carbon nano-tube of the invention
Method with the acid with strong oxidizing property purifying carbon nano-tube of boiling temperature is in, treatment process is simple, processing time is short, eliminates pumping
Filter, centrifugation etc. process and substantially increase the efficiency of purifying carbon nano-tube；Purification process damaged caused by carbon nanotubes it is small, it is pure
Carbon nanotubes after change is heat-resist and has good reactivity and compatibility；And acid can be recycled and recycled, greatly
Resource is saved greatly.Although the patent describes the partial impurities removed in carbon nanotubes crude product, but have no mention of how
The impurity in acid with strong oxidizing property and deionized water is separated, it can be reused, is unfavorable for industrial mass production application.
The content of the invention
Above-mentioned in order to solve the problems, such as, the invention discloses a kind of carbon nanotubes for removing metal ion to purify system
System, its concrete technical scheme are as follows：
Remove the carbon nanotubes purification system of metal ion, including fluid reaction bed, heat exchanger, acid storage tank, two grindings
Machine and two filter presses, the place that the fluid reaction bed is used for carbon nanometer tube material powder and acid solution is reacted are described to change
Hot device is used for the sour gas that cooling fluid reaction bed produces, and the acid storage tank is used to store the acid solution that heat exchanger cools down
And the acid solution that filter press squeezes out, the filter press are used to extrude the liquid in carbon nanotubes crude product, the grinder
For being uniformly mixed by carbon nanotubes crude product and with non-oxidizable acid solution,
The acid vapors of the fluid reaction bed discharge are passed through heat exchanger, and the acid coolant of the heat exchanger discharge is passed through
Acid storage tank, the carbon nanotubes crude product of the fluid reaction bed discharge are passed through filter press, and the acid solution of the filter press discharge leads to
Enter acid storage tank, the carbon nanotubes crude product of the filter press discharge is passed through grinder, and the carbon nanotubes after the grinder grinding is thick
Product pass through a grinder again, then pass to next filter press, obtain finished product carbon nanotubes.
Air pump is provided with the acid storage tank, the air pump conveys air into acid storage tank from the bottom of acid storage tank, is used for
Acid solution in acid storage tank is uniformly mixed.
The heat exchanger selects jacketed type exchanger, and the jacketed type exchanger includes container and chuck, the chuck bag
Bottom and the surrounding of container are trapped among, gap is left between the chuck and container, the upper end of the chuck is provided with steam inlet,
The lower end of the chuck is provided with cooling liquid outlet, and the top of the container is provided with liquid outlet, and the bottom of the container is set
There is inlet,
Sour gas from fluid reaction bed is entered in chuck from steam inlet, is formed by the cooling effect of chuck
Coolant, and from cooling liquid outlet discharge, be passed into acid storage tank, in the container injection be used for cooling jacket in gas it is molten
Liquid, the bottom liquid inlet mouth of the solution from container in the container enter, and are discharged from the liquid outlet of container top.
Agitating device is provided with the container, the agitating device includes central actuating shaft, and the central actuating shaft passes through
It extend into container through chuck, and is stretched out from the top of container, the central actuating shaft surrounding is provided with several paddles,
Several described paddles are evenly distributed on the horizontal surrounding of central actuating shaft, and the paddle includes several one end and center
The horizon bar that drive shaft is fixed, each horizon bar are fixed with several perpendicular vertical plates, and the vertical plate is in half
Toroidal, adjacent vertical plate on the same horizon bar mutually stagger.
The through hole of several semicircular arcs is offered on the vertical plate, the circle where the through hole of the semicircular arc is with erecting
Circle where straight panel is concentric circles.
The heat exchanger landfill is flushed in underground, the steam inlet with ground, and the top of the central actuating shaft passes through
Driving device connects motor.
The inlet and cooling liquid outlet are located at around the bottom of central actuating shaft, and the liquid outlet is located at centre-driven
Beside the top of axis.
The present invention operation principle be：
The present invention, carbon nanometer tube material powder and acid solution chemically react on fluid reaction bed, generate carbon nanotubes,
Acid mist can be produced in the reaction process, is directly discharged in air, not only pollutes environment, while wastes industrial chemicals, by acid mist
It is passed into heat exchanger, acid mist is cooled to acid solution, then the acid solution is passed into acid storage tank, the acid solution in adjustment acid storage tank
PH, you can reuse.
The carbon nanotubes crude product generated on fluid reaction bed is input to filter press, and the acid solution of filter press extrusion is also transported to acid
Storage tank, treats that industry reuses.Handle to obtain filter cake by filter press, then the filter cake is put into twice grinder, add
Non-oxidizing acid, the metal impurities on carbon nanotubes crude product surface are rinsed out, which is also passed into acid storage tank, treat work again
Industry uses.Obtained in grinder after removing impurity, more clean carbon nanotubes.Pass through grinder twice, impurity removes more
Add thoroughly.
The beneficial effects of the invention are as follows：
1. the present invention, the carbon nanotubes crude product obtained from fluid reaction bed pass through the continuous grinder of twice, go to clean
Matter effect is good, and energy consumption is low, reduces carbon nanotubes crude product and repeatedly passes through filter press, longevity of service, reduces carbon nanotubes
The time of crude product cleaning；
2. the present invention, acid solution are recovered, treat industrial application again, avoid the wasting of resources；
3. it is of the invention, air pump is provided with acid storage tank, air pump conveys air into acid storage tank from the bottom of acid storage tank, can incite somebody to action
Acid solution in acid storage tank is uniformly mixed, and is conducive to the PH of accurately adjustment acid solution；
4. the present invention, soil heat exchanging device of the heat exchanger landfill around underground, heat exchanger has the effect of insulation, sour gas
In chuck, thermal energy fully by the liquid absorption in container, fully improves the heat utilization rate in sour gas, avoids industry body
Thermal energy wastes；
5. it is of the invention, agitating device is provided with heat exchanger, agitating device flows the liquid agitation in container, with container
The heat exchanger effectiveness of liquid in gas and container of the liquid of wall contact in constantly flow regime, increase chuck, is improved
Heat exchange efficiency, also improves thermal energy and is absorbed and used rate；
6. the present invention, paddle offers several to fix multiple semicircular vertical plates on horizon bar on vertical plate
The through hole of semicircular arc, in paddle rotary course, liquid is passed through from the through hole of semicircular arc, forms turbulent flow, liquid is under
When being passed through in the through hole of the semicircular arc of one paddle, to change direction again, and liquid is stirred leaf and promotes towards chamber wall
Flowing, liquid flowing are more uniform；Mutually staggering for adjacent vertical plate on the same horizon bar, adds liquid flow
Dynamic path, allows liquid sufficient heat exchange in flow process.
Brief description of the drawings
Fig. 1 is the connection relationship diagram of the present invention,
Fig. 2 is the structure diagram of the jacketed type exchanger of the present invention,
Reference numerals list：1-central actuating shaft, 2-liquid outlet, 3-container, 4-steam inlet, 5-chuck, 6-
Vertical plate, 7-horizon bar, 8-inlet, 9-cooling liquid outlet.
Embodiment
With reference to the accompanying drawings and detailed description, the present invention is furture elucidated.It should be understood that following embodiments are only
For illustrating the present invention rather than limiting the scope of the invention.
Fig. 1 is the connection relationship diagram of the present invention, with reference to attached drawing as it can be seen that the carbon nanotubes purification of this removal metal ion
System, including fluid reaction bed, heat exchanger, acid storage tank, two grinders and two filter presses, the fluid reaction bed are used for carbon
The place that nanotube source powder and acid solution are reacted, the heat exchanger are used for the sour gas that cooling fluid reaction bed produces
Body, the acid storage tank is for storing the acid solution that heat exchanger cools down and the acid solution that filter press squeezes out, the pressure
Filter is used to extruding liquid in carbon nanotubes crude product, and the grinder is used for carbon nanotubes crude product and molten with non-oxidizing acid
Liquid is uniformly mixed.
The acid vapors of the fluid reaction bed discharge are passed through heat exchanger, and the acid coolant of the heat exchanger discharge is passed through
Acid storage tank, the carbon nanotubes crude product of the fluid reaction bed discharge are passed through filter press, and the acid solution of the filter press discharge leads to
Enter acid storage tank, the carbon nanotubes crude product of the filter press discharge is passed through grinder, and the carbon nanotubes after the grinder grinding is thick
Product pass through a grinder again, then pass to next filter press, obtain finished product carbon nanotubes.The acidity of fluid reaction bed discharge
Steam is stored after being cooled down by heat exchanger by acid storage tank, treats industrial application again, and filter press extrudes the acid solution in carbon nanotubes crude product,
Grinder cleaning removes the impurity on carbon nanotubes crude product.Carbon nanotubes crude product passes through the continuous grinder of twice, removes impurity
Effect is good, and energy consumption is low, reduces carbon nanotubes crude product and repeatedly passes through filter press, longevity of service, it is thick to reduce carbon nanotubes
The time of product cleaning.
Air pump is provided with the acid storage tank, the air pump conveys air into acid storage tank from the bottom of acid storage tank, is used for
Acid solution in acid storage tank is uniformly mixed.Under the action of air stream, air stream agitates the acid solution in acid storage tank effect, acid
Liquid is in continuous turbulence state, is conveniently adjusted to obtain accurate pH value.
Fig. 2 is the structure diagram of the jacketed type exchanger of the present invention, with reference to attached drawing as it can be seen that the heat exchanger selects chuck
Formula heat exchanger, the jacketed type exchanger include container 3 and chuck 5, and the chuck 5 is enclosed in bottom and the surrounding of container 3, institute
State and gap is left between chuck 5 and container 3, the upper end of the chuck 5 is provided with steam inlet 4, and the lower end of the chuck 5 is set
There is cooling liquid outlet 9, the top of the container 3 is provided with liquid outlet 2, and the bottom of the container 3 is provided with inlet 8, comes from
The sour gas of fluid reaction bed is entered in chuck 5 from steam inlet 4, and coolant is formed by the cooling effect of chuck 5, and
Discharge, be passed into acid storage tank from cooling liquid outlet 9, solution of the injection for gas in cooling jacket 5, institute in the container 3
The bottom liquid inlet mouth 8 for stating the solution from container 3 in container 3 enters, and is discharged from the liquid outlet 2 at the top of container 3.From fluid reaction
The acid vapors of bed are cooled into liquid, and the heat in steam is by liquid absorption in container 3, steam and the liquid flow in container 3
To on the contrary, improving heat exchanger effectiveness.
Agitating device is provided with the container 3, the agitating device includes central actuating shaft 1, the central actuating shaft 1
Penetrate chuck 5 to extend into container 3, and stretched out from the top of container 3,1 surrounding of central actuating shaft is provided with several
Paddle, several described paddles are evenly distributed on the horizontal surrounding of central actuating shaft 1, the paddle include several one
The horizon bar 7 that end is fixed with central actuating shaft 1, each horizon bar 7 are fixed with several perpendicular vertical plates 6, institute
6 semicircular in shape shape of vertical plate is stated, the through hole of several semicircular arcs is offered on the vertical plate 6, the semicircular arc leads to
Circle where hole and the circle where vertical plate 6 are concentric circles.Paddle can flow the liquid agitation in container 3, liquid
Inside carries out heat exchange, avoids that the fluid temperature close to container 3 wall is high, and the fluid temperature close to 3 center of container is low, allows container 3
In liquid can fully absorb thermal energy.Adjacent vertical plate 6 on the same horizon bar 7 mutually staggers.Strengthen container 3
The scrambling of middle liquid flowing, makes the liquid internal thermal energy in container 3 fully dispersed uniformly.
The heat exchanger landfill is flushed in underground, the steam inlet 4 with ground, and the top of the central actuating shaft 1 leads to
Over-driving device connects motor.Avoid the thermal energy in heat exchanger by diffusion in atmosphere, soil is solid around heat exchanger again
Surely it is ignorant of, and the good heat insulating of soil, after soil is heated to predetermined temperature by chuck 5, the thermal energy in steam is with regard to abundant
By the liquid absorption in container 3.
The inlet 8 and cooling liquid outlet 9 are located at around the bottom of central actuating shaft 1, and the liquid outlet 2 is located at center
Beside the top of drive shaft 1.Ensure that the longitudinal center of central actuating shaft 1 from 5 heat exchanger of chuck passes through.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, further includes
Formed technical solution is combined by above technical characteristic.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (5)
1. the carbon nanotubes purification system of metal ion is removed, it is characterized in that including fluid reaction bed, heat exchanger, acid storage tank, two
A grinder and two filter presses, the place that the fluid reaction bed is used for carbon nanometer tube material powder and acid solution is reacted,
The heat exchanger is used for the sour gas that cooling fluid reaction bed produces, and the acid storage tank is used to store what heat exchanger cooled down
The acid solution that acid solution and filter press squeeze out, the filter press is used to extrude the liquid in carbon nanotubes crude product, described
Grinder is used to be uniformly mixed by carbon nanotubes crude product and with non-oxidizable acid solution, the acid steaming of the fluid reaction bed discharge
Vapour is passed through heat exchanger, and the acid coolant of the heat exchanger discharge is passed through acid storage tank, the carbon nanometer of the fluid reaction bed discharge
Pipe crude product is passed through filter press, and the acid solution of the filter press discharge is passed through acid storage tank, the carbon nanotubes of the filter press discharge
Crude product is passed through grinder, and the carbon nanotubes crude product after the grinder grinding passes through a grinder, then passes to next again
Filter press, obtains finished product carbon nanotubes；
Air pump is provided with the acid storage tank, the air pump conveys air into acid storage tank from the bottom of acid storage tank, for by acid
Acid solution in storage tank is uniformly mixed；
Agitating device is provided with the container, the agitating device includes central actuating shaft, and the central actuating shaft penetrates
Chuck is extend into container, and is stretched out from the top of container, and the central actuating shaft surrounding is provided with several paddles, if
The dry paddle is evenly distributed on the horizontal surrounding of central actuating shaft, and the paddle includes several one end and driven with center
The horizon bar that moving axis is fixed, each horizon bar are fixed with several perpendicular vertical plates, and the vertical plate is in semicircle
Shape, adjacent vertical plate on the same horizon bar mutually stagger.
2. the carbon nanotubes purification system according to claim 1 for removing metal ion, it is characterized in that the heat exchanger selects
With jacketed type exchanger, the jacketed type exchanger includes container and chuck, and the chuck is enclosed in bottom and the surrounding of container,
Gap is left between the chuck and container, the upper end of the chuck is provided with steam inlet, and the lower end of the chuck is provided with
Cooling liquid outlet, the top of the container are provided with liquid outlet, and the bottom of the container is provided with inlet, from fluid reaction
The sour gas of bed is entered in chuck from steam inlet, forms coolant by the cooling effect of chuck, and go out from coolant
Mouth discharge, is passed into acid storage tank, solution of the injection for gas in cooling jacket in the container, molten in the container
Liquid enters from the bottom liquid inlet mouth of container, is discharged from the liquid outlet of container top.
3. the carbon nanotubes purification system according to claim 2 for removing metal ion, it is characterized in that on the vertical plate
The through hole of several semicircular arcs is offered, the circle where the through hole of the semicircular arc and the circle where vertical plate are concentric
Circle.
4. the carbon nanotubes purification system according to claim 3 for removing metal ion, it is characterized in that the heat exchanger is filled out
Underground is embedded in, the steam inlet is flushed with ground, and motor is connected via drive in the top of the central actuating shaft.
5. it is according to claim 4 remove metal ion carbon nanotubes purification system, it is characterized in that the inlet and
Cooling liquid outlet is located at around the bottom of central actuating shaft, and the liquid outlet is located at beside the top of central actuating shaft.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610768180.7A CN106395797B (en) | 2016-08-31 | 2016-08-31 | Remove the carbon nanotubes purification system of metal ion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610768180.7A CN106395797B (en) | 2016-08-31 | 2016-08-31 | Remove the carbon nanotubes purification system of metal ion |
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| Publication Number | Publication Date |
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| CN106395797A CN106395797A (en) | 2017-02-15 |
| CN106395797B true CN106395797B (en) | 2018-04-24 |
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ID=58003211
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|---|---|---|---|
| CN201610768180.7A Active CN106395797B (en) | 2016-08-31 | 2016-08-31 | Remove the carbon nanotubes purification system of metal ion |
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| Country | Link |
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| CN (1) | CN106395797B (en) |
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Denomination of invention: Purification system of carbon nanotubes for removing metal ions Effective date of registration: 20200824 Granted publication date: 20180424 Pledgee: Bank of Jiangsu Co.,Ltd. Wuxi Shanbei sub branch Pledgor: WUXI DONGHENG NEW ENERGY TECHNOLOGY Co.,Ltd. Registration number: Y2020320010125 |