CN106167259B - The Carbon nanotube purification system of precipitate metal ion - Google Patents
The Carbon nanotube purification system of precipitate metal ion Download PDFInfo
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- CN106167259B CN106167259B CN201610763581.3A CN201610763581A CN106167259B CN 106167259 B CN106167259 B CN 106167259B CN 201610763581 A CN201610763581 A CN 201610763581A CN 106167259 B CN106167259 B CN 106167259B
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Abstract
The Carbon nanotube purification system of precipitate metal ion, including fluid reaction bed, jacketed type exchanger, acid storage tank, stirred tank, precipitation by metallic ion pond and two filter presses, the acid vapors of the fluid reaction bed discharge are passed through jacketed type exchanger, the acid coolant of the jacketed type exchanger discharge is passed through acid storage tank, the acid solution that the CNT crude product solution of the fluid reaction bed discharge is discharged after filter press press filtration processing is passed through acid storage tank, the CNT crude product solution of the filter press discharge is passed through stirred tank, then pass to next filter press, obtain finished product CNT, the solution discharged in the stirred tank is passed through precipitation by metallic ion pond, the acid solution of precipitation by metallic ion pond discharge is passed through acid storage tank.The present invention, after jacket heat-exchanger cools down acid vapors, it is passed through in acid storage tank, precipitation by metallic ion pond precipitation separating metal ions, and corresponding acid solution is discharged into acid storage tank, it is ready to be reused.
Description
Technical field
The present invention relates to the Carbon nanotube purification system of precipitate metal ion, belongs to CNT production technical field.
Background technology
CNT is a kind of tubular nanometer material being made up of carbon atom.Tube wall contains multilayer carbon atom and is referred to as more walls
CNT（MWNT）, it is referred to as single-walled carbon nanotube containing single layer of carbon atom（SWNT）.CNT 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 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 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 CNT.One outstanding advantages of this method are that Residual reactants are gas, may exit off reaction
System, the higher CNT of purity is obtained, while temperature also need not be very high, comparatively 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 CNT in pipe.
The technique that metal impurities are removed from CNT is referred to as purifying.CNT can produce during purification reaction
Acid mist and spent acid.At present, acid mist and spent acid not only cause problem of environmental pollution, and increase all without by recycling
Production cost.
Inventor has found by retrieval：Application No. 201510466039.7, entitled CNT method of purification,
The patent discloses a kind of CNT method of purification, and the CNT method of purification mainly includes the following steps that：A, in fixation
After the completion of bed or fluid unit are prepared during CNT or prepared, 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, room temperature is dropped in the protection of inert gas, inert gas is nitrogen and/or argon gas, that is, obtains purity as 99.5%
CNT above.CNT 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, simple to operate, and purification efficiency is high and cost is relatively low, it is adapted to the CNT 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 CNT can be cooled down in reducing gas and/or inert gas without by autoxidation,
The purity of CNT 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 is comprised the steps of：Extracted using soxhlet extraction
Impurity in CNT 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, handling process is simple, processing time is short, eliminates and takes out
Filter, centrifugation etc. process and substantially increase the efficiency of purifying carbon nano-tube；Purification process damaged to caused by CNT it is small, it is pure
CNT after change is heat-resist and has good reactivity and compatibility；And acid can be reclaimed and recycled, greatly
Resource is saved greatly.Although the patent describes the partial impurities removed in CNT 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
In order to solve above-mentioned problem, the invention discloses a kind of Purification of Carbon Nanotubes system of precipitate metal ion
System, its concrete technical scheme are as follows：
The Carbon nanotube purification system of precipitate metal ion, including fluid reaction bed, jacketed type exchanger, acid storage tank, stir
Kettle, precipitation by metallic ion pond and two filter presses are mixed, the fluid reaction bed is used for carbon nanometer tube material powder and acid solution is carried out
The place of reaction, the jacketed type exchanger are used for acid vapors caused by cooling fluid reaction bed, and the acid storage tank is used to deposit
Storage jacketed type exchanger cools down obtained acid solution and the acid solution discharged in filter press and precipitation by metallic ion pond, and the filter press is used
In extruding the liquid in CNT crude product, the stirred tank is used to mix by CNT crude product and with non-oxidizable acid solution
Uniformly, and the impurity metal ion in CNT crude product is rinsed out, the precipitation by metallic ion pond is used for the gold in solution
Category ion precipitation gets off,
The acid vapors of the fluid reaction bed discharge are passed through jacketed type exchanger, the acid of the jacketed type exchanger discharge
Property coolant be passed through acid storage tank, the CNT crude product solution of the fluid reaction bed discharge is by filter press press filtration processing heel row
The acid solution gone out is passed through acid storage tank, and the CNT crude product solution of the filter press discharge is passed through stirred tank, then passed to down
One filter press, obtains finished product CNT, and the solution discharged in the stirred tank is passed through precipitation by metallic ion pond, metal ion
The acid solution of sedimentation basin discharge is passed through acid storage tank.
The jacketed type exchanger includes container, inner bag and chuck, and the inner bag is suspended in container, and the chuck surrounds
Space is left between the bottom of container and surrounding, the chuck and container.
The upper end of the chuck is provided with steam inlet, and the steam inlet and chuck are tangent, under the chuck
End is provided with cooling liquid outlet, and the top of the container is provided with liquid outlet, and the bottom of the container is provided with inlet, described
The bottom of inner bag is provided with the liquid inlet extended to outside chuck, is provided with and is extended to outside chuck at the top of the inner bag
Liquid outlet,
Sour gas from fluid reaction bed is entered in chuck from steam inlet, is formed by the cooling effect of chuck
Coolant, and discharged from cooling liquid outlet, it is passed into acid storage tank, is injected separately into the container and inner bag for cooling jacket
The industry solution of middle gas.
Several heat transfer sheets, the heat transfer sheet connection inner bag and container are provided with the container.
The Surface coating of the jacketed type exchanger has heat-insulation layer.
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 well mixed.
The present invention operation principle be：
The present invention, carbon nanometer tube material powder and acid solution chemically react on fluid reaction bed, generate CNT,
Acid mist can be produced in the course of reaction, is directly discharged in air, not only pollutes environment, while wastes industrial chemicals, by acid mist
It is passed into jacketed type exchanger, acid mist is cooled to acid solution, then the acid solution is passed into acid storage tank, adjusts in acid storage tank
The PH of acid solution, you can reuse.
The CNT crude product solution generated on fluid reaction bed is input to filter press, and the acid solution of filter press extrusion is transported to
Acid storage tank.Handle to obtain filter cake by filter press, then the filter cake is put into stirred tank, add non-oxidizing acid, carbon is received
The impurity metal ion on mitron crude product surface rinses out, and the acid solution containing metal ion emitted in stirred tank is passed into gold
Belong in ion precipitation pond, precipitation by metallic ion therein is got off, then acid solution is discharged into acid storage tank, treats that industry makes again
With.
The beneficial effects of the invention are as follows：
1. the present invention, the acid vapors obtained from fluid reaction bed, after being cooled down by jacket heat-exchanger, is passed through acid storage tank
In, used after being directly adjusted pH value, the total acid solution of CNT crude product solution after filter press and stirred tank also by
Recycle；
2. of the invention, the container in jacketed type exchanger is internally provided with inner bag, with heat transfer between inner bag and container inner wall
Piece is connected, and the heat energy on container is quickly delivered on inner bag by heat transfer sheet, increases the heat exchange efficiency of container, meanwhile, it is capable to
Two kinds of different industry solutions are added in container and inner bag, requirement of two kinds of industry solutions to temperature is different, allows two kinds of solution to lead to
Corresponding container and inner bag are crossed, is warming up to corresponding temperature, improves heat utilization rate；
3. the present invention, the metal ion of CNT crude product solution is separated by adding non-oxidizing acid in stirred tank,
CNT is purified, obtains the higher CNT of purity, meanwhile, the acid solution discharged from stirred tank is passed into metal ion and sunk
Shallow lake pond, it is discharged into after precipitation by metallic ion therein, then by acid solution in acid storage tank, it is ready to be reused；
4. 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 well mixed, and is advantageous to the PH of accurate adjustment acid solution；
5. the present invention, the Surface coating of jacketed type exchanger has a heat-insulation layer, and the heat energy in acid vapors in chuck is abundant
By the liquid absorption in container, the heat utilization rate in sour gas is fully improved, avoids industrial heat energy from wasting.
Brief description of the drawings
Fig. 1 is the connection relationship diagram of the present invention,
Fig. 2 is the structural representation of the jacketed type exchanger of the present invention,
Reference numerals list：1-liquid outlet, 2-liquid outlet, 3-container, 4-steam inlet, 5-chuck, 6-
Heat transfer sheet, 7-inner bag, 8-liquid inlet, 9-inlet, 10-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 limitation the scope of the present invention.
Fig. 1 be the present invention connection relationship diagram, the Purification of Carbon Nanotubes of this precipitate metal ion visible with reference to accompanying drawing
System, including fluid reaction bed, jacketed type exchanger, acid storage tank, stirred tank, precipitation by metallic ion pond and two filter presses, institute
The place that fluid reaction bed is used for carbon nanometer tube material powder and acid solution is reacted is stated, the jacketed type exchanger is used to cool down
Acid vapors caused by fluid reaction bed, the acid storage tank are used to store acid solution and filter press that jacketed type exchanger cools down to obtain
And the acid solution discharged in precipitation by metallic ion pond, the filter press are used to extrude the liquid in CNT crude product, the stirring
Kettle is used to be well mixed by CNT crude product and with non-oxidizable acid solution, and rinse out the metal in CNT crude product from
Sub- impurity, the precipitation by metallic ion pond are used to get off the precipitation by metallic ion in solution.
The acid vapors of the fluid reaction bed discharge are passed through jacketed type exchanger, the acid of the jacketed type exchanger discharge
Property coolant be passed through acid storage tank, the CNT crude product solution of the fluid reaction bed discharge is by filter press press filtration processing heel row
The acid solution gone out is passed through acid storage tank, and the CNT crude product solution of the filter press discharge is passed through stirred tank, then passed to down
One filter press, obtains finished product CNT, and the solution discharged in the stirred tank is passed through precipitation by metallic ion pond, metal ion
The acid solution of sedimentation basin discharge is passed through acid storage tank.The present invention, acid vapors are cooled down using the heat exchanger of chuck 5, reclaim heat energy and acid solution,
Precipitated using precipitation by metallic ion pond from the metal ion in the acid solution in stirred tank.
Fig. 2 be the present invention jacketed type exchanger structural representation, the jacketed type exchanger bag visible with reference to accompanying drawing
Container 3, inner bag 7 and chuck 5 are included, the inner bag 7 is suspended in container 3, and the chuck 5 is enclosed in bottom and the surrounding of container 3,
Space is left between the chuck 5 and container 3.Demand according to industry solution to temperature, by the molten of two kinds of different temperatures demands
Liquid is each led into inner bag 7 and container 3, is heated to the temperature of demand.
The upper end of the chuck 5 is provided with steam inlet 4, and the steam inlet 4 and chuck 5 are tangent, the chuck 5
Lower end be provided with cooling liquid outlet 10, the top of the container 3 is provided with liquid outlet 1, the bottom of the container 3 be provided with into
Liquid mouth 9, the bottom of the inner bag 7 are provided with the liquid inlet 8 for extending to the outside of chuck 5, and the top of the inner bag 7 is provided with
Extend to the liquid outlet 2 of the outside of chuck 5.
Sour gas from fluid reaction bed is entered in chuck 5 from steam inlet 4, passes through the cooling effect of chuck 5
Coolant is formed, and is discharged from cooling liquid outlet 10, is passed into acid storage tank, is injected separately into and is used in the container 3 and inner bag 7
The industry solution of gas in cooling jacket 5.
Several heat transfer sheets 6 are provided with the container 3, the heat transfer sheet 6 connects inner bag 7 and container 3.The energy of heat transfer sheet 6
It is enough that heat energy on container 3 is delivered on inner bag 7, increase heat transfer rate.
The Surface coating of the jacketed type exchanger has heat-insulation layer.The heat energy in acid vapors in chuck 5 is fully held
Liquid absorption in device 3, the heat utilization rate in sour gas is fully improved, avoids industrial heat energy from wasting.
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 well mixed.In the presence 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.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, in addition to
Formed technical scheme 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 (6)
1. the Carbon nanotube purification system of precipitate metal ion, it is characterized in that including fluid reaction bed, jacketed type exchanger, acid storage
Tank, stirred tank, precipitation by metallic ion pond and two filter presses, the fluid reaction bed are used for carbon nanometer tube material powder and acid solution
The place reacted, the jacketed type exchanger are used for acid vapors caused by cooling fluid reaction bed, and the acid storage tank is used
Obtained acid solution and the acid solution discharged in filter press and precipitation by metallic ion pond, the press filtration are cooled down in storage jacketed type exchanger
Machine is used to extruding liquid in CNT crude product, the stirred tank be used for by CNT crude product and with non-oxidizable acid solution
It is well mixed, and the impurity metal ion in CNT crude product is rinsed out, the precipitation by metallic ion pond is used in solution
Precipitation by metallic ion get off,
The acid vapors of the fluid reaction bed discharge are passed through jacketed type exchanger, and the jacketed type exchanger is discharged acid cold
But liquid is passed through acid storage tank, what the CNT crude product solution that the fluid reaction bed is discharged was discharged after filter press press filtration processing
Acid solution is passed through acid storage tank, and the CNT crude product solution of the filter press discharge is passed through stirred tank, then passed to next
Filter press, obtains finished product CNT, and the solution discharged in the stirred tank is passed through precipitation by metallic ion pond, precipitation by metallic ion
The acid solution of pond discharge is passed through acid storage tank.
2. the Carbon nanotube purification system of precipitate metal ion according to claim 1, it is characterized in that the jacket type changes
Hot device includes container, inner bag and chuck, and the inner bag is suspended in container, and the chuck is enclosed in bottom and the surrounding of container,
Space is left between the chuck and container.
3. the Carbon nanotube purification system of precipitate metal ion according to claim 2, it is characterized in that the chuck is upper
End is provided with steam inlet, and the steam inlet and chuck are tangent, and the lower end of the chuck is provided with cooling liquid outlet, the appearance
The top of device is provided with liquid outlet, and the bottom of the container is provided with inlet, and the bottom of the inner bag, which is provided with, extends to folder
The liquid inlet of outside is covered, the liquid outlet extended to outside chuck is provided with the top of the inner bag,
Sour gas from fluid reaction bed is entered in chuck from steam inlet, and cooling is formed by the cooling effect of chuck
Liquid, and discharged from cooling liquid outlet, it is passed into acid storage tank, is injected separately into the container and inner bag for gas in cooling jacket
The industry solution of body.
4. the Carbon nanotube purification system of precipitate metal ion according to claim 3, it is characterized in that being set in the container
It is equipped with several heat transfer sheets, the heat transfer sheet connection inner bag and container.
5. the Carbon nanotube purification system of precipitate metal ion according to claim 1, it is characterized in that the jacket type changes
The Surface coating of hot device has heat-insulation layer.
6. the Carbon nanotube purification system of precipitate metal ion according to claim 1, it is characterized in that in the acid storage tank
Air pump is provided with, the air pump conveys air into acid storage tank from the bottom of acid storage tank, for the acid solution in acid storage tank to be mixed
Uniformly.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100080748A1 (en) * | 2008-09-30 | 2010-04-01 | Joo Hee Han | Continuous method and apparatus of purifying carbon nanotubes |
| CN104176723A (en) * | 2014-08-07 | 2014-12-03 | 无锡东恒新能源科技有限公司 | Small-tube-diameter carbon nano-tube purification device and small-tube-diameter carbon nano-tube purification method |
| CN206033244U (en) * | 2016-08-31 | 2017-03-22 | 无锡东恒新能源科技有限公司 | Deposit metal ion's carbon nanotube purification system |
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- 2016-08-31 CN CN201610763581.3A patent/CN106167259B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100080748A1 (en) * | 2008-09-30 | 2010-04-01 | Joo Hee Han | Continuous method and apparatus of purifying carbon nanotubes |
| CN104176723A (en) * | 2014-08-07 | 2014-12-03 | 无锡东恒新能源科技有限公司 | Small-tube-diameter carbon nano-tube purification device and small-tube-diameter carbon nano-tube purification method |
| CN206033244U (en) * | 2016-08-31 | 2017-03-22 | 无锡东恒新能源科技有限公司 | Deposit metal ion's carbon nanotube purification system |
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