CN111943173B - Equipment for preparing carbon nanohorn by electric arc method and method for preparing carbon nanohorn - Google Patents
Equipment for preparing carbon nanohorn by electric arc method and method for preparing carbon nanohorn Download PDFInfo
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Abstract
The invention provides equipment for preparing carbon nanohorns by an electric arc method, wherein a main body (1) of the equipment comprises a columnar reaction chamber (2), a chamber inner wall (18), cathode graphite rods, anode graphite rods (3 and 4), a carbon nanohorn collecting assembly and a gas input pipeline; after discharging, gas is conveyed to a gap between the cathode graphite rod and the anode graphite rod through a gas input pipeline, wherein the gas comprises oxygen, helium and carbon-containing gas. The gas is conveyed to the gap between the graphite rods of the cathode and the anode through the gas input pipeline, the proportion and the flow rate of the gas are optimized, and particularly the position and the distance of the gas outlet of the gas conveying pipeline are optimized, so that the efficiency of producing the carbon nanohorn can be greatly improved, and the efficiency is more than 10 times of that of a common electric arc method.
Description
Technical Field
The invention belongs to the technical field of carbon nano-material preparation, and particularly relates to equipment and a method for preparing carbon nanohorns by an electric arc method.
Background
Single-walled carbon nanohorns (SWNHs for short) are another emerging carbon nanomaterial that has been followed by carbon nanotubes in recent years. The diameter of the single carbon nanohorn is 2-5nm, one end of the single carbon nanohorn is of a closed conical structure, the other end of the single carbon nanohorn is open, and the length of the single carbon nanohorn is 10-20 nm. Carbon nanohorns usually exist as spherical aggregates with a diameter of 50-100nm, and the morphology of the aggregates is three types, namely, marble-like (dahlia-like aggregates), bud-like (bud-like aggregates) and seed-like (seed-like aggregates) (Azami T, et al. J PhysChem C,2008,112: 1330.). The pyramidal hollow structure and the unique morphology of the carbon nanohorn enable the carbon nanohorn to have great application potential in the aspects of catalyst carriers, fuel cells, lithium ion batteries, drug transport carriers and the like. Therefore, synthesis and property research of carbon nanohorns have been a hot spot in scientific research in recent years.
At present, the methods for preparing carbon nanohorns mainly include a laser method and an arc method. Among them, the carbon nanohorn prepared by the laser method has high cost, the carbon nanohorn prepared by the direct current arc method has high purity and relatively low cost, but the production efficiency is low, most researches stay in a laboratory stage, and large-scale industrial production is not realized. For example, human CO such as Ijima in Japan2The graphite rod was evaporated by a laser under a pressure of 760Torr in an Ar atmosphere to obtain high purity carbon nanohorns (chem. Phys. Lett.,1999, 165-170). CN104609390A was the result of an early study by the applicant of the present application, and discloses that the distance between the anode and the cathode is set to 1And (3) preparing the carbon nanohorn by direct current arc discharge in a compressed air atmosphere.
Disclosure of Invention
In order to overcome the defects of the prior art, the high-purity carbon nanohorn can be efficiently obtained by modifying direct-current arc equipment and selecting an arc discharge atmosphere.
The invention provides equipment for preparing carbon nanohorns by an electric arc method, wherein a main body (1) of the equipment comprises a columnar reaction chamber (2), a chamber inner wall (18), cathode graphite rods, anode graphite rods (3 and 4), a carbon nanohorn collecting assembly and a gas input pipeline; after discharging, gas is conveyed to a gap between the cathode graphite rod and the anode graphite rod through a gas input pipeline, wherein the gas comprises oxygen, helium and carbon-containing gas.
The carbon-containing gas includes but is not limited to carbon monoxide, diethyl ether, acetylene.
Preferably, the distance between the graphite rods of the anode and the cathode is 1-10mm, preferably 2-3 mm. In the whole process of preparing the carbon nanohorn, the distance between the graphite rods of the cathode and anode is always kept in the above range. For example, a stepper motor may be used to control the movement of the graphite rods so as to maintain a constant distance between the graphite rods.
The carbon nanohorn collecting assembly comprises a collecting push-pull device positioned at the upper part of the columnar reaction chamber, and a collector I (5) and a collector II (6) which are positioned outside the columnar reaction chamber, wherein the collecting push-pull device comprises a push-pull rod (10) and a hollow annular push plate (11), the push-pull rod and the hollow annular push plate are connected through a plurality of connecting ribs (13) at intersection points, and the hollow annular push plate can scrape the carbon nanohorns attached to the inner wall (18) of the columnar reaction chamber under the driving of the push-pull rod.
The outer diameter of the hollow annular push plate is 0.01-1mm smaller than the inner diameter of the columnar reaction chamber, and the inner diameter of the annular push plate is 50-100mm smaller than the outer diameter, so that when the push rod is pulled upwards, the carbon nanohorn on the inner wall of the chamber is hung on the hollow annular push plate. That is, the setting of the inner diameter of the annular push plate requires that gas can pass through the hollow circular part of the annular push plate without hindrance, and the scraped carbon nanohorns cannot fall out of the hollow circular part of the push plate.
The number of the connecting ribs is not particularly limited, and the push plate (11) can be stably moved by the push-pull rod (10), and is generally more than or equal to 3. The connecting ribs (13) are uniformly arranged along the push plate at intervals. The push rod is connected with the center intersection points of the connecting ribs.
The outer side of the upper area of the main body (1) is provided with a cooler (8) and a cooling jacket (9), the lower area of the main body (1) is provided with an air inlet and an air outlet which are communicated with the columnar reaction chamber (2), and the air inlet and the air outlet are provided with a valve II (19) for vacuumizing or conveying gas.
When the carbon nanohorn is prepared, the interior of the chamber (2) is vacuumized to 0.001-0.01 MPa, carbon monoxide gas and mixed air are charged, wherein the volume ratio of the carbon monoxide to the mixed air is 1-2:1-2, and the gas is charged to 0.05-0.07 MPa. The evacuation and the gas filling can be performed through valves II (19), and the number of the valves II can be one or more, such as two or three.
The collector is preferably a plurality of collectors, such as 2, 3, 4. A plurality of collectors are disposed at intervals along an upper ring of the cylindrical reaction chamber. The purpose of providing a plurality of collectors is to collect the generated carbon nanohorns sufficiently to avoid waste. In one embodiment of the invention, there are 2 collectors, collector I and collector II respectively.
Collector I (5) and collector II (6) are communicated with reaction chamber (2) through connecting line (7), be equipped with valve I (12) on connecting line (7), valve I (12) and negative pressure device are connected. Closing a valve I (12) on a pipeline in the arc discharge process, attaching carbon nanohorns generated in a reaction chamber to the inner wall (18) of the upper area of a columnar reaction chamber with a cooling jacket, after the arc discharge is finished, driving a push plate (11) to scrape the carbon nanohorns attached to the inner wall (18) of the columnar reaction chamber through a push-pull rod (10), then opening the valve (12), and siphoning the carbon nanohorns collected on the round push plate into a collector I (5) and a collector II (6) through negative pressure.
The negative pressure generated by the negative pressure means is not particularly limited, and the carbon nanohorns on the pusher may be sucked into the collector. Generally, the negative pressure is controlled to be 1-100 pa.
Preferably, the gas input pipeline comprises an oxygen input pipeline (16), a helium input pipeline (17) and an ether input pipeline (14).
More preferably, the gas input line further comprises an acetylene gas input line (15).
The gas outlet of each gas input pipeline faces to the convergence point of the electric arc between the anode and the cathode.
The number of each gas input pipeline is 1-4 independently, namely the number of the oxygen input pipelines, the helium input pipelines, the ether input pipelines and the acetylene input pipelines (if any) is 1-4, and if the number of the gas input pipelines is more than 1, a plurality of gas input pipelines are uniformly arranged along the circumference of the columnar reaction chamber at intervals.
Wherein, an oxygen input pipeline (16) and a helium input pipeline (17) are positioned below the cathode graphite rod and the anode graphite rod in the columnar reaction chamber, and the diethyl ether input pipeline (14) and/or the acetylene input pipeline (15) are positioned above the anode graphite rod and the cathode graphite rod in the columnar reaction chamber.
Further preferably, the gas outlet of the gas feed line is spaced from the point of convergence of the arc (i.e. the gap between the cathode and the anode of the graphite rod) by 40-100mm, preferably 50-70 mm.
Most preferably, the ratio of the distance between the anode graphite rod and the cathode graphite rod to the distance between the gas outlet of the gas input pipeline and the convergence point of the electric arc is 1: 20-30.
The inventor is unique all towards the convergent point of electric arc with a plurality of gas input pipeline to be close to electric arc convergent point certain distance for various gas are through the not equidirectional rapid convergence in electric arc convergent point, can be fully fast with the mist mixing, are favorable to the preparation of carbon nanohorn. In addition, the distance between the graphite rods at the anode and the cathode and the distance between the gas outlet of the gas input pipeline and the convergence point of the electric arc are controlled, so that the gas outlets of the gas output pipelines are uniformly distributed around the convergence point in an approximately spherical shape, the mixing generated during gas output is mainly concentrated near the convergence point of the electric arc, the production efficiency is ensured, and meanwhile, the obtained product carbon nanohorn has high purity and good quality. Gas outlets too far from the point of convergence may not adequately mix the gas, and gas outlets too close to the point of convergence may result in turbulent gas flow.
The present invention also provides a method for preparing carbon nanohorns by an arc process, in which the aforementioned apparatus is used, comprising the steps of: under the atmosphere of carbon monoxide and air, graphite rods are used as a cathode and an anode, the graphite rods horizontally and oppositely extend into the columnar reaction chamber, a plurality of gas input pipelines inwards face to a gap between the cathode and the anode stone grinding rod, input gas is gathered between the cathode and the anode stone grinding rod, and carbon nanohorns are generated through direct current arc discharge.
Preferably, when the gas input pipeline is an oxygen input pipeline, a helium input pipeline and an ether input pipeline, the ratio of the total flow of the oxygen, the helium and the ether gas is 4-6: 4-6:1-2, wherein the total flow rate of oxygen is 300-.
More preferably, when the gas input lines are an oxygen input line, a helium input line, an ether input line and an acetylene input line, the ratio of the total flow rates of oxygen, helium, ether and acetylene gas is 4-6: 4-6:1-2:0.2-0.5, wherein the total flow rate of oxygen is 300-500 mL/min.
Preferably, the discharge current during the direct current arc discharge is 1000 to 2000A.
Preferably, the pressure of the carbon monoxide-air atmosphere is 5X 10-2～7×10-2MPa, and the volume ratio of carbon monoxide to air is 1-2: 1-2.
Preferably, the arc ignition temperature in the air atmosphere is 2000-3500 ℃.
The invention has the following beneficial effects:
in the process of preparing the carbon nanohorn by the electric arc method, the gas is conveyed to the gap between the graphite rods of the cathode and the anode through the gas input pipeline, the proportion and the flow rate of the gas are optimized, particularly the position and the distance of the gas outlet of the gas conveying pipeline are optimized, the efficiency of producing the carbon nanohorn can be greatly improved, and in the specific implementation mode of the carbon nanohorn production equipment, the carbon nanohorn with higher purity can be produced by about 3kg per hour. Is more than 10 times of the efficiency of the common arc method.
The invention also provides a specific carbon nanohorn collecting assembly, which comprises a collecting push-pull device positioned at the upper part of the columnar reaction chamber and a carbon nanohorn collector positioned outside the columnar reaction chamber, wherein the collecting push-pull device comprises a push-pull rod and a hollow annular push plate, and the carbon nanohorns attached to the inner wall (18) of the columnar reaction chamber can be scraped off by the round push plate under the driving of the push-pull rod. Thus, the produced carbon nanohorns can be collected under the condition of not opening the reaction equipment, and after the scraping, the collection of the product carbon nanohorns can be completed by only opening the valve I connected to the collector and the negative pressure in the collector. After the collection is finished, the chamber (2) is only needed to be vacuumized again, carbon monoxide and air gas are filled, discharge is carried out, and gases such as oxygen, helium, ether and the like are conveyed through the gas input pipeline, so that the production of the carbon nanohorn can be continued, and the production efficiency is further improved.
Drawings
Fig. 1 is a schematic view of the internal structure of an apparatus for manufacturing carbon nanohorns by an arc process according to the present invention.
Fig. 2 is a side view of the internal structure of an apparatus for manufacturing carbon nanohorns by an arc process according to the present invention.
Fig. 3 is a front view of the internal structure of an apparatus for manufacturing carbon nanohorns by an arc process according to the present invention.
Fig. 4 is a side view of the internal structure of an apparatus for manufacturing carbon nanohorns by an arc process according to the present invention.
Fig. 5 is a partial view of a push plate (10) in the apparatus for manufacturing carbon nanohorns by the arc process according to the present invention.
FIG. 6 is a Transmission Electron Micrograph (TEM) of carbon nanohorns prepared by the arc method of example 1.
FIG. 7 is a Transmission Electron Micrograph (TEM) of carbon nanohorns prepared by the arc method of example 1.
FIG. 8 is a Transmission Electron Micrograph (TEM) of carbon nanohorns prepared by the arc process in example 2.
In the figure: the device comprises a main body 1, a reaction chamber 2, a cathode graphite rod 3, an anode graphite rod 4, a carbon nanohorn collector I5, a carbon nanohorn collector II 6, a connecting pipeline 7, a cooler 8, a cooling jacket 9, a push-pull rod 10, a push plate 11, a valve I12, a connecting rib 13, an ether input pipeline 14, an acetylene gas input pipeline 15, an oxygen input pipeline 16, a helium input pipeline 17, a chamber inner wall 18 and a valve II 19.
Detailed Description
For further understanding of the present invention, the apparatus for arc process for preparing carbon nanohorns and the method for arc process for preparing carbon nanohorns according to the present invention will be described below with reference to examples, but it should be understood that these descriptions are only for the purpose of illustrating the features and advantages of the present invention in more detail, but do not limit the scope of the present invention in any way.
The graphite rod used in the embodiment of the invention is a square spectrum graphite electrode, the purity is more than or equal to 99.99%, and the size is 30mm multiplied by 310 mm.
Example 1
An apparatus for preparing carbon nanohorns by an electric arc method comprises a columnar reaction chamber, cathode and anode graphite rods, a carbon nanohorn collecting assembly and a gas input pipeline. The distance between the graphite rods of the cathode and the anode is 3mm, and the distance is kept unchanged in the whole production process by using a stepping motor. The carbon nanohorn collecting assembly comprises a collecting push-pull device positioned at the top of the columnar reaction chamber, a carbon nanohorn collector positioned outside the columnar reaction chamber, and a cooling jacket sleeved on the upper area of the columnar reaction chamber; the collecting push-pull device comprises a push-pull rod and a hollow annular push plate, and the push-pull rod is connected with the centers of 3 connecting ribs of the hollow annular push plate. The outer diameter of the circular push plate is 0.1mm smaller than the inner diameter of the columnar reaction chamber, and the inner diameter of the annular push plate is 70mm smaller than the outer diameter. The collector is 2 collectors I and II which are symmetrically arranged, the collectors I and II are communicated with the reaction chamber through pipelines, and the pipelines are provided with valves which are connected with a negative pressure device. The gas input pipeline comprises an oxygen input pipeline, a helium input pipeline, an ether input pipeline and an acetylene input pipeline, wherein the oxygen input pipeline and the helium input pipeline are positioned below the cathode graphite rod and the anode graphite rod in the columnar reaction chamber, and the ether input pipeline and the acetylene input pipeline are positioned above the anode graphite rod and the cathode graphite rod in the columnar reaction chamber; and the gas feed line is directed towards the point of convergence of the arc between the anode and the cathode. The number of the oxygen input pipeline, the helium input pipeline, the ether input pipeline and the acetylene input pipeline is respectively 3, and the oxygen input pipeline, the helium input pipeline, the ether input pipeline and the acetylene input pipeline are uniformly arranged along the circumference of the columnar reaction chamber at intervals.
The method for preparing carbon nanohorns by the arc method using the apparatus of this example was: firstly, the vacuum is pumped to 1 multiplied by 10 through a valve II arranged at the lower part of the chamber-3MPa, charging mixed gas of carbon monoxide and air according to the volume ratio of 1:1 to ensure that the pressure inside the chamber is 5 x 10-2MPa. The graphite rod is used as the anode and the cathode, the graphite rod horizontally and rightly extends into the columnar reaction chamber, each gas input pipeline inwards faces to a gap between the cathode and the anode graphite rod, and the distance between the outlet of each pipeline gas and the junction between the cathode and the anode is 70mm, so that the input gas is converged between the cathode and the anode graphite rod, the flow rate of the gas outlet is adjusted, and the ratio of the total flow of oxygen, helium and ether gas is 5: 5: 1: 0.2, wherein the total flow rate of oxygen is 350mL/min, the carbon nanohorn is generated by direct current arc discharge with the discharge current of 1300A and the arc burning temperature of 3000 ℃. The temperature of the cooling jacket is set at 5-8 ℃, the productivity of the carbon nanohorn per hour is 3.26kg through calculation, and the purity of the carbon nanohorn is 97.3% through test. The transmission electron micrographs are shown in FIGS. 6 and 7.
Example 2
An apparatus for preparing carbon nanohorns by an electric arc method comprises a columnar reaction chamber, a cathode, an anode graphite rod, an automatic anode graphite rod conveying part, an automatic cathode graphite rod conveying part, an automatic carbon nanohorn collecting component and an automatic gas input pipeline. The distance between the graphite rods of the cathode and the anode is 2mm, and the distance is kept unchanged in the whole production process by using a stepping motor. The carbon nanohorn collecting assembly comprises a collecting push-pull device positioned at the top of the columnar reaction chamber, a carbon nanohorn collector positioned outside the columnar reaction chamber, and a cooling jacket sleeved on the upper area of the columnar reaction chamber; the collecting push-pull device comprises a push-pull rod and a hollow annular push plate, and the push-pull rod is connected with the centers of 3 connecting ribs of the hollow annular push plate. The outer diameter of the circular push plate is 0.2mm smaller than the inner diameter of the columnar reaction chamber, and the inner diameter of the annular push plate is 50mm smaller than the outer diameter. The collector is 2 collectors I and II which are symmetrically arranged, the collectors I and II are communicated with the reaction chamber through pipelines, and the pipelines are provided with valves which are connected with a negative pressure device. The gas input pipeline comprises an oxygen input pipeline, a helium input pipeline, an ether input pipeline and an acetylene input pipeline, wherein the oxygen input pipeline and the helium input pipeline are positioned below the cathode graphite rod and the anode graphite rod in the columnar reaction chamber, and the ether input pipeline and the acetylene input pipeline are positioned above the anode graphite rod and the cathode graphite rod in the columnar reaction chamber; and the gas feed line is directed towards the point of convergence of the arc between the anode and the cathode. The number of the oxygen input pipeline, the helium input pipeline, the ether input pipeline and the acetylene input pipeline is respectively 2, and the oxygen input pipeline, the helium input pipeline, the ether input pipeline and the acetylene input pipeline are uniformly arranged along the circumference of the columnar reaction chamber at intervals.
The method for preparing carbon nanohorns by the arc method using the apparatus of this example was: firstly, the vacuum is pumped to 0.5 multiplied by 10 through a valve II arranged at the lower part of the chamber-2MPa, charging mixed gas of carbon monoxide and air according to the volume ratio of 1:1 to ensure that the pressure inside the chamber is 7 x 10-2MPa. The graphite rod is used as a cathode and an anode, the graphite rod horizontally and rightly extends into the columnar reaction chamber, each gas input pipeline inwards faces to a gap between the cathode and the anode stone grinding rod, and the outlet of pipeline gas is 50mm away from the junction between the cathode and the anode, so that the input gas is converged between the cathode and the anode stone grinding rod, the flow rate of the gas outlet is adjusted, and the ratio of total flow of oxygen, helium, ether and acetylene gas is 5: 5:1: 0.3, wherein the total flow rate of oxygen is 400mL/min, the carbon nanohorn is generated by direct current arc discharge with the discharge current of 1600A and the arc burning temperature of 2500 ℃. The productivity of the carbon nanohorn per hour was calculated to be 3.32 kg. The purity of the carbon nanohorn was 96.5% by test, and the transmission electron micrograph thereof is shown in fig. 8.
Example 3
The other conditions and parameters were the same as in example 1, except that the outlet of each line gas was adjusted to be 100mm from the junction between the cathode and the anode. The productivity of the carbon nanohorn per hour is calculated to be 2.88 kg. The purity of the carbon nanohorn was tested to be 96.3%.
Example 4
The other conditions and parameters were the same as in example 2, except that the outlet of each line gas was adjusted to be 40mm from the junction between the cathode and the anode. The productivity of the carbon nanohorn per hour is 3.15kg by calculation. The purity of the carbon nanohorn was tested to be 94.6%.
Example 5
The other conditions and parameters were the same as in example 1, except that the outlet of each line gas was adjusted to be 50mm from the junction between the cathode and the anode. The productivity of the carbon nanohorn per hour is 3.07kg by calculation. The purity of the carbon nanohorn was tested to be 95.3%.
Example 6
The other conditions and parameters were the same as in example 1 except that the gas outlet flow rate was adjusted so that the ratio of the total flow rates of oxygen, helium, ether and acetylene gases was 5: 5:1: 1. the productivity of the carbon nanohorn per hour was calculated to be 3.35 kg. The purity of the carbon nanohorn was tested to be 93.7%.
Example 7
The other conditions and parameters were the same as in example 1 except that the gas outlet flow rate was adjusted so that the ratio of the total flow rates of oxygen, helium, ether and acetylene gases was 5: 5:1: 0.1. the productivity of the carbon nanohorn per hour is 3.02kg by calculation. The purity of the carbon nanohorn was tested to be 96.7%.
Example 8
The other conditions and parameters were the same as in example 1, except that, without acetylene feed line, the ratio of the total flow rates of oxygen, helium and diethyl ether was 5: 5:1. The productivity of the carbon nanohorn per hour was calculated to be 2.87 kg. The purity of the carbon nanohorn was tested to be 97.2%.
Claims (15)
1. A main body (1) of the equipment comprises a columnar reaction chamber (2), a chamber inner wall (18), a cathode graphite rod (3), an anode graphite rod (4), a carbon nanohorn collecting assembly and a gas input pipeline; after discharging, conveying gas to a gap between the cathode graphite rod and the anode graphite rod through a gas input pipeline, wherein the gas comprises oxygen, helium and carbon-containing gas;
the carbon nanohorn collecting assembly comprises a collecting push-pull device positioned on the upper part of the columnar reaction chamber, and a carbon nanohorn collector I (5) and a carbon nanohorn collector II (6) positioned outside the columnar reaction chamber, wherein the collecting push-pull device comprises a push-pull rod (10) and a hollow annular push plate (11), the push-pull rod and the hollow annular push plate are connected through a plurality of connecting ribs (13) at intersection points, and the hollow annular push plate can scrape off carbon nanohorns attached to the inner wall (18) of the columnar reaction chamber under the driving of the push-pull rod.
2. The apparatus of claim 1, wherein the distance between the anode and cathode graphite rods is 1-10 mm.
3. The apparatus of claim 2, wherein the distance between the anode and cathode graphite rods is 2-3 mm.
4. The apparatus of claim 1, wherein the hollow annular push plate has an outer diameter 0.01 to 1mm smaller than the inner diameter of the columnar reaction chamber, and the annular push plate has an inner diameter 50 to 100mm smaller than the outer diameter.
5. The apparatus according to claim 1, wherein the collector is 2 collectors, collector I (5) and collector II (6), respectively; the collector I (5) and the collector II (6) are communicated with the reaction chamber (2) through a connecting pipeline (7), a valve I (12) is arranged on the connecting pipeline (7), and the valve I (12) is connected with a negative pressure device; closing a valve I (12) on a pipeline in the arc discharge process, attaching carbon nanohorns generated in a reaction chamber to the inner wall (18) of the upper part area of a columnar reaction chamber with a cooling jacket, after the arc discharge is finished, driving a push plate (11) to scrape the carbon nanohorns attached to the inner wall (18) of the columnar reaction chamber through a push-pull rod (10), then opening the valve I (12), and siphoning the carbon nanohorns collected on the round push plate into a collector I (5) and a collector II (6) through negative pressure.
6. The apparatus according to claim 1, wherein the gas input lines comprise an oxygen input line (16), a helium input line (17), and an ether input line (14).
7. The apparatus according to claim 6, wherein said gas input line further comprises an acetylene gas input line (15); and the gas outlet of the gas inlet line is directed towards the point of convergence of the arc between the anode and the cathode.
8. The apparatus of claim 6, wherein the gas outlet of the gas feed line is spaced from the convergence point of the arc by 40-100 mm.
9. The apparatus of claim 8, wherein the gas outlet of the gas feed line is spaced 50-70mm from the convergence point of the arc.
10. The apparatus of claim 8, wherein the ratio of the distance between the anode and cathode graphite rods to the distance between the gas outlet of the gas inlet line and the convergence point of the arc is 1: 20-30.
11. The apparatus of claim 6, wherein the number of each gas input line is independently 1-4;
wherein, an oxygen input pipeline (16) and a helium input pipeline (17) are positioned below the cathode graphite rod and the anode graphite rod in the columnar reaction chamber, and the diethyl ether input pipeline (14) and/or the acetylene input pipeline (15) are positioned above the anode graphite rod and the cathode graphite rod in the columnar reaction chamber.
12. The apparatus of claim 11, wherein the number of the gas supply lines is 1 or more, and the plurality of gas supply lines are uniformly arranged along the circumference of the cylindrical reaction chamber at intervals.
13. A method for producing carbon nanohorns by an arc process using the apparatus of any one of claims 1 to 12, comprising the steps of: under the atmosphere of carbon monoxide and air, graphite rods are used as a cathode and an anode, the graphite rods horizontally and oppositely extend into the columnar reaction chamber, a plurality of gas input pipelines inwards face to a gap between the cathode and the anode graphite rods, input gas is gathered between the cathode and the anode graphite rods, and carbon nanohorns are generated through direct current arc discharge.
14. The method of claim 13, wherein when the gas input lines are an oxygen input line, a helium input line, and an ether input line, the ratio of the total flow rates of oxygen, helium, and ether gas is 4-6: 4-6:1-2, wherein the total flow rate of oxygen is 300-.
15. The method of claim 13, wherein when the gas input lines are an oxygen input line, a helium input line, an ether input line, and an acetylene input line, a ratio of total flow rates of the oxygen, helium, ether, and acetylene gases is 4-6: 4-6:1-2:0.2-0.5, wherein the total flow rate of oxygen is 300-500 mL/min.
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| CN109665510A (en) * | 2011-04-15 | 2019-04-23 | 大场基美雄 | Carbon nanomaterial manufacturing device and its utilization |
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