CN104843666A - Device for growth of carbon nano-tube aerogel - Google Patents
Device for growth of carbon nano-tube aerogel Download PDFInfo
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Abstract
The present invention discloses a device for growth of a carbon nano-tube aerogel. The device comprises a main reaction cavity and a collection box, wherein the main reaction cavity is provided with an air inlet and an air outlet formed opposite to the air inlet; the collection box is communicated with the main reaction cavity; at least one secondary reaction cavity communicated with the main reaction cavity is sleeved in the main reaction cavity, the secondary reaction cavities are formed close to the air inlet of the main reaction cavity, and the length of each of the secondary reaction cavities in the axial direction of the main reaction cavity is less than that of the main reaction cavity. Compared with the prior art, the defect that a single reaction cavity is taken as a reaction chamber for the growth of the carbon nano-tube is overcome by virtue of sleeving the secondary reaction cavities in the main reaction cavity, so that not only is continuous and uniform carbon nano-tube aerogel generated, but also the yield of the carbon nano-tube aerogel is greatly improved by enlarging the tube diameter of the reaction chamber. The production cost is saved, the production period is shortened, and the industrial production of the carbon nano-tube aerogel becomes probable.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of device for carbon nano-tube aerogel.
Background technology
Carbon nanotube is in the new texture form of the another kind of carbon of discovery at the beginning of the nineties after C60, for individual layer or Multi-layer graphite pipe nested, interior sky, diameter is the one dimension carbon structure form of a few nanometer or tens nanometers, after finding under adopting high resolution electron microscopy from 1991, just cause great research boom in the whole world, as a kind of novel nano material, because the geometry of its uniqueness and electronic band structure bring excellent mechanical property, electric property, thermal property and electromagnetic performance etc., the performance of these excellences makes carbon nanotube there is application advantage potential greatly.As a kind of tridimensional network be made up of carbon nanotube, carbon nanotube aerogel can prepare carbon nano-tube macroscopic structure very easily by it, if film, thick film, block, macroscopic fiber etc. are compared with the macroscopical form of variform, thus studying carbon nanotube aerogel will have very important promotion meaning to the application of carbon nanotube.The method preparing carbon nanotube at present mainly contains: arc process, laser evaporization method, chemical Vapor deposition process.The current all comparative maturities of these three kinds of methods, can prepare single wall and multi-walled carbon nano-tubes.Chemical Vapor deposition process becomes because equipment is simple, most probable realizes suitability for industrialized production studies to obtain synthetic method the most widely at present.The method of current employing chemical Vapor deposition process carbon nano-tube aerogel mainly adopts an independent silica tube or alundum tube as reaction chamber, then rare gas element or reducing gas is used, also or both mixed gass, the high temperature reaction zone high-temperature catalytic cracking growth of reaction solution being brought into reaction chamber obtains.
What current carbon nano-tube aerogel all adopted is single alundum tube or silica tube growth, and production capacity and continuity low, in raising production capacity and continuity, current employing be the method increasing caliber and tube length, also or use the method for more expensive catalyst instead, complex process and cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of device for carbon nano-tube aerogel that can solve the problems of the technologies described above.
Wherein, the device for carbon nano-tube aerogel comprises:
Main reaction chamber, its air outlet that there is an inlet mouth and be oppositely arranged with described inlet mouth;
Collection box, is connected with the air outlet in described main reaction chamber;
Described main reaction chamber is used for catalysis and generates carbon nanotube aerogel, be provided with the collection device spinning axle and spin described in being arranged on axle in described collection box, described in spin axle can be rotated the carbon nanotube aerogel that catalysis in described main reaction chamber generates is wound on described collection device with driving;
Wherein, the secondary response chamber that at least one is communicated with described main reaction chamber is also arranged with in described main reaction chamber, the inlet mouth of described secondary response chamber near described main reaction chamber is arranged, and is less than the length in described main reaction chamber in the length in the axially described secondary response chamber in described main reaction chamber.
As a further improvement on the present invention, the described device for carbon nano-tube aerogel is included in multiple secondary response chambeies sheathed step by step in the radial direction in described main reaction chamber, and multiple secondary response chamber is from inside to outside set in the radial direction in described main reaction chamber, in described main reaction chamber, length axially and the sectional area in the radial direction of main reaction chamber increase gradually.
As a further improvement on the present invention, in described main reaction chamber, axially complete coated setting is in the inner and adjacent secondary response chamber in arbitrary secondary response chamber.
As a further improvement on the present invention, described main reaction chamber and described secondary response chamber are tubulose, and described main reaction chamber and described secondary response chamber are coaxially arranged.
As a further improvement on the present invention, the one end in described secondary response chamber and the concordant setting of inlet mouth in described main reaction chamber.
As a further improvement on the present invention, there is space between described main reaction chamber and described secondary response chamber, described space adopts insulating cotton to fill.
As a further improvement on the present invention, described main reaction chamber overcoat horizontal electric resistance furnace.
As a further improvement on the present invention, the material in described main reaction chamber and described secondary response chamber is corundum or quartzy or mullite.
As a further improvement on the present invention, the described device for carbon nano-tube aerogel also comprises injection device, and described injection device is selected from the one in syringe pump, liquid ejector, ultrasonic atomizatio injection device.
As a further improvement on the present invention, between described injection device and described main reaction chamber, carbon source inlet and carrier gas inlet is also provided with.
Compared with prior art, the present invention solves the drawback of single reaction chamber as reaction chamber carbon nano-tube by establishing secondary response chamber at main reaction cavity inner sleeve, continuous print, uniform carbon nanotube aerogel can not only be grown, but also the productive rate of carbon nanotube aerogel greatly can be improved by augmenting response room caliber, save production cost, shorten the production time, make the suitability for industrialized production of carbon nanotube aerogel become possibility.
Accompanying drawing explanation
Fig. 1 is the structural representation for the device of carbon nano-tube aerogel in an embodiment of the present invention.
Fig. 2 is the stereoscan photograph of the carbon nanotube aerogel macroscopic view continuum prepared for the device of carbon nano-tube aerogel in an embodiment of the present invention.
Embodiment
Describe the present invention below with reference to embodiment shown in the drawings.But these embodiments do not limit the present invention, the structure that those of ordinary skill in the art makes according to these embodiments, method or conversion functionally are all included in protection scope of the present invention.
Should be appreciated that, used herein such as " on ", " top ", D score, the representation space relative position such as " below " term be describe a unit as shown in the drawings or the feature relation relative to another unit or feature for the object being convenient to illustrate.The term of relative space position can be intended to comprise equipment in the different azimuth used or in work except orientation shown in figure.
Further, although should be understood that term primary and secondary etc. can be used to describe various element or structure in this article, these are described the restriction that object should not be subject to these terms.These terms are only for being distinguished from each other out these description objects.Such as, main reaction chamber can be called as secondary response chamber, and secondary response chamber also can be called as main reaction chamber similarly, and this does not deviate from the protection domain of the application.
Ginseng Fig. 1, introduces an embodiment of the device 100 for carbon nano-tube aerogel of the present invention.Device 100 for carbon nano-tube aerogel comprises a main reaction chamber 11, the collection box 20 be communicated with main reaction chamber 11 and injection device 50, wherein, the air outlet 112 that main reaction chamber 11 comprises an inlet mouth 111 and is oppositely arranged with inlet mouth 111, collection box 20 is connected with the air outlet 112 in main reaction chamber 11.
Inlet mouth 111 place near main reaction chamber 11 in main reaction chamber 11 is also arranged with at least one secondary response chamber 12 be communicated with main reaction chamber 11, and the length in main reaction chamber 11 is less than in the length in the axially secondary response chamber 12 in main reaction chamber 11, main reaction chamber 11 forms telescopic composite reaction chamber 10 together with secondary response chamber 12.
In the present invention, sheathed multiple secondary response chamber 12 step by step in the radial direction thereof in main reaction chamber 11, and multiple secondary response chambeies are from inside to outside set in the radial direction in main reaction chamber 11, in main reaction chamber 11, length axially and the sectional area in the radial direction of main reaction chamber 11 increase gradually.It should be noted that, expression position described in the present invention and the word in direction are all using the axis in main reaction chamber 11 as reference, and in one end of the axis in main reaction chamber 11 is, the one end away from the axis in main reaction chamber 11 is outward.In main reaction chamber 11, axially complete coated setting is in the inner and adjacent secondary response chamber in arbitrary secondary response chamber.Multiple secondary response chamber 12 is all arranged near the inlet mouth 111 in main reaction chamber 11, on from inlet mouth 111 to the direction of air outlet 112, each reaction chamber in telescopic composite reaction chamber 10 increases gradually in the length axially in main reaction chamber 11, and the section area of each reaction chamber in the radial direction of main reaction chamber 11 increases gradually.Namely, the length in multiple secondary response chamber is not identical with its section area diametrically, large secondary response chamber can be set in outside little secondary response chamber, multiple little secondary response chamber is to be enclosed within main reaction chamber 11 in the mode of sleeve, be structure in layer from inside to outside, the telescopic composite reaction chamber 10 combined put into the burner hearth of horizontal electric resistance furnace 30.The benefit of such design is, solve single employing pipe with small pipe diameter or the Large Diameter Pipeline drawback as reaction chamber, the problem of gas air turbulence when entering reaction chamber is solved at the alundum tube of the pipe with small pipe diameter of the leading portion inner sleeve certain length of the alundum tube of Large Diameter Pipeline, ensure that the carbon source reaction solution after vaporization can be continuously, carried by carrier gas equably and enter high temperature reaction zone, simultaneously due to reactant gases stablized by the alundum tube of this section of pipe with small pipe diameter after can be relatively uniform, mild enters into high temperature reaction zone, reactant gases is enable to be evenly distributed in whole high temperature reaction zone, metal catalyst is more easily reduced, thus the higher carbon nanotube of degree of crystallinity can be grown, therefore, reaction chamber front end inner sleeve pipe with small pipe diameter alundum tube can not only play the effect of steady air flow, and the quality of grown carbon nanotube can also be improved.When the reaction solution after vaporization enters the high temperature reaction zone of Large Diameter Pipeline under the carrying of carrier gas, reaction solution is in this region cracking, simultaneously because caliber increases, the area of catalytic pyrolysis carbon source is not only made to increase, growth efficiency improve, and due to the air-flow in reaction process unobstructed, enable carbon nanotube aerogel be moved out of reaction chamber smoothly, not easily block reaction chamber, make to grow the continuity of collecting and be greatly enhanced.
Preferably, main reaction chamber 11 and secondary response chamber 12 are tubulose, and both materials are corundum or quartzy or mullite, and main reaction chamber 11 and each secondary response chamber 12 are all coaxially arranged to ensure that carbon source reaction solution and carrier gas stream pass through smoothly.Especially, the one end in secondary response chamber 12 and the concordant setting of inlet mouth 111 in main reaction chamber 11.
In the present embodiment, the alundum tube of a 60 × 350mm can be enclosed within 120 × 1400mm alundum tube, wherein 120 × 1400mm alundum tube is decided reaction chamber, the alundum tube of 60 × 350mm does secondary response chamber, space insulating cotton between two pipes is filled, ensure that the center of circle of two pipe cross sections overlaps, then, the telescopic composite reaction chamber 10 combined is put into the burner hearth of horizontal electric resistance furnace 30, one end flange 60 of main reaction chamber 11 inlet mouth 111 seals, air outlet 112 is communicated with collection box 20, complete the installation of carbon nano-tube aerogel device 100.Certainly, in other embodiments of the present invention, each reaction chamber also can be other suitable shape.The size Selection of the alundum tube in main reaction chamber 11 and secondary response chamber 12 also can be varied, can select in two of 40 × 350mm and 100 × 1400mm alundum tubes and be nested together, also can select 40 × 350mm, 100 × 700mm, 150 × 1400mm, tri-alundum tubes are nested together in carrying out, to improve the productive rate of carbon nanotube aerogel.
Injection device 50, be used for carbon source reaction solution to inject telescopic composite reaction chamber 10, preferably, injection device 50 can adopt the one in syringe pump, liquid ejector or ultrasonic atomizatio injection device, and injection mode can adopt single tube or multitube to connect or side-by-side configuration.
Between injection device 50 and telescopic composite reaction chamber 10, be also provided with carbon source inlet 41 and carrier gas inlet 42, preferably, carbon source inlet 41 and carrier gas inlet 42 adopt stainless-steel pipe to make.Carbon source reaction solution is injected in telescopic composite reaction chamber 10 by carbon source inlet 41 by injection device 50.Especially, at carrier gas inlet 42, place is also provided with mass-flow gas meter (not shown), is used for controlling to pass into telescopic composite reaction chamber 10 flow of carrier gas.
Collection box 20, comprise a casing and be arranged on and spin axle 21 in casing, the air outlet 112 in main reaction chamber 11 is communicated with a sidewall of the casing of collection box 20.Preferably, casing is provided with air seal set (not shown), air outlet (not shown) and viewing window (not shown).After carbon nanotube aerogel growth collection completes, open air seal set, pass into shielding gas, the gases such as the carbon-source gas in casing and carrier gas are carried out certain dilution, carbon nanotube aerogel is taken out from casing.Viewing window convenient operation person observes the collection situation of casing inner carbon nanotube aerogel.
Spinning axle 21 is hang in collection box 20 by a mechanical arm (not shown), particularly, mechanical arm one end is fixedly connected with the inner roof wall of collection box 20 casing, the other end with spin axle 22 and be fixedly connected with, spin axle 21 be by a motor (not shown) drive and around himself axis rotate, the outside of casing 21 is located at by this motor.
As preferred embodiment, spin on axle 21 and be also provided with collection device (not shown), this collection device is be wrapped in spin magnetic roller on axle 22 or magnetic track, is used for carbon nanotube aerogel to be adsorbed onto on collection device.It should be noted that, magnetic roller here or magnetic track only need can meet the collection needs of carbon nanotube aerogel with micromagnetism, and above-mentioned magnetic roller or magnetic track preferably adopt and have resistance to chemical attack and resistant to elevated temperatures roller or crawler belt.
It is worth mentioning that at this, collection device 221 be set to can be controlled along spinning moving axially of axle 21, to realize the collection of the carbon nanotube aerogel to different in width.
The specific embodiment utilizing the device of above-mentioned carbon nano-tube aerogel to prepare carbon nanotube aerogel is below provided.
The preparation of S1, carbon source reaction solution
Choose dehydrated alcohol as carbon source, add acetylferrocene as catalyzer simultaneously in dehydrated alcohol, thiophene, as promotor, filters after ultrasonic one hour and obtains homogeneous, stable carbon source reaction solution.Selected carbon source can also be the one in methyl alcohol, ethanol, ethylene glycol, acetone, normal hexane, dimethylbenzene, also can be two kinds in above-mentioned substance or several mixture, at this preferred dehydrated alcohol as carbon source.Catalyzer also can also be 1,1-diethyl ferrocene, acetylferrocene, ferrocene, 1-(2-hydroxyethyl) ferrocene, nickelocene, at this preferred acetylferrocene as catalyzer, the ratio shared in carbon source reaction solution of catalyzer in catalyzer in the quality of ferro element, ferro element accounts for the massfraction of reaction solution between 0.5%-1.0%, and the massfraction of the carbon source reaction solution that thiophene accounts for is between 1.0%-5.0%.
The installation in S2, telescopic composite reaction chamber
The present embodiment adopts two alundum tube inner sleeves, the telescopic composite reaction chamber of composition in the alundum tube selecting the alundum tube of 60 × 350mm to be enclosed within 120 × 1400mm, and the alundum tube of 60 × 350mm does secondary response chamber, and the alundum tube of 120 × 1400mm is decided reaction chamber.
The growth of S3, carbon nanotube aerogel and collection
During carbon nanotube aerogel growth, if use pipe with small pipe diameter pipe to grow as reaction chamber, mainly there is the defect of following three aspects, one is due to catalysis limited area, and carbon source lysis efficiency is low, causes the growth efficiency of carbon nanotube aerogel low.Two is because the space of reaction chamber is too little, and air-flow is smooth, and that causes that the carbon nanotube aerogel of generation can not be very fast is moved out of reaction chamber, and the angle chemically balanced is said, also counteracts that the generating rate of carbon nanotube aerogel.Three are horizontal reacting chambeies is horizontal positioned, level is caused to enter and the product generated can not arrive the other end of equal height in time and block, reaction is caused to interrupt, as needed restoration ecosystem, then require a great deal of time and growth parameter(s) regulated, so not only need to spend the plenty of time, but also can because discontinuous before and after technique, the product grown has the difference of aspect of performance, can have an impact in follow-up utilization to product.
If but use the pipe of Large Diameter Pipeline to grow as reaction chamber, the problem that the carbon source lysis efficiency that causes due to catalysis limited area is low can be solved, thus improve carbon nanotube aerogel growth efficiency, also can be that the product generated can be carried out reaction chamber by carrier gas rapidly, but, carbon nanotube aerogel passes into hydrogen in necessary for growth and carrys out reducing catalyst, pass into the rare gas elementes such as argon gas to provide inert atmosphere, above-mentioned gas also needs as carrier gas simultaneously, by even for the reaction solution after vaporization, stable is carried into high temperature reaction zone, if use the pipe of Large Diameter Pipeline as reaction chamber, strong air turbulence can be there is in the moment that then carrier gas is entering reaction chamber, not only stably the reactive component after vaporization can not be brought into the high temperature reaction zone reaction of reaction chamber, but also the vapor phase stream of high temperature reaction zone can be caused also to get muddled, cause carbon nanotube aerogel cannot be continuous, efficient growth, thus, the carbon nanotube aerogel of continuous uniform cannot be collected at the exit end of reaction chamber.
In the present embodiment, adopt telescopic composite reaction chamber 10 to put into the burner hearth of horizontal electric resistance furnace 30, horizontal electric resistance furnace 30 adopts resistive heating rod 31 to heat, and the temperature setting range of horizontal electric resistance furnace is between 800 DEG C ~ 1600 DEG C.In the present embodiment, preferably by horizontal electric resistance furnace 30 temperature programming to 1300 DEG C.One end flange 60 of main reaction chamber 11 inlet mouth 111 seals.First passing into a certain amount of argon gas by carrier gas inlet 42 carries out emptying by telescopic composite reaction chamber 10 with the air in collection box 20, then, in telescopic composite reaction chamber 10, hydrogen and argon gas is passed into by the control of mass-flow gas meter, after 20 minutes, in telescopic composite reaction chamber 10, carbon source reaction solution is injected with 2ml/min by precise injection pump, carbon source reaction solution is after cold zone (the pipe with small pipe diameter alundum tube region) vaporization of front end, telescopic composite reaction chamber 10, the high-temperature zone catalytic cracking growth entering into main reaction chamber 11 under the carrying of hydrogen and argon gas becomes carbon nanotube aerogel, and then the carbon nanotube aerogel generated can shift out main reaction chamber 11 from air outlet 112 together under the carrying of air-flow, spinning on axle in collection box 20 is collected.In the reaction, temperature of reaction can set according to doing other to carbon nanotube caliber, wall number or otherwise performance and requirement, the setting range of temperature is between 800 DEG C-1600 DEG C, and the injection speed of reaction solution also can set according to actual needs to be injected between 0.2-7ml/min.
Driving is spun axle 21 and is rotated, to make the carbon nanotube aerogel of generation be wound on collection device.Due to carbon nanotube aerogel also remaining metal catalyst, the roller or magnetic track absorption that spin magnetic on axle 21 can be wrapped in, spin axle 21 to be rotated by motor (not shown) driving, along with the rotation spinning axle 21, collection of being broken by carbon nanotube aerogel spins, define carbon nanotube aerogel, its microscopic appearance is joined shown in Fig. 2.
After single collection completes, open air seal set, pass into shielding gas, preferred nitrogen, certain dilution is carried out in the carbon source raw material gas in collection box 20 and carrier gas etc., carbon nanotube aerogel is taken out.Pass through aforesaid method, solve the drawback of single pipe as reaction chamber carbon nano-tube, the production productive rate of carbon nanotube aerogel (collecting the quality of the carbon nanotube aerogel obtained in the unit time) can also be made to bring up to more than 20 times of single alundum tube productive rate, continuous collection time also extends to more than ten times of single alundum tube, this not only greatly reduces production cost and time cost, and provides a kind of feasible scheme for suitability for industrialized production.
Be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
A series of detailed description listed is above only illustrating for feasibility embodiment of the present invention; they are also not used to limit the scope of the invention, all do not depart from the skill of the present invention equivalent implementations done of spirit or change all should be included within protection scope of the present invention.
Claims (10)
1. for a device for carbon nano-tube aerogel, it is characterized in that, it comprises:
Main reaction chamber, its air outlet that there is an inlet mouth and be oppositely arranged with described inlet mouth;
Collection box, is connected with the air outlet in described main reaction chamber;
Described main reaction chamber is used for catalysis and generates carbon nanotube aerogel, be provided with the collection device spinning axle and spin described in being arranged on axle in described collection box, described in spin axle can be rotated the carbon nanotube aerogel that catalysis in described main reaction chamber generates is wound on described collection device with driving;
Wherein, the secondary response chamber that at least one is communicated with described main reaction chamber is also arranged with in described main reaction chamber, the inlet mouth of described secondary response chamber near described main reaction chamber is arranged, and is less than the length in described main reaction chamber in the length in the axially described secondary response chamber in described main reaction chamber.
2. the device for carbon nano-tube aerogel according to claim 1, it is characterized in that, the described device for carbon nano-tube aerogel is included in multiple secondary response chambeies sheathed step by step in the radial direction in described main reaction chamber, and multiple secondary response chamber is from inside to outside set in the radial direction in described main reaction chamber, in described main reaction chamber, length axially and the sectional area in the radial direction of main reaction chamber increase gradually.
3. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, in described main reaction chamber, axially complete coated setting is in the inner and adjacent secondary response chamber in arbitrary secondary response chamber.
4. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, described main reaction chamber and described secondary response chamber are tubulose, and described main reaction chamber and described secondary response chamber are coaxially arranged.
5. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, the one end in described secondary response chamber and the concordant setting of inlet mouth in described main reaction chamber.
6. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, there is space between described main reaction chamber and described secondary response chamber, and described space adopts insulating cotton to fill.
7. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, described main reaction chamber overcoat horizontal electric resistance furnace.
8. the device for carbon nano-tube aerogel according to claim 1, is characterized in that, the material in described main reaction chamber and described secondary response chamber is corundum or quartzy or mullite.
9. the device for carbon nano-tube aerogel according to claim 1, it is characterized in that, the described device for carbon nano-tube aerogel also comprises injection device, and described injection device is selected from the one in syringe pump, liquid ejector, ultrasonic atomizatio injection device.
10. the device for carbon nano-tube aerogel according to claim 9, is characterized in that, is also provided with carbon source inlet and carrier gas inlet between described injection device and described main reaction chamber.
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