CN106365147A - Carbon nano tube purification system for acid recovery - Google Patents
Carbon nano tube purification system for acid recovery Download PDFInfo
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- CN106365147A CN106365147A CN201610768316.4A CN201610768316A CN106365147A CN 106365147 A CN106365147 A CN 106365147A CN 201610768316 A CN201610768316 A CN 201610768316A CN 106365147 A CN106365147 A CN 106365147A
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Abstract
A carbon nano tube purification system for acid recovery comprises a fluid reaction bed, a heat exchanger, a pure acid storage tank, a heteroacid storage tank, a grinding machine and two filter presses, wherein acid vapor discharged by the fluid reaction bed, is led to the heat exchanger, acid cooling liquid discharged by the heat exchanger is led to the pure acid storage tank, a carbon nano tube crude product discharged by the fluid reaction bed is led to one filter press, an acid solution discharged by the filter press is led to the heteroacid storage tank, the carbon nano tube crude product discharged by the filter press is led to the grinding machine and then is led to the next filter press, and a finished product carbon nano tube is obtained. According to the carbon nano tube purification system, the acid vapor obtained from the fluid reaction bed is cooled through the heat exchanger, then is led to the pure acid storage tank and can be directly used after a PH value is regulated, and the acid in the carbon nano tube crude product from the fluid reaction bed contains a metal catalyst and other impurities and ihs led to the heteroacid storage tank, and metal ions and acid liquid to be separated are used respectively.
Description
Technical field
The present invention relates to the CNT purification system of recovery acid, 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), is referred to as SWCN (swnt) containing monolayer carbon atom.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 comprises the 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 is also found that Application No. 201210476918.4, a kind of invention entitled purified carbon nanometer through retrieval
The method of pipe, the invention discloses a kind of method of purifying carbon nano-tube, it is comprised the steps of and is 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 of recovery acid, its tool
Body technique scheme is as follows:
The CNT purification system of recovery acid, including fluid reaction bed, heat exchanger, pure acid storage tank, heteroacid storage tank, 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
The acid vapors producing for cooling fluid reaction bed, described pure acid storage tank is used for storing the acid solution that heat exchanger cooling obtains, institute
State heteroacid storage tank and be used for extruding in CNT crude product for storing the acid solution discharged in pressure filter and grinder, described pressure filter
Liquid, described grinder is used for mixing homogeneously by CNT crude product with non-oxidizable acid solution, and rinses out carbon nanometer
Metal impurities in pipe crude product,
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 pure 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
Heteroacid storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, then passes to next pressure filter, obtains finished product
CNT.
It is provided with air pump, described air pump conveys sky from the bottom of pure acid storage tank is to pure acid storage tank in described pure acid storage tank
Gas, for by the acid solution mix homogeneously in pure 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 stretch out from the top of container, described central actuating shaft surrounding is provided with auger leaf, institute
State the top that auger leaf is threaded to container from the bottom of container, described auger leaf offers several through holes, described
Through hole is distributed horizontally on auger leaf.
Described auger leaf is divided longitudinally into some sections, leaves space between the auger leaf of adjacent segment.
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 pure acid storage tank, the acid solution in adjustment acid storage tank
Ph, you 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 transported to heteroacid
Storage tank, treats industrial abstract metal ion therein, reuses, and meanwhile, also isolates purer acid, treats industrial application.Warp
Cross pressure filter and process and obtain filter cake, then this filter cake is put in grinder, add non-oxidizing acid, by CNT crude product table
The metal impurities in face rinse out, and this acid solution is also passed in acid storage tank, treat industrial application again.
The invention has the beneficial effects as follows:
1. the present invention, the acid vapors obtaining from fluid reaction bed, acid purity therein is high, after being cooled down by heat exchanger, leads to
Enter in pure acid storage tank, use after being directly adjusted ph value, and in the acid in CNT crude product solution on fluid reaction bed
Containing impurity such as metallic catalysts, direct is the acid solution containing metal impurities by the liquid that pressure filter is extruded, and is passed through heteroacid storage
Tank, metal ion to be separated and acid solution；
2. 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；
3. the present invention, in auger leaf rotary course, liquid is stirred rotation by auger leaf, promotes towards chamber wall flowing,
Liquid passes through through hole, forms turbulent flow, allows liquid sufficient heat exchange in flow process；
4. 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；
5. 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.
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 spirals
Paddle, 7 inlets, 8 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 system of this recovery acid,
Including fluid reaction bed, heat exchanger, pure acid storage tank, heteroacid storage tank, 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 acid steaming that cooling fluid reaction bed produces
Vapour, described pure acid storage tank is used for storing the acid solution that heat exchanger cooling obtains, and described heteroacid storage tank is used for storing pressure filter and grinding
The acid solution discharged in machine, described pressure filter is used for extruding the liquid in CNT crude product, and described grinder is used for carbon nanometer
Pipe crude product and mixing homogeneously with non-oxidizable acid solution, and rinse out the metal impurities in CNT crude product.
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
Pure acid storage tank, the CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, the acid solution that described pressure filter is discharged
It is passed through heteroacid storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, then passes to next pressure filter, obtain
Finished product CNT.The present invention, the purity according to acid solution collects acid solution respectively, is discharged into pure acid storage tank after acid vapors cooling
In, the acid solution containing impurity is discharged in heteroacid storage tank.
It is provided with air pump, described air pump conveys sky from the bottom of pure acid storage tank is to pure acid storage tank in described pure acid storage tank
Gas, for by the acid solution mix homogeneously in pure acid storage tank.In the presence of air stream, air stream has to the acid solution in pure acid storage tank
Agitate effect, acid solution is in continuous turbulence state, be conveniently adjusted and obtain 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 8, the top of described container 3 is provided with liquid outlet 2, and the bottom of described container 3 is provided with inlet 7.
Sour gas from fluid reaction bed enters into chuck 5 from steam inlet 4, by the cooling effect of chuck 5
Form coolant, and discharge from cooling liquid outlet 8, be passed in acid storage tank, inject in cooling jacket 5 in described container 3
The solution of gas, the bottom liquid inlet mouth 7 of the solution from container 3 in described container 3 enters, from liquid outlet 2 row at container 3 top
Go out.Be cooled into liquid from the acid vapors of fluid reaction bed, the heat in steam is absorbed by liquid in container 3, steam with
Liquid flow direction in container 3 is contrary, improves 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 spiral and stirs
Mix leaf 6, described auger leaf 6 is threaded to the top of container 3 from the bottom of container 3, described auger leaf 6 offers some
Individual through hole, described through hole is distributed horizontally on auger leaf 6.Liquid agitation in container 3 can be flowed by auger leaf 6
Come, liquid internal carries out heat exchange, it is to avoid high near the temperature of liquid of container 3 wall, the temperature of liquid near container 3 center is low,
Allow the liquid in container 3 can fully absorb heat energy.
Described auger leaf 6 is divided longitudinally into some sections, leaves space between the auger leaf 6 of adjacent segment.Avoid liquid
Body inertia flows, and liquid interrupts inertia flowing in space, strengthens the scrambling that in container 3, liquid flows, and allows in container 3
Liquid internal heat energy is 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 leads to
Over-driving device connects motor.Avoid heat 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 heat energy in steam is just fully
Absorbed by the liquid in container 3.
Described inlet 7 and cooling liquid outlet 8 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. the CNT purification system of recovery acid, is characterized in that including fluid reaction bed, heat exchanger, pure acid storage tank, heteroacid storage
Tank, 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 acid vapors that cooling fluid reaction bed produces, and described pure acid storage tank is used for storing heat exchanger and cooling down obtaining
Acid solution, described heteroacid storage tank is used for storing the acid solution discharged in pressure filter and grinder, and described pressure filter receives for extruded carbon
Liquid in mitron crude product, described grinder is used for mixing homogeneously by CNT crude product with non-oxidizable acid solution, and rushes
Wash the metal impurities in CNT crude product off,
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 pure 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
Heteroacid storage tank, the CNT crude product that described pressure filter is discharged is passed through grinder, then passes to next pressure filter, obtains finished product
CNT.
2. the CNT purification system of recovery acid according to claim 1, is characterized in that setting in described pure acid storage tank
There is air pump, described air pump conveys air from the bottom of pure acid storage tank is to pure acid storage tank, for mixing the acid solution in pure acid storage tank
Close uniformly.
3. the CNT purification system of recovery acid according to claim 1, is characterized in that chuck selected by described heat exchanger
Formula heat exchanger, described jacketed type exchanger includes container and chuck, and described chuck is enclosed in bottom and the surrounding of container, described folder
Space is left, the upper end of described chuck is provided with steam inlet, and the lower end of described chuck is provided with coolant between set and container
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 of recovery acid according to claim 3, is characterized in that being provided with described container and stirs
Mix device, described agitating device includes central actuating shaft, described central actuating shaft penetrates chuck and extend in container, and calmly
The top of device is stretched out, and described central actuating shaft surrounding is provided with auger leaf, and described auger leaf is from the bottom spiral shell of container
It is screwed into the top of container, described auger leaf offers several through holes, and described through hole is distributed horizontally on auger leaf.
5. the CNT purification system of recovery acid according to claim 4, is characterized in that described auger leaf longitudinally
It is divided into some sections, between the auger leaf of adjacent segment, leave space.
6. the CNT purification system of recovery acid according to claim 3, is characterized in that described heat exchanger fills in ground
Under, described steam inlet is flushed with ground, and the top of described central actuating shaft is connected via drive motor.
7. the CNT purification system of recovery acid according to claim 4, is characterized in that described inlet and coolant
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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610768316.4A CN106365147A (en) | 2016-08-31 | 2016-08-31 | Carbon nano tube purification system for acid recovery |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610768316.4A CN106365147A (en) | 2016-08-31 | 2016-08-31 | Carbon nano tube purification system for acid recovery |
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| CN106365147A true CN106365147A (en) | 2017-02-01 |
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Citations (7)
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|---|---|---|---|---|
| CN1277146A (en) * | 1999-06-15 | 2000-12-20 | 李铁真 | Method for purifying carbon nanometre tube in large scale |
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| CN101780951A (en) * | 2010-03-09 | 2010-07-21 | 北京大学 | Purification method for obtaining high-purity carbon nano tube |
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| CN104211042A (en) * | 2014-08-07 | 2014-12-17 | 无锡东恒新能源科技有限公司 | Method for removing metal impurities from carbon nano tube |
| CN104310375A (en) * | 2014-10-09 | 2015-01-28 | 清华大学 | Method for removing carbon impurities in single-walled carbon nanotube |
| CN206089045U (en) * | 2016-08-31 | 2017-04-12 | 无锡东恒新能源科技有限公司 | Carbon nanotube purification system of recovered acid |
-
2016
- 2016-08-31 CN CN201610768316.4A patent/CN106365147A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1277146A (en) * | 1999-06-15 | 2000-12-20 | 李铁真 | Method for purifying carbon nanometre tube in large scale |
| CA2681292A1 (en) * | 2008-09-30 | 2010-03-30 | Hanwha Chemical Corporation | Continuous method and apparatus of purifying carbon nanotubes |
| CN101780951A (en) * | 2010-03-09 | 2010-07-21 | 北京大学 | Purification method for obtaining high-purity carbon nano tube |
| 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 |
| CN104211042A (en) * | 2014-08-07 | 2014-12-17 | 无锡东恒新能源科技有限公司 | Method for removing metal impurities from carbon nano tube |
| CN104310375A (en) * | 2014-10-09 | 2015-01-28 | 清华大学 | Method for removing carbon impurities in single-walled carbon nanotube |
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Non-Patent Citations (1)
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