CN110589805A - Device and method for preparing carbon aerogel through CVD after carbon nanotubes are activated by electric arc - Google Patents
Device and method for preparing carbon aerogel through CVD after carbon nanotubes are activated by electric arc Download PDFInfo
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Abstract
The invention belongs to the field of carbon aerogel synthesis, and discloses a device and a method for preparing carbon aerogel through CVD after carbon nanotubes are activated by electric arc. The vacuum system is connected with a carbon nanotube storage tank through a pipeline, the carbon nanotube storage tank is provided with a carbon nanotube feeding port, an inert carrier gas inlet is arranged on the left side of the carbon nanotube feeding port and connected with the left end of the reactor through a pipeline, the reactor is provided with an electric arc generator and a carbon source inlet, a temperature control system is arranged outside the reactor, and the right end of the reactor is connected with a finished product collecting storage tank through a pipeline. The invention uses the high temperature of the high-power electric arc to excite the metal into fine nano-grade gaseous particles which can be uniformly coated on the surface of the carbon nano tube, and the carbon aerogel grown by CVD has high graphitization degree, lower bulk density, low heat conductivity coefficient and good heat-insulating property. The device has simple structure, the method is stable and easy to control, and the continuous preparation of the carbon nanotube aerogel with different character indexes can be realized through the switching of the electric arc power.
Description
Technical Field
The invention belongs to the field of carbon aerogel synthesis, and particularly relates to a device and a method for preparing carbon aerogel through CVD after carbon nanotubes are activated by electric arc.
Background
Carbon nanotubes, which are one-dimensional nanomaterials having excellent physical and mechanical properties, are mainly coaxial circular tubes having several to tens of layers of carbon atoms arranged in a hexagonal pattern. It has a very large aspect ratio, typically between 1-100nm in diameter and several microns to hundreds of microns in length. Due to the large length-diameter ratio, the carbon nano tube has excellent mechanical, electrical, electric conduction and heat conduction performances. Because of the excellent performance, the carbon nano tube has wide and potential application prospect in various fields such as catalyst carriers, rubber plastic composite materials, electrochemical materials, photoelectric sensing and the like.
In 2013, scientists at university in Zhejiang developed an ultra-light material, which is a solid material called "all-carbon aerogel" with a density of only 0.16 mg per cubic centimeter, one sixth of the air density, and the lightest material in the world to date. The basic principle of aerogel preparation is to remove the solvent from the gel, leaving it with an intact framework. The carbon aerogel is a novel heat-insulating material which is prepared by a plurality of methods based on carbon materials and has larger specific surface area, smaller density and higher strength.
CN110143591A composite carbon aerogel with high specific surface area and a preparation method thereof, and the invention discloses the composite carbon aerogel with high specific surface area and the preparation method thereof. The method comprises the following steps: firstly, dispersing a nano carbon material in water, adding a certain amount of PVP dispersing agent, dispersing in a high-speed dispersing machine to obtain a suspension of the nano carbon material, dispersing a biomass raw material in water, violently stirring and dissolving to obtain a dispersion liquid, mixing the two, violently stirring and uniformly mixing to obtain a nano carbon material/biological cellulose suspension; freezing for 24-48h at the temperature of minus 40 ℃ to minus 80 ℃, then freeze-drying, then heating to 700-900 ℃ in an inert atmosphere, and preserving heat for 0-6 h to obtain the composite carbon aerogel. The composite carbon aerogel is obtained without solvent exchange, but the mixed dispersion liquid needs to be frozen at ultralow temperature for a long time and needs to be freeze-dried, the preparation conditions are relatively harsh, and large-scale preparation is not easy to realize.
CN110040713A preparation method of carbon aerogel, the invention discloses a preparation method of carbon aerogel. The carbon aerogel is prepared by taking carbon nanospheres as raw materials, heating and reacting in an aqueous solution system in the presence of a cross-linking agent polyvinyl alcohol and a structure directing agent borax, freeze-drying, freezing a reaction product at-78 ℃, and circularly freeze-drying for more than 2 times at-78 ℃. The carbon aerogel prepared by the method has good mechanical properties, but still needs to be freeze-dried for many times and needs the use of a cross-linking agent and guiding borax, which is not favorable for cost control and scale-up production.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device and a method for preparing carbon aerogel by CVD after activating carbon nanotubes by electric arc, aiming at optimizing various complicated links and adverse factors such as solvent removal after sol-gel is needed, repeated ultralow temperature freeze drying, higher preparation cost and the like in the existing preparation method of the carbon aerogel, innovatively carrying out effective dispersion and loading catalytic site activation treatment on the carbon nanotubes in advance by exciting metal steam by high-power electric arc, and then preparing the carbon nanotube aerogel by CVD reaction. To solve the above technical problems.
In a first aspect, the present invention provides an apparatus for preparing carbon aerogel by CVD after arc activation of carbon nanotubes, comprising: the device comprises a reactor, a temperature control system, an electric arc generator, a carbon source air inlet, an inert carrier gas air inlet, a carbon nanotube feeding hole, a carbon nanotube storage tank, a vacuum system and a finished product collecting storage tank;
the vacuum system is connected with the carbon nanotube storage tank through a pipeline, the lower end of the carbon nanotube storage tank is provided with a carbon nanotube feeding port, an inert carrier gas inlet is formed in the left side of the carbon nanotube feeding port and connected with the left end of the reactor through the pipeline, an electric arc generator is fixed at the left end of the reactor, a carbon source inlet is formed in the right side of the electric arc generator and the upper portion of the reactor, a temperature control system is arranged outside the reactor, and the right end of the reactor is connected with a finished product collecting storage tank through the pipeline.
Furthermore, the front end of the reactor is provided with three feeding holes, namely an inert gas inlet, a carbon nano tube powder feeding hole and a carbon source gas inlet from front to back in sequence, and the inert gas inlet, the carbon nano tube powder feeding hole and the carbon source gas inlet have strict front-back logic relation.
In a second aspect, the present invention provides a method for preparing carbon aerogel by CVD after arc activation of carbon nanotubes, comprising:
the method comprises the following steps: introducing preheated inert gas into the reactor through an inert carrier gas inlet, and heating the reactor to the reaction temperature through a temperature control system;
step two: adding carbon nanotube powder into a carbon nanotube storage tank, continuously filling inert gas for many times through a vacuum system, emptying, and then vacuumizing for inert gas replacement;
step three: starting the arc generator to discharge the arc from the active metal connected to the anode and cathode tips of the arc generator;
step four: introducing preheated inert gas from an inert carrier gas inlet, and simultaneously adding carbon nanotube powder from a carbon nanotube inlet and introducing preheated carbon source gas from a carbon source inlet according to the volume ratio;
step five: the carbon nano tube aerogel generated by the reaction enters a finished product collecting tank from the other end of the reactor through a pipeline.
Further, the reaction temperature in the first step is set to be 500-1100 ℃, preferably 600-800 ℃, and more preferably 660-740 ℃.
Further, the carbon nanotubes in the second step are one or a combination of more of single-walled, double-walled and multi-walled carbon nanotubes in a shape of conglomerate, oriented vertical array, oriented horizontal array.
Further, the arc generator in the third step is a direct current arc generator, an alternating current arc generator, an intermittent alternating current arc generator, preferably an alternating current arc generator; the power of the arc generator is 50-3000W, preferably 300-2000W.
Further, in the third step, the active metal connecting the anode and the cathode tip of the arc generator is one or a combination of iron, cobalt, nickel, copper, molybdenum, zinc, chromium, vanadium, tungsten and lanthanum.
Further, the inert gas is one of nitrogen, argon and a mixture thereof.
Further, the carbon source gas is one of methane, ethane, ethylene, propylene, propane, toluene, xylene, methanol, ethanol, carbon monoxide and a combination thereof.
Further, the volume ratio of the inert gas to the carbon source gas in the fourth step is 0.02-30: 1, preferably 0.3-10: 1, more preferably 0.5-6: 1; the ratio of the inlet flow of the inert gas to the carbon nano tube powder is 3-200L/min to 0.1 Kg/min.
Further, the preheating temperature of the inert gas is 400-1100 ℃, preferably 550-800 ℃; the preheating temperature of the carbon source gas is 500 ℃ to 900 ℃, preferably 600 ℃ to 800 ℃.
And repeating the first step to the fifth step to realize the continuous preparation of the high-performance carbon nanotube aerogel by the arc method.
The beneficial effect of the invention is that,
(1) according to the device for preparing the carbon aerogel by CVD after the carbon nano tubes are activated by the electric arc, the high-power electric arc generating device is adopted, the type and the proportion of the loaded active metal of the carbon nano tube carrier can be regulated and controlled by regulating and transforming the power and the tip connecting metal of the generating device, and finally the carbon nano tube aerogel with different property indexes can be prepared;
(2) the invention adopts the high-power arc generator to realize one-time explosive physical dispersion under the condition of small amount of water in the carbon tube while point discharge is carried out, so that the carbon nano tube carrier is further expanded in volume, and the formation of high-performance carbon nano tube aerogel is facilitated.
(3) The preparation equipment has simple structure, the method is stable and easy to control, and the continuous preparation of the carbon nano tube aerogel with different property indexes can be realized by switching the electric arc power.
(4) According to the method for preparing the carbon aerogel by CVD after the carbon nano tube is activated by the electric arc, metal is excited into fine nano-grade gaseous particles by using the high temperature of high-power electric arc, and then the fine nano-grade gaseous particles can be uniformly coated on the surface of the carbon nano tube, so that the active sites are small and are uniformly distributed; most of the multi-wall double carbon aerogel grows by CVD, the specific surface area is greatly improved, the graphitization degree is high, the bulk density is lower, the heat conductivity coefficient is low, and the heat insulation performance is good.
(5) The specific surface area of the carbon nano tube aerogel prepared by the invention is 1500-2450m2The tap density is 0.002-0.015g/cm3The thermal conductivity coefficient is 0.020-0.045W/(m.K).
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic view of an apparatus for preparing carbon aerogel by CVD after arc activation of carbon nanotubes according to the present invention.
FIG. 2 is a schematic flow chart of a method for preparing carbon aerogel by CVD after arc activation of carbon nanotubes according to the present invention.
Fig. 3 is a SEM schematic view of the carbon nanotube aerogel prepared in fig. 1 and 2.
In the figure, the device comprises a reactor 1, a temperature control system 2, an arc generator 3, a carbon source inlet 4, an inert carrier gas inlet 5, a carbon nanotube inlet 6, a carbon nanotube storage tank 7, a carbon nanotube storage tank 8, a vacuum system 9 and a finished product collection storage tank.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the present invention provides an apparatus for preparing carbon aerogel by CVD after arc-activating carbon nanotubes, comprising: the device comprises a reactor 1, a temperature control system 2, an arc generator 3, a carbon source air inlet 4, an inert carrier gas air inlet 5, a carbon nanotube feeding hole 6, a carbon nanotube storage tank 7, a vacuum system 8 and a finished product collecting storage tank 9;
vacuum system 8 is connected with carbon nanotube storage tank 7 through the pipeline, carbon nanotube storage tank 7 lower extreme is provided with carbon nanotube feed inlet 6, carbon nanotube feed inlet 6 left side is provided with inert carrier gas air inlet 5, inert carrier gas air inlet 5 is connected with the left end of reactor 1 through the pipeline, reactor 1 left end is fixed with arc generator 3, arc generator 3's right side, the upper portion of reactor 1 is provided with carbon source air inlet 4, reactor 1 outside is provided with temperature control system 2, reactor 1's right-hand member is collected storage tank 9 through pipeline and finished product and is connected.
The front end of the reactor 1 is provided with three feeding holes, and the three feeding holes are an inert gas inlet 5, a carbon nano tube powder feeding hole 6 and a carbon source gas inlet 4 which have strict front-back logic relation from front to back in sequence.
As shown in fig. 2, the present invention provides a method for preparing carbon aerogel by CVD after arc activation of carbon nanotubes, comprising:
s101: introducing preheated inert gas into the reactor 1 through an inert carrier gas inlet 5, and heating the reactor 1 to the reaction temperature through a temperature control system 2;
s102: adding carbon nanotube powder into a carbon nanotube storage tank 7, continuously filling inert gas for many times through a vacuum system 8, emptying, and then vacuumizing for replacing the inert gas;
s103: starting the arc generator 3 to discharge an arc from the active metal connected to the tips of the anode and cathode of the arc generator 3;
s104: introducing preheated inert gas from an inert carrier gas inlet 5, and simultaneously respectively adding carbon nanotube powder from a carbon nanotube feeding hole 6 and introducing preheated carbon source gas from a carbon source inlet 4 according to the volume ratio;
s105: the carbon nanotube aerogel generated by the reaction enters a finished product collecting tank 9 from the other end of the reactor 1 through a pipeline.
The reaction temperature in the S101 is set to be 500-1100 ℃, preferably 600-800 ℃, and more preferably 660-740 ℃.
The carbon nanotubes in the S102 are one or a combination of more of single-walled, double-walled and multi-walled carbon nanotubes in a clustered shape, an oriented vertical array shape and an oriented horizontal array shape.
The arc generator 3 in the step S103 is a direct current arc generator, an alternating current arc generator or an intermittent alternating current arc generator, preferably an alternating current arc generator; the power of the arc generator is 50-3000W, preferably 300-2000W.
In the step S103, the active metal connecting the anode and the cathode of the arc generator 3 is one or a combination of iron, cobalt, nickel, copper, molybdenum, zinc, chromium, vanadium, tungsten, and lanthanum.
The inert gas is one of nitrogen, argon and their mixture.
The carbon source gas is one of methane, ethane, ethylene, propylene, propane, toluene, xylene, methanol, ethanol, carbon monoxide and a combination thereof.
The volume ratio of the inert gas to the carbon source gas in the S104 is 0.02-30: 1, preferably 0.3-10: 1, and more preferably 0.5-6: 1; the ratio of the inlet flow of the inert gas to the carbon nano tube powder is 3-200L/min to 0.1 Kg/min.
The preheating temperature of the inert gas is 400-1100 ℃, preferably 550-800 ℃; the preheating temperature of the carbon source gas is 500 ℃ to 900 ℃, preferably 600 ℃ to 800 ℃.
And repeating the first step to the fifth step to realize the continuous preparation of the high-performance carbon nanotube aerogel by the arc method.
According to the device and the method for preparing the carbon aerogel through CVD after the carbon nano tubes are activated through the electric arc, the obtained carbon aerogel is prepared and shown in figure 3.
The specific surface area of the carbon nano tube aerogel prepared by the invention is 1500-2450m2The tap density is 0.002-0.015g/cm3The thermal conductivity coefficient is 0.020-0.045W/(m.K).
The invention uses the high temperature of the high-power electric arc to excite the metal into fine nanometer gaseous particles which can be uniformly coated on the surface of the carbon nano tube, and the carbon aerogel grown by CVD has high graphitization degree, lower bulk density, low heat conductivity coefficient and good heat insulation performance.
The application of the present invention will be further described with reference to the following specific examples;
example 1:
(1) introducing nitrogen preheated at 800 ℃ into the 1-reactor from the position 5, starting the equipment 2, heating to 790-800 ℃;
(2) adding 900g of vertical array carbon nanotube powder into a 7-carbon nanotube storage tank, continuously performing three times of flushing with nitrogen for emptying through 8 times, and then performing vacuum pumping for inert gas replacement;
(3) starting a 1800W power direct current arc generating device to enable the tip of the 3-connection iron simple substance to emit an arc;
(4) 3L/min of nitrogen is introduced by adjusting a 5-air inlet, and 5g/min of carbon nano tube powder is added from a 6-carbon nano tube feeding port and 1L/min of carbon monoxide gas preheated at 750 ℃ is introduced from a 4-carbon source air inlet;
(5) the generated carbon nano tube aerogel enters a finished product collecting tank 9 from the other end of the reactor through a pipeline;
(6) keeping the reaction for 90min, and continuously preparing the high-performance carbon nanotube aerogel;
(7) the product was weighed 478g and tested, ID/IG0.039, SSA 2421m2(ii) a tap density of 0.008g/cm3The thermal conductivity coefficient is 0.026W/(m.K).
Example 2:
(1) introducing argon preheated at the temperature of 920 ℃ into the 1-reactor from the position 5, starting the equipment 2, heating to the temperature of 910-920 ℃;
(2) adding 2000g of vertical array carbon nanotube powder into a 7-carbon nanotube storage tank, continuously performing flushing with argon for five times through 8 times, emptying, and then vacuumizing to complete replacement;
(3) starting a 2000W power alternating current arc generating device to enable the tip of the 3-connection nickel simple substance to emit an arc;
(4) adjusting a 5-gas inlet and introducing 20L/min of argon gas, and simultaneously respectively adding 12g/min of carbon nano tube powder from a 6-carbon nano tube feed inlet and introducing 5L/min of methane gas preheated at 880 ℃ from a 4-carbon source gas inlet;
(5) the generated carbon nano tube aerogel enters a finished product collecting tank 9 from the other end of the reactor through a pipeline;
(6) keeping the reaction for 120min, and continuously preparing the high-performance carbon nanotube aerogel;
(7) the product was weighed 1619g and tested, ID/IG0.056, SSA 2147m2(ii)/g, tap density 0.012g/cm3The thermal conductivity was 0.031W/(m.K).
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An apparatus for preparing carbon aerogel by arc activation of carbon nanotubes and CVD, the apparatus comprising: the device comprises a reactor (1), a temperature control system (2), an electric arc generator (3), a carbon source air inlet (4), an inert carrier gas air inlet (5), a carbon nano tube feeding hole (6), a carbon nano tube storage tank (7), a vacuum system (8) and a finished product collecting storage tank (9);
the vacuum system (8) is connected with the carbon nanotube storage tank (7) through a pipeline, the lower end of the carbon nanotube storage tank (7) is provided with a carbon nanotube feeding port (6), the left side of the carbon nanotube feeding port (6) is provided with an inert carrier gas inlet (5), the inert carrier gas inlet (5) is connected with the left end of the reactor (1) through a pipeline, the left end of the reactor (1) is fixed with an electric arc generator (3), the right side of the electric arc generator (3) is provided with a carbon source inlet (4) on the upper portion of the reactor (1), the temperature control system (2) is arranged outside the reactor (1), and the right end of the reactor (1) is connected with a finished product collecting storage tank (9) through a.
2. A method for preparing carbon aerogel through CVD after carbon nanotubes are activated by electric arc is characterized in that the method for preparing the carbon aerogel through CVD after the carbon nanotubes are activated by electric arc comprises the following steps:
the method comprises the following steps: introducing preheated inert gas into the reactor (1) through an inert carrier gas inlet (5), and heating the reactor (1) to the reaction temperature through a temperature control system (2);
step two: adding carbon nano tube powder into a carbon nano tube storage tank (7), continuously filling inert gas for many times through a vacuum system (8), emptying, and vacuumizing to perform inert gas replacement;
step three: starting the arc generator (3) to discharge an arc from the active metal connected to the anode and cathode tips of the arc generator (3);
step four: introducing preheated inert gas from an inert carrier gas inlet (5), and simultaneously respectively adding carbon nanotube powder from a carbon nanotube feeding hole (6) and introducing preheated carbon source gas from a carbon source gas inlet (4) according to the volume ratio;
step five: the carbon nano tube aerogel generated by the reaction enters a finished product collecting tank (9) from the other end of the reactor (1) through a pipeline.
3. The method for preparing carbon aerogel by CVD after arc-activating carbon nanotubes according to claim 2, wherein the reaction temperature in the first step is set to 500 ℃ to 1100 ℃, preferably 600 ℃ to 800 ℃, more preferably 660 ℃ to 740 ℃.
4. The method for preparing carbon aerogel by CVD after arc-activating carbon nanotubes according to claim 2, wherein the carbon nanotubes in step two are one or more of clustered, oriented vertically arrayed, oriented horizontally arrayed single-walled, double-walled, and multi-walled carbon nanotubes.
5. The method for preparing carbon aerogel by arc-activating carbon nanotubes and then CVD according to claim 2, wherein the arc generator (3) in the third step is a DC arc generator, an AC arc generator, an interrupted AC arc generator, preferably an AC arc generator; the power of the arc generator is 50-3000W, preferably 300-2000W.
6. The method for preparing carbon aerogel by arc-activated carbon nanotubes and CVD according to claim 2, wherein the active metal of the anode and cathode tip of the arc generator (3) in the third step is one or a combination of Fe, Co, Ni, Cu, Mo, Zn, Cr, V, W, La.
7. The method for arc activation of carbon nanotubes followed by CVD for producing carbon aerogel of claim 2, wherein said inert gas is one of nitrogen, argon and mixtures thereof.
8. The method of arc activating carbon nanotubes and CVD for producing carbon aerogel as claimed in claim 2, wherein said carbon source gas is one of methane, ethane, ethylene, propylene, propane, toluene, xylene, methanol, ethanol, carbon monoxide and combinations thereof.
9. The method for preparing carbon aerogel by CVD after arc-activating carbon nanotubes according to claim 2, wherein the volume ratio of the inert gas to the carbon source gas in said fourth step is 0.02-30: 1, preferably 0.3-10: 1, more preferably 0.5-6: 1; the ratio of the inlet flow of the inert gas to the carbon nano tube powder is 3-200L/min to 0.1 Kg/min.
10. The method for preparing carbon aerogel by CVD after arc-activating carbon nanotubes according to claim 2, wherein the preheating temperature of the inert gas is 400 ℃ to 1100 ℃, preferably 550 ℃ to 800 ℃; the preheating temperature of the carbon source gas is 500 ℃ to 900 ℃, preferably 600 ℃ to 800 ℃.
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| CN111312430A (en) * | 2020-02-25 | 2020-06-19 | 深圳市三顺纳米新材料股份有限公司 | Carbon nanotube conductive agent and preparation method thereof |
| CN111578513A (en) * | 2020-05-25 | 2020-08-25 | 中国空气动力研究与发展中心超高速空气动力研究所 | Low-pollution electric arc heater |
| CN111592376A (en) * | 2020-06-08 | 2020-08-28 | 北京化工大学 | Composite aerogel functional material based on ferroferric oxide nanowire/graphene oxide interpenetrating structure and preparation method thereof |
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