CN106167258A - Pipe with small pipe diameter CNT purification system - Google Patents

Pipe with small pipe diameter CNT purification system Download PDF

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Publication number
CN106167258A
CN106167258A CN201610763523.0A CN201610763523A CN106167258A CN 106167258 A CN106167258 A CN 106167258A CN 201610763523 A CN201610763523 A CN 201610763523A CN 106167258 A CN106167258 A CN 106167258A
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China
Prior art keywords
pipe
pipe diameter
container
storage tank
passed
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Pending
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CN201610763523.0A
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Chinese (zh)
Inventor
沈宇栋
顾灵锋
程阳
张晓�
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Wuxi Dongheng New Energy Technology Co Ltd
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Wuxi Dongheng New Energy Technology Co Ltd
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Priority to CN201610763523.0A priority Critical patent/CN106167258A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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Abstract

Pipe with small pipe diameter CNT purification system, it is characterized in that including fluid reaction bed, heat exchanger, acid storage tank, grinder and two pressure filter, described fluid reaction bed expellant gas is passed through heat exchanger, the acid coolant that described heat exchanger is discharged is passed through acid storage tank, the pipe with small pipe diameter CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, the acid solution that described pressure filter is discharged is passed through acid storage tank, the pipe with small pipe diameter CNT crude product that described pressure filter is discharged is passed through grinder, pipe with small pipe diameter CNT crude product after described grinder grinds is passed through next pressure filter, obtain finished product pipe with small pipe diameter CNT.The present invention, acid solution is recovered, and treats industrial application again, it is to avoid the wasting of resources.

Description

Pipe with small pipe diameter CNT purification system
Technical field
The present invention relates to pipe with small pipe diameter CNT purification system, 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 Directly structure and excellent performance with its uniqueness are paid close attention to by researcher.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 be 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 be Residual reactants be gas, may exit off reaction System, obtains the CNT that purity is higher, and temperature also need not the highest simultaneously, saves energy comparatively speaking.But, CVD Method need to use transition-metal catalyst, if Fe, Co, Ni and alloy etc. thereof are as catalyst.This causes prepared carbon nanometer Often containing the metal impurities of high level in pipe, the existence 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 the most through recycling, not only do not cause problem of environmental pollution, and increase Production cost.
Inventor finds through retrieval: Application No. 201510466039.7, invention entitled CNT method of purification, The open a kind of CNT method of purification of this patent, described CNT method of purification mainly comprises the steps that a, fixing During CNT prepared by bed or fluid unit or after prepare, it is passed through reducing gas and/or noble gas, 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, the protection at noble gas drops to room temperature, and noble gas is nitrogen and/or argon, and i.e. 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, the advantages such as purification efficiency is high and cost is relatively low, the CNT being suitable for industrial mass purifies.But In this patent, after being passed through noble gas, can not fully the oxidizing gas in fixed bed or fluid unit all be got rid of Go out, in fact, be difficult to accomplish that CNT can cool down in reducing gas and/or noble gas and not by autoxidation, cause The purity of CNT does not reaches more than 99.5%.
Inventor is also found that Application No. 201210476918.4, invention entitled a kind of purified carbon nanometer through retrieval The method of pipe, a kind of method that the invention discloses purifying carbon nano-tube, it comprises the steps of and utilizes soxhlet extraction to extract Impurity in CNT crude product: first extract by acid with strong oxidizing property, then use deionized water extraction.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, process that technique is simple, it is short to process the time, eliminate and take out Filter, the process such as centrifugal and substantially increase the efficiency of purifying carbon nano-tube;The damage that CNT is caused by purification process 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 removed in CNT crude product, but has no mention of how Separate the impurity in acid with strong oxidizing property and deionized water, it can be reused, is unfavorable for that industrial mass production is applied.
Summary of the invention
In order to solve the problem of above-mentioned existence, the invention discloses a kind of pipe with small pipe diameter CNT purification system, it is concrete Technical scheme is as follows:
Pipe with small pipe diameter CNT purification system, including fluid reaction bed, heat exchanger, acid storage tank, grinder and two pressure filter, institute Stating the place that fluid reaction bed carries out reacting for pipe with small pipe diameter carbon nanometer tube material powder and acid solution, described heat exchanger is used for cooling down The sour gas that fluid reaction bed produces, acid solution and pressure filter that described acid storage tank obtains for storing heat exchanger cooling squeeze The acid solution pressed out, described pressure filter is for extruding the liquid in pipe with small pipe diameter CNT crude product, and described grinder is used for will Pipe with small pipe diameter CNT crude product and mixed solution mix homogeneously,
Described fluid reaction bed expellant gas is passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through acid storage tank, The pipe with small pipe diameter 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 pipe with small pipe diameter CNT crude product that described pressure filter is discharged is passed through grinder, the pipe with small pipe diameter after the grinding of described grinder CNT crude product is passed through next pressure filter, obtains finished product pipe with small pipe diameter CNT.
Being provided with air pump in described acid storage tank, described air pump carries air from the bottom of acid storage tank to acid storage tank, is used for 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 Being trapped among bottom and the surrounding of container, leave space between described chuck and container, 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, and the bottom of described container is arranged 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, described container injects the solution of 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.
Being provided with agitating device, described agitating device central actuating shaft in described container, described central actuating shaft penetrates Chuck extend in container, and stretches out from the top of container, and described central actuating shaft surrounding is provided with several paddles, some Individual described paddle is evenly distributed on the horizontal surrounding of central actuating shaft, described paddle central actuating shaft longitudinal direction in Rectangular patch, described paddle offers several circular holes, and described circular hole is covered with the paddle of correspondence.
Described paddle has several at the longitudinal direction of central actuating shaft, and longitudinally adjacent paddle mutually staggers, The most at grade.
Described heat exchanger fills in underground, and described steam inlet flushes with ground, and the top of described central actuating shaft is passed through Driving means connects motor.
Described inlet and cooling liquid outlet are positioned at around the bottom of central actuating shaft, and described liquid outlet is positioned at centre-driven The side, top of axle.
The operation principle of the present invention is:
The present invention, there is chemical reaction, generates pipe with small pipe diameter in pipe with small pipe diameter carbon nanometer tube material powder and acid solution on fluid reaction bed CNT, can produce acid mist, be directly discharged in air in this course of reaction, not only pollute environment, and waste chemical industry is former simultaneously Material, is passed into acid mist in heat exchanger, acid mist is cooled to acid solution, then this acid solution is passed in acid storage tank, adjust acid storage tank In the PH of acid solution, can reuse.
The pipe with small pipe diameter CNT crude product generated on fluid reaction bed is input to pressure filter, and the acid solution of pressure filter extrusion is the most defeated Deliver to acid storage tank, treat that industry reuses.Process through pressure filter and obtain filter cake, then this filter cake is put in grinder, adds Entering non-oxidizing acid, rinsed out by the metal impurities on pipe with small pipe diameter CNT crude product surface, this acid solution is also passed in acid storage tank, Treat industrial application again.After grinder obtains the removal of impurity, the cleanest pipe with small pipe diameter CNT.
The invention has the beneficial effects as follows:
1. the present invention, acid solution is recovered, and treats industrial application again, it is to avoid the wasting of resources;
2. the present invention, is provided with air pump in acid storage tank, and air pump carries air from the bottom of acid storage tank to acid storage tank, can acid be stored up Acid solution mix homogeneously in tank, is conducive to accurately adjusting the PH of acid solution;
3. the present invention, heat exchanger fills the earth heat exchanger around underground, heat exchanger 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;
4. 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 The liquid touched, 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;
5. the present invention, paddle is provided with circular hole, and in paddle rotary course, liquid passes from circular hole, forms turbulent flow, liquid When body passes from the circular hole of next paddle, to again change direction, and liquid is stirred leaf and promotes towards chamber wall flowing, Liquid flowing is more uniform.
Accompanying drawing explanation
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,
Fig. 3 be the A-A of the jacketed type exchanger of the present invention to cross sectional view,
Reference numerals list: 1 central actuating shaft, 2 liquid outlets, 3 containers, 4 steam inlets, 5 chucks, 6 stirrings Leaf, 7 circular holes, 8 inlets, 9 cooling liquid outlets.
Detailed description of the invention
Below in conjunction with the accompanying drawings and detailed description of the invention, it is further elucidated with the present invention.It should be understood that following detailed description of the invention is 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, this pipe with small pipe diameter CNT purification system, bag Including fluid reaction bed, heat exchanger, acid storage tank, grinder and two pressure filter, described fluid reaction bed is used for pipe with small pipe diameter carbon nanometer Pipe material powder and acid solution carry out the place reacted, and described heat exchanger is for cooling down the sour gas that fluid reaction bed produces, institute Stating acid storage tank for the acid solution storing the heat exchanger acid solution that obtains of cooling and pressure filter squeezes out, described pressure filter is used Liquid in extruding pipe with small pipe diameter CNT crude product, described grinder is for by pipe with small pipe diameter CNT crude product and mixed Solution mix homogeneously.
Described fluid reaction bed expellant gas is passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through acid storage Tank, the pipe with small pipe diameter CNT crude product that described fluid reaction bed is discharged is passed through pressure filter, the acid solution that described pressure filter is discharged Being passed through acid storage tank, the pipe with small pipe diameter CNT crude product that described pressure filter is discharged is passed through grinder, described grinder grind after little Caliber CNT crude product is passed through next pressure filter, obtains finished product pipe with small pipe diameter 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, in pressure filter extrusion pipe with small pipe diameter CNT crude product Acid solution, grinder cleans the impurity removed on pipe with small pipe diameter CNT crude product.
Being provided with air pump in described acid storage tank, described air pump carries air from the bottom of acid storage tank to acid storage tank, is used for By the acid solution mix homogeneously in acid storage tank.Under the effect of air stream, the acid solution in acid storage tank is agitated effect by air stream, acid Liquid is in continuous turbulence state, it is simple to adjusts and obtains accurate pH value.
Fig. 2 is the structural representation of the jacketed type exchanger of the present invention, and Fig. 3 is the A-A of the jacketed type exchanger of the present invention To cross sectional view, visible in conjunction with accompanying drawing, jacketed type exchanger selected by described heat exchanger, and described jacketed type exchanger includes container 3 With chuck 5, described chuck 5 is enclosed in bottom and the surrounding of container 3, leaves space, described folder between described chuck 5 and container 3 The upper end of set 5 is provided with steam inlet 4, and the lower end of described chuck 5 is provided with cooling liquid outlet 9, and the top of described container 3 is arranged Having liquid outlet 2, the bottom of described container 3 to be provided with inlet 8, chuck 5 cools down for steam, places cooling solution in container 3.
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 9, be passed in acid storage tank, described container 3 injects in cooling jacket 5 The solution of gas, the bottom liquid inlet mouth 8 of the solution from container 3 in described container 3 enters, from liquid outlet 2 row at container 3 top Go out.Steam is cooled into liquid, and the heat in steam is absorbed by liquid in container 3, and steam flows to phase with the liquid in container 3 Instead, heat exchanger effectiveness is improved.
Being provided with agitating device, described agitating device central actuating shaft 1 in described container 3, described central actuating shaft 1 runs through Crossing 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 stirrings Leaf 6, several described paddles 6 are evenly distributed on the horizontal surrounding of central actuating shaft 1, and described paddle 6 is at central actuating shaft 1 The rectangular lamellar of longitudinal direction, described paddle 6 offers several circular holes 7, described circular hole 7 be covered with correspondence paddle 6.Liquid agitation in container 3 can be flowed by paddle 6, and liquid internal carries out heat exchange, it is to avoid near the liquid of container 3 wall Temperature is high, and the temperature of liquid near container 3 center is low, allows the liquid in container 3 can fully absorb heat energy.
Described paddle 6 has several at the longitudinal direction of central actuating shaft 1, and longitudinally adjacent paddle 6 mutually mistake Open, the most at grade.Strengthen the scrambling of liquid flowing in container 3, allow the liquid internal heat energy in container 3 fully divide Dissipate uniformly.
Described heat exchanger fills in underground, and described steam inlet 4 flushes with ground, and the top of described central actuating shaft 1 leads to Over-driving device connects motor.Avoid the heat energy in heat exchanger by diffusion in atmosphere, be solid around soil 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 the most fully Absorbed by the liquid in container 3.
Described inlet 8 and cooling liquid outlet 9 are positioned at around the bottom of central actuating shaft 1, and described liquid outlet 2 is positioned at center The side, top of drive shaft 1.Guarantee that central actuating shaft 1 passes from the longitudinal center of chuck 5 heat exchanger.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also includes 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 can carry out various change and amendment 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. pipe with small pipe diameter CNT purification system, is characterized in that including fluid reaction bed, heat exchanger, acid storage tank, grinder and two Individual pressure filter, described fluid reaction bed carries out the place reacted for pipe with small pipe diameter carbon nanometer tube material powder and acid solution, described in change Hot device is for cooling down the sour gas that fluid reaction bed produces, and 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 for extruding the liquid in pipe with small pipe diameter CNT crude product, described Grinder is used for pipe with small pipe diameter CNT crude product and mixed solution mix homogeneously,
Described fluid reaction bed expellant gas is passed through heat exchanger, and the acid coolant that described heat exchanger is discharged is passed through acid storage tank, The pipe with small pipe diameter 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 pipe with small pipe diameter CNT crude product that described pressure filter is discharged is passed through grinder, the pipe with small pipe diameter after the grinding of described grinder CNT crude product is passed through next pressure filter, obtains finished product pipe with small pipe diameter CNT.
Pipe with small pipe diameter CNT purification system the most according to claim 1, is characterized in that being provided with gas in described acid storage tank Pump, described air pump carries air from the bottom of acid storage tank to acid storage tank, for by the acid solution mix homogeneously in acid storage tank.
Pipe with small pipe diameter CNT purification system the most according to claim 1, is characterized in that jacket type selected by described heat exchanger Heat exchanger, described jacketed type exchanger includes that container and chuck, described chuck are enclosed in bottom and the surrounding of container, described chuck And leaving space between container, the upper end of described chuck is provided with steam inlet, and the lower end of described chuck is provided with coolant and goes out Mouthful, 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, described container injects the solution of 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.
Pipe with small pipe diameter CNT purification system the most according to claim 3, is characterized in that being provided with stirring in described container Device, described agitating device central actuating shaft, described central actuating shaft penetrates chuck and extend in container, and from the top of container Portion stretches out, and described central actuating shaft surrounding is provided with several paddles, and several described paddles are evenly distributed on center and drive The horizontal surrounding of moving axis, described paddle, in the rectangular lamellar of longitudinal direction of central actuating shaft, described paddle offers Several circular holes, described circular hole is covered with the paddle of correspondence.
Pipe with small pipe diameter CNT purification system the most according to claim 4, is characterized in that described paddle is in centre-driven The longitudinal direction of axle has several, and longitudinally adjacent paddle mutually staggers, the most at grade.
Pipe with small pipe diameter CNT purification system the most according to claim 3, is characterized in that described heat exchanger fills in underground, Described steam inlet flushes with ground, and the top of described central actuating shaft is connected via drive motor.
Pipe with small pipe diameter CNT purification system the most according to claim 4, is characterized in that described inlet and coolant go out Mouth is positioned at around the bottom of central actuating shaft, and described liquid outlet is positioned at the side, top of central actuating shaft.
CN201610763523.0A 2016-08-31 2016-08-31 Pipe with small pipe diameter CNT purification system Pending CN106167258A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
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
CN202898036U (en) * 2012-10-24 2013-04-24 无锡东恒新能源材料有限公司 Carbon nanotube purification system
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
CN204699437U (en) * 2015-04-17 2015-10-14 池州龙华医药化工有限公司 A kind of water cooling crystallization kettle
CN206089046U (en) * 2016-08-31 2017-04-12 无锡东恒新能源科技有限公司 Tubule footpath carbon nanotube purification system

Patent Citations (6)

* Cited by examiner, † Cited by third party
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
CN202898036U (en) * 2012-10-24 2013-04-24 无锡东恒新能源材料有限公司 Carbon nanotube purification system
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
CN204699437U (en) * 2015-04-17 2015-10-14 池州龙华医药化工有限公司 A kind of water cooling crystallization kettle
CN206089046U (en) * 2016-08-31 2017-04-12 无锡东恒新能源科技有限公司 Tubule footpath carbon nanotube purification system

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Application publication date: 20161130