CN106395797A - Carbon nano tube purification system capable of removing metal ions - Google Patents
Carbon nano tube purification system capable of removing metal ions Download PDFInfo
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- CN106395797A CN106395797A CN201610768180.7A CN201610768180A CN106395797A CN 106395797 A CN106395797 A CN 106395797A CN 201610768180 A CN201610768180 A CN 201610768180A CN 106395797 A CN106395797 A CN 106395797A
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- heat exchanger
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- 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
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Abstract
The invention discloses a carbon nano tube purification system capable of removing metal ions. The carbon nano tube purification system comprises a fluid reaction bed, a heat exchanger, an acid storage tank, two grinding machines and two pressure filters, wherein acidic steam discharged by the fluid reaction bed is fed into the heat exchanger; acidic cooling liquid discharged by the heat exchanger is fed into the acid storage tank; a carbon nano tube coarse product discharged by the fluid reaction bed is fed into one pressure filter; an acidic solution discharged by the pressure filter is fed into the acid storage tank; the carbon nano tube coarse product discharged by the pressure filter is fed into the grinding machine; the carbon nano tube coarse product ground by the grinding machine passes through the other grinding machine and then is fed into the next pressure filter to obtain a carbon nano tube finished product. According to the carbon nano tube purification system, the carbon nano tube coarse product is treated by the two continuous grinding machines, so that the impurity removal effect is good, and the energy consumption is low.
Description
Technical field
The present invention relates to removing the CNT purification system of metal ion, belong to CNT production technical field.
Background technology
CNT is a kind of tubular nanometer material being made up of carbon atom.Tube wall contains multilamellar carbon atom and is referred to as many walls
CNT（MWNT）, it is referred to as SWCN containing monolayer carbon atom（SWNT）.CNT since being found, one
Straight of interest for researcher with its unique structure and excellent performance.Novel conductive/high-strength meet material, electronic device,
The aspects such as catalyst carrier material have potential application prospect.
The preparation technology of CNT mainly has：Arc discharge method, laser ablation method, chemical vapour deposition technique, solid-phase thermal
Solution, flame synthesis, electric glow discharge method and polyreaction synthetic method etc..Wherein, the application of chemical vapour deposition technique (CVD)
The most extensive, the 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 CNT.One outstanding advantages of this method are Residual reactants is gas, may exit off reaction
System, obtains the higher CNT of purity, and temperature does not also need very high simultaneously, comparatively saves energy.However, CVD
Method need to use transition-metal catalyst, and such as Fe, Co, Ni and its alloy etc. is as catalyst.This leads to prepared carbon nanometer
Often metal impurities containing high level in pipe, the presence of metal impurities can directly affect performance and the application of CNT.
The technique removing metal impurities from CNT is referred to as purification.CNT can produce during purification reaction
Acid mist and spent acid.At present, acid mist and spent acid, all not through recycling, not only cause problem of environmental pollution, and increase
Production cost.
Inventor finds through retrieval：Application No. 201510466039.7, invention entitled CNT method of purification,
This patent discloses a kind of CNT method of purification, and described CNT method of purification mainly includes the following steps that：A, fixing
Bed or fluid unit prepare CNT during or preparation after the completion of, be passed through reducing gas and/or noble gases, specially
Hydrogen and/or carbon dioxide, the temperature of reaction be 100 DEG C -800 DEG C it
Between, the response time is 3-60 minute, and gas flow rate is between 0.06m3/h-1000m3/h；B, stopping are passed through reduction
Gas, drops to room temperature in the protection of noble gases, and noble gases are nitrogen and/or argon, that is, obtaining purity is more than 99.5%
CNT.CNT method of purification of the present invention can have technique Impurity removal on the premise of not injuring carbon pipe
Simply, simple to operate, purification efficiency is high and the advantages of cost is relatively low, the CNT purification of suitable industrial mass.But
In this patent, after being passed through noble gases, can not fully the oxidizing gas in fixed bed or fluid unit all be excluded
Go out, in fact, be difficult to accomplish that CNT can cool down in reducing gas and/or noble gases and not by autoxidation, cause
The purity of CNT does not reach more than 99.5%.
Inventor also finds through retrieval：Application No. 201210476918.4, a kind of invention entitled purified carbon nanometer
The method of pipe, the invention discloses a kind of method of purifying carbon nano-tube, it comprises the steps of：Extracted using soxhlet extraction
Impurity in CNT crude product：First extracted with acid with strong oxidizing property, then deionized water is extracted.The purifying carbon nano-tube of this invention
Method with being in the acid with strong oxidizing property purifying carbon nano-tube of boiling temperature, handling process is simple, process time is short, eliminates and takes out
The process such as filter, be centrifuged and substantially increasing the efficiency of purifying carbon nano-tube；The damage that purification process causes to CNT is little, pure
CNT after change is heat-resist and has good reactivity and the compatibility；And acid can be reclaimed and be recycled, greatly
Save greatly resource.Although this patent describes the partial impurities removing in CNT crude product, have no mention of how
Separate the impurity in acid with strong oxidizing property and deionized water, it can be reused, be unfavorable for that industrial mass production is applied.
Content of the invention
In order to solve above-mentioned problem, the invention discloses a kind of CNT purification system removing metal ion
System, its concrete technical scheme is as follows：
Remove metal ion CNT purification system, including fluid reaction bed, heat exchanger, acid storage tank, two grinders and
Two pressure filter, described fluid reaction bed is used for the place that carbon nanometer tube material powder and acid solution are reacted, described heat exchanger
The sour gas producing for cooling fluid reaction bed, described acid storage tank be used for storing the heat exchanger acid solution that obtains of cooling and
The acid solution that pressure filter squeezes out, described pressure filter is used for extruding the liquid in CNT crude product, and described grinder is used for
Mix homogeneously by CNT crude product with non-oxidizable acid solution,
The acid vapors that described fluid reaction bed is discharged are passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through acid storage
Tank, the CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, and the acid solution that described pressure filter is discharged is passed through acid
Storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, and the CNT crude product after described grinder grinding is again
Through a grinder, then pass to next pressure filter, obtain finished product CNT.
It is provided with air pump, described air pump conveys air from the bottom of acid storage tank is to acid storage tank, is used in described acid storage tank
By the acid solution mix homogeneously in acid storage tank.
Jacketed type exchanger selected by described heat exchanger, and described jacketed type exchanger includes container and chuck, described chuck bag
It is trapped among bottom and the surrounding of container, between described chuck and container, leaves space, the upper end of described chuck is provided with steam inlet,
The lower end of described chuck is provided with cooling liquid outlet, and the top of described container is provided with liquid outlet, the bottom setting of described container
There is inlet,
Sour gas from fluid reaction bed enters into chuck from steam inlet, forms cooling by the cooling effect of chuck
Liquid, and discharge from cooling liquid outlet, it is passed in acid storage tank, in described container, inject the solution for gas in cooling jacket,
The bottom liquid inlet mouth of the solution from container in described container enters, and discharges from the liquid outlet of container top.
It is provided with agitating device, described agitating device includes central actuating shaft, described central actuating shaft passes through in described container
It extend in container through chuck, and stretches out from the top of container, described central actuating shaft surrounding is provided with several paddles,
Several described paddles are evenly distributed on the horizontal surrounding of central actuating shaft, and described paddle includes several one end and center
The fixing horizon bar of drive shaft, each described horizon bar is fixed with several perpendicular vertical plates, and described vertical plate is in half
Toroidal, mutually the staggering of the adjacent vertical plate on same described horizon bar.
The through hole of several semicircular arcs offered on described vertical plate, the circle that the through hole of described semicircular arc is located with perpendicular
The circle that straight panel is located is concentric circular.
Described heat exchanger fills in underground, and described steam inlet is flushed with ground, and the top of described central actuating shaft is passed through
Driving means connect motor.
Described inlet and cooling liquid outlet are located at around the bottom of central actuating shaft, and described liquid outlet is located at centre-driven
The top side of axle.
The operation principle of the present invention is：
There is chemical reaction in the present invention, carbon nanometer tube material powder and acid solution on fluid reaction bed, generate CNT, this is anti-
Acid mist can be produced during answering, be directly discharged in the air, not only pollute environment, waste industrial chemicals simultaneously, acid mist is passed through
To in heat exchanger, acid mist is cooled to acid solution, then this acid solution is passed in acid storage tank, the PH of the acid solution in adjustment acid storage tank,
Can reuse.
The CNT crude product generating on fluid reaction bed is input to pressure filter, and the acid solution of pressure filter extrusion is also transported to acid
Storage tank, treats that industry reuses.Process through pressure filter and obtain filter cake, then this filter cake is put in twice grinder, add
Non-oxidizing acid, the metal impurities on CNT crude product surface is rinsed out, this acid solution is also passed in acid storage tank, treats work again
Industry uses.After obtaining the removal of impurity in grinder, more clean CNT.Twice through grinder, Impurity removal obtains more
Plus thoroughly.
The invention has the beneficial effects as follows：
1. the present invention, the CNT crude product obtaining from fluid reaction bed, through the continuous grinder of twice, goes the removal of impurity to imitate
Really good, and energy consumption is low, decreases CNT crude product repeatedly through pressure filter, longevity of service, decreases CNT crude product
The time of cleaning；
2. the present invention, acid solution is recovered, and treats industrial application again, it is to avoid the wasting of resources；
3. the present invention, is provided with air pump in acid storage tank, air pump conveys air from the bottom of acid storage tank is to acid storage tank, can be by acid storage
Acid solution mix homogeneously in tank, is conducive to accurately adjusting the PH of acid solution；
4. the present invention, the soil heat exchanger that heat exchanger fills around underground, heat exchanger has the effect of insulation, and sour gas exists
In chuck, heat energy is fully absorbed by the liquid in container, fully improves the heat utilization rate in sour gas, it is to avoid industrial heat energy
Waste；
5. the present invention, is provided with agitating device in heat exchanger, the liquid agitation in container is flowed by agitating device, connects with chamber wall
Tactile liquid, in constantly flow regime, increases the heat exchanger effectiveness of the gas in chuck and the liquid in container, improves heat exchange
Efficiency, also improves heat energy and is absorbed and used rate；
6. the present invention, paddle is to fix multiple semicircular vertical plates on horizon bar, and vertical plate offers several semicircles
The through hole of arc, in paddle rotary course, liquid passes through from the through hole of semicircular arc, forms turbulent flow, liquid is from the next one
When passing through in the through hole of the semicircular arc of paddle, direction to be changed again, and liquid is stirred leaf and promotes towards chamber wall flowing,
Liquid flowing is more uniform；Mutually staggering of adjacent vertical plate on same described horizon bar, increased liquid flowing
Path, allows liquid sufficient heat exchange in flow process.
Brief description
Fig. 1 is the annexation schematic diagram of the present invention,
Fig. 2 is the structural representation of the jacketed type exchanger of the present invention,
Reference numerals list：1 central actuating shaft, 2 liquid outlets, 3 containers, 4 steam inlets, 5 chucks, 6 is vertical
Plate, 7 horizon bars, 8 inlets, 9 cooling liquid outlets.
Specific embodiment
With reference to the accompanying drawings and detailed description, it is further elucidated with the present invention.It should be understood that following specific embodiments are only
For the present invention being described rather than limiting the scope of the present invention.
Fig. 1 is the annexation schematic diagram of the present invention, visible in conjunction with accompanying drawing, the CNT purification of this removal metal ion
System, including fluid reaction bed, heat exchanger, acid storage tank, two grinders and two pressure filter, described fluid reaction bed is used for carbon
The place that nanotube source powder and acid solution are reacted, described heat exchanger is used for the sour gas that cooling fluid reaction bed produces
Body, described acid storage tank is for storing the acid solution that heat exchanger cooling obtains and the acid solution that pressure filter squeezes out, described pressure
Filter is used for extruding liquid in CNT crude product, and described grinder is used for CNT crude product and molten with non-oxidizing acid
Liquid mix homogeneously.
The acid vapors that described fluid reaction bed is discharged are passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through
Acid storage tank, the CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, and the acid solution that described pressure filter is discharged leads to
Enter acid storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, the CNT after described grinder grinds is thick
Product through a grinder, then pass to next pressure filter again, obtain finished product CNT.The acidity that fluid reaction bed is discharged
Steam is stored by acid storage tank after being cooled down by heat exchanger, treats industrial application again, and the acid solution in CNT crude product extruded by pressure filter,
Grinder cleaning removes the impurity on CNT crude product.CNT crude product, through the continuous grinder of twice, goes the removal of impurity
Effect is good, and energy consumption is low, decreases CNT crude product repeatedly through pressure filter, longevity of service, decreases CNT thick
The time of product cleaning.
It is provided with air pump, described air pump conveys air from the bottom of acid storage tank is to acid storage tank, is used in described acid storage tank
By the acid solution mix homogeneously in acid storage tank.In the presence of air stream, air stream agitates effect to the acid solution in acid storage tank, acid
Liquid is in continuous turbulence state, is conveniently adjusted and obtains accurate pH value.
Fig. 2 is the structural representation of the jacketed type exchanger of the present invention, visible in conjunction with accompanying drawing, and chuck selected by described heat exchanger
Formula heat exchanger, described jacketed type exchanger includes container 3 and chuck 5, and described chuck 5 is enclosed in bottom and the surrounding of container 3, institute
State and between chuck 5 and container 3, leave space, the upper end of described chuck 5 is provided with steam inlet 4, the lower end setting of described chuck 5
There is cooling liquid outlet 9, the top of described container 3 is provided with liquid outlet 2, and the bottom of described container 3 is provided with inlet 8, is derived from
The sour gas of fluid reaction bed enters into chuck 5 from steam inlet 4, forms coolant by the cooling effect of chuck 5, and
Discharge from cooling liquid outlet 9, be passed in acid storage tank, in described container 3, inject the solution for gas in cooling jacket 5, institute
The bottom liquid inlet mouth 8 stating the solution from container 3 in container 3 enters, and discharges from the liquid outlet 2 at container 3 top.From fluid reaction
The acid vapors of bed are cooled into liquid, and the heat in steam is absorbed by liquid in container 3, the liquid flow in steam and container 3
To contrary, improve heat exchanger effectiveness.
It is provided with agitating device, described agitating device includes central actuating shaft 1, described central actuating shaft 1 in described container 3
Penetrate chuck 5 to extend in container 3, and stretch out from the top of container 3, described central actuating shaft 1 surrounding is provided with several
Paddle, several described paddles are evenly distributed on the horizontal surrounding of central actuating shaft 1, described paddle include several one
The end horizon bar 7 fixing with central actuating shaft 1, each described horizon bar 7 is fixed with several perpendicular vertical plates 6, institute
State vertical plate 6 semicircular in shape shape, described vertical plate 6 offer the through hole of several semicircular arcs, described semicircular arc logical
The circle that the circle that hole is located is located with vertical plate 6 is concentric circular.Liquid agitation in container 3 can be flowed by paddle, liquid
Inside carries out heat exchange, it is to avoid high near the temperature of liquid of container 3 wall, and the temperature of liquid near container 3 center is low, allows container 3
In liquid can fully absorb heat energy.Mutually the staggering of adjacent vertical plate 6 on same described horizon bar 7.Strengthen container 3
The scrambling of middle liquid flowing, makes the liquid internal heat energy in container 3 fully dispersed uniformly.
Described heat exchanger fills in underground, and described steam inlet 4 is flushed with ground, and the top of described central actuating shaft 1 is passed through to drive
Dynamic device connects motor.Avoid heat energy in heat exchanger by diffusion in atmosphere, soil around heat exchanger be again fixing not
Understand, and the good heat insulating of soil, after soil is heated to predetermined temperature by chuck 5, the heat energy in steam is just fully held
Liquid in device 3 absorbs.
Described inlet 8 and cooling liquid outlet 9 are located at around the bottom of central actuating shaft 1, and described liquid outlet 2 is located at center
The top side of drive shaft 1.Guarantee that central actuating shaft 1 passes through from the longitudinal center of chuck 5 heat exchanger.
Technological means disclosed in the present invention program are not limited only to the technological means disclosed in above-mentioned technological means, also include
The technical scheme being made up of above technical characteristic combination in any.
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, relevant staff is complete
Entirely various change and modification can be carried out in the range of without departing from this invention technological thought.The technology of this invention
The content that property scope is not limited in description it is necessary to determine its technical scope according to right.
Claims (7)
1. remove metal ion CNT purification system, it is characterized in that including fluid reaction bed, heat exchanger, acid storage tank, two
Individual grinder and two pressure filter, described fluid reaction bed is used for the place that carbon nanometer tube material powder and acid solution are reacted,
Described heat exchanger is used for the sour gas that cooling fluid reaction bed produces, and described acid storage tank is used for storing what heat exchanger cooling obtained
The acid solution that acid solution and pressure filter squeeze out, described pressure filter is used for extruding the liquid in CNT crude product, described
Grinder is used for mixing homogeneously by CNT crude product with non-oxidizable acid solution,
The acid vapors that described fluid reaction bed is discharged are passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through acid storage
Tank, the CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, and the acid solution that described pressure filter is discharged is passed through acid
Storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, and the CNT crude product after described grinder grinding is again
Through a grinder, then pass to next pressure filter, obtain finished product CNT.
2. the CNT purification system removing metal ion according to claim 1, is characterized in that in described acid storage tank
It is provided with air pump, described air pump conveys air from the bottom of acid storage tank is to acid storage tank, for mixing the acid solution in acid storage tank
Uniformly.
3. the CNT purification system removing metal ion according to claim 1, is characterized in that described heat exchanger choosing
With jacketed type exchanger, described jacketed type exchanger includes container and chuck, and described chuck is enclosed in bottom and the surrounding of container,
Space is left, the upper end of described chuck is provided with steam inlet, and the lower end of described chuck is provided between described chuck and container
Cooling liquid outlet, the top of described container is provided with liquid outlet, and the bottom of described container is provided with inlet,
Sour gas from fluid reaction bed enters into chuck from steam inlet, forms cooling by the cooling effect of chuck
Liquid, and discharge from cooling liquid outlet, it is passed in acid storage tank, in described container, inject the solution for gas in cooling jacket,
The bottom liquid inlet mouth of the solution from container in described container enters, and discharges from the liquid outlet of container top.
4. the CNT purification system removing metal ion according to claim 3, is characterized in that setting in described container
It is equipped with agitating device, described agitating device includes central actuating shaft, described central actuating shaft penetrates chuck and extend in container,
And stretch out from the top of container, described central actuating shaft surrounding is provided with several paddles, and several described paddles are uniform
It is centrally located the horizontal surrounding of drive shaft, described paddle includes several one end horizon bar fixing with central actuating shaft,
Each described horizon bar is fixed with several perpendicular vertical plates, described vertical plate semicircular in shape shape, same described water
Mutually the staggering of adjacent vertical plate on flat bar.
5. the CNT purification system removing metal ion according to claim 4, is characterized in that on described vertical plate
Offer the through hole of several semicircular arcs, the circle that the circle at the through hole place of described semicircular arc is located with vertical plate is concentric
Circle.
6. the CNT purification system removing metal ion according to claim 3, is characterized in that described heat exchanger is filled out
It is embedded in underground, described steam inlet is flushed with ground, the top of described central actuating shaft is connected via drive motor.
7. according to claim 4 remove metal ion CNT purification system, it is characterized in that described inlet and
Cooling liquid outlet is located at around the bottom of central actuating shaft, and described liquid outlet is located at the top side 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 |
Publications (2)
| Publication Number | Publication Date |
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| CN106395797A true CN106395797A (en) | 2017-02-15 |
| CN106395797B CN106395797B (en) | 2018-04-24 |
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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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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 |
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