CN117865132A - Continuous preparation device and preparation method of single-walled carbon nanotubes - Google Patents

Continuous preparation device and preparation method of single-walled carbon nanotubes Download PDF

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CN117865132A
CN117865132A CN202410093966.8A CN202410093966A CN117865132A CN 117865132 A CN117865132 A CN 117865132A CN 202410093966 A CN202410093966 A CN 202410093966A CN 117865132 A CN117865132 A CN 117865132A
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walled carbon
plasma arc
carbon nanotubes
arc furnace
anode
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陈名海
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Wuhu Hi Tech New Materials Co ltd
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Wuhu Hi Tech New Materials Co ltd
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Abstract

The invention relates to a continuous preparation device and a preparation method of single-walled carbon nanotubes, wherein the continuous preparation device comprises a plasma arc furnace, a cathode and an anode are arranged in the plasma arc furnace, the cathode is connected with an evaporation feeding device, a reaction air inlet and a discharge outlet are arranged on the plasma arc furnace, a shrinkage solidification bath is distributed at the discharge outlet, and a winding collecting device is distributed above the shrinkage solidification bath. The method is characterized in that the molten liquid metal is used for providing a heat source for the growth of the single-walled carbon nanotubes in an anode plasma arc furnace, ultrahigh transient high temperature can be generated, the central plasma arc temperature can reach 20000 ℃ theoretically, high-efficiency cracking of growth precursors and catalyst evaporation can be guaranteed, huge driving energy is provided for the growth of the single-walled carbon nanotubes, rapid reaction of high-concentration catalyst particles and a cracking carbon source is realized, the growth efficiency is greatly improved, and the yield is 2-3 orders of magnitude higher than that of a conventional floating chemical vapor deposition and plasma torch method.

Description

Continuous preparation device and preparation method of single-walled carbon nanotubes
Technical Field
The invention relates to the technical field of new materials, in particular to a continuous preparation device and a preparation method of single-walled carbon nanotubes.
Background
The single-wall carbon nano tube is a one-dimensional tubular nano material formed by sp2 hybridized carbon-carbon bonds, can be regarded as a single-layer graphite curled hollow structure, has great application prospect in the fields of conductive modification, mechanical enhancement and functional devices because of excellent mechanical, electrical, thermal and other physical and chemical properties, becomes a hot spot for current basic research and application research, and has been applied in the fields of new energy, catalysis, conductive modification and the like on a large scale. However, due to the perfect characteristics of the single-walled carbon nanotube structure, the preparation method and the process conditions are far different from those of the conventional multi-walled carbon nanotubes, so that the realization of large-scale preparation still has great challenges. At present, the preparation methods of single-wall carbon nanotubes include an arc method, a plasma method, a laser method, a high-pressure carbon monoxide method and a chemical vapor deposition method, and although remarkable progress is made in laboratories, various methods generally have difficulty in achieving both quality and efficiency. The floating chemical vapor deposition method has relatively advantages, is mainly characterized by simple process, can spontaneously aggregate into an aerogel structure in the growth stage of the carbon nanotubes, can realize continuous preparation and collection, has shown great advantages compared with other methods, and is the most popular single-wall carbon nanotube preparation method in current research. However, because the reaction temperature is low, the energy cross-domain reaction barrier required by the rapid growth of the single-walled carbon nanotubes cannot be met, the reaction can be carried out only under the condition of very low catalyst concentration, and the growth of the catalyst and the carbon source to the multi-walled carbon nanotubes is caused by increasing the concentration of the catalyst and the carbon source, so that the aerogel structure and the continuity are rapidly reduced. The yield of single-walled carbon nanotubes prepared by floating chemical vapor deposition is very low, which is also the root cause of the future industrialization for more than 20 years. In order to improve the preparation efficiency of the floating chemical vapor deposition method, a great deal of research and study is conducted. Because the mode of the existing tubular furnace as a reaction vessel cannot bear too high furnace temperature, a great amount of heat is taken away by air flow in the growth process, and a steady-state high-temperature reaction cannot be provided, so that the improvement of the furnace temperature simply cannot realize a leap of yield quality. Therefore, the growth efficiency of the single-walled carbon nanotubes is improved, and the novel catalytic reaction system and the high-efficiency catalyst for the growth of the single-walled carbon nanotubes are explored, so that the method is a key link for realizing continuous large-scale preparation.
The plasma arc has ultrahigh temperature, and theoretically the core temperature can reach 20000 ℃, so that the plasma arc is an ideal ultrahigh temperature heat source. Meanwhile, the plasma can also crack organic matters to generate a large number of free radicals to realize the function of activating reactants, so that the method is widely used for carbon nano tube growth research, such as a traditional plasma method and a plasma enhanced chemical vapor deposition technology. However, the transient high temperature generated by the plasma arc is difficult to control, and particularly, the growth condition of the single-wall carbon nano tube is greatly disturbed, the residence time of the catalyst in a high temperature area is very short in the conventional plasma method, and the catalyst and the carbon source are not fully utilized, so that the yield reported by the conventional plasma method is still very low. Therefore, how to develop the advantages of the high-temperature plasma arc, the advantages are improved, the growth of the single-wall carbon nano tube is practically promoted, and a great challenge still exists.
Disclosure of Invention
In order to solve the technical problems, the invention provides a continuous preparation device and a continuous preparation method of single-walled carbon nanotubes. The technical problems to be solved by the invention are realized by adopting the following technical scheme:
the continuous preparation device of the single-walled carbon nanotube comprises a plasma arc furnace, wherein a cathode and an anode are arranged in the plasma arc furnace, the cathode is connected with an evaporation feeding device, a reaction air inlet and a discharge port are arranged on the plasma arc furnace, a shrinkage coagulation bath is distributed at the discharge port, and a winding collecting device is distributed above the shrinkage coagulation bath;
the evaporation feeding device comprises a heating evaporator connected with the cathode, and the heating evaporator is connected with a feeding pump.
The feeding pump is a syringe pump or a peristaltic pump or the same type of product.
The cathode is a graphite electrode, the anode is a high-melting-point alloy, a second-phase catalyst composed of refractory metals is contained in the anode, and the anode takes part in the reaction by molten liquid metal.
The shrinkage coagulation bath is water or an aqueous solution containing a surfactant.
A continuous process for the preparation of single-walled carbon nanotubes, comprising the steps of:
the first step: dissolving a cocatalyst consisting of a metal organic compound formed by any one of iron, cobalt and nickel and a chalcogen simple substance or a compound thereof in an organic solvent to prepare a single-walled carbon nanotube growth precursor;
and a second step of: loading a single-walled carbon nanotube growth precursor into an evaporation feeding device, and simultaneously heating the heating evaporator to a specified temperature;
and a third step of: under the protection of the inert gas of the hearth, introducing plasma arc gas from a cathode, energizing and exciting to generate a plasma arc, melting an anode arranged in the plasma arc furnace into a liquid state, and raising the hearth temperature of the plasma arc furnace to a specified temperature;
fourth step: starting an evaporation feeding device, injecting a single-wall carbon nanotube growth precursor into a heating evaporator, introducing the single-wall carbon nanotube growth precursor into a plasma arc furnace from a cathode under the drive of inert gas, introducing carbon source gas and carrier gas for reaction, and continuously discharging a product out of the plasma arc furnace along with tail gas;
fifth step: and (3) carrying out coagulation bath on the discharged single-walled carbon nanotube product through a shrinkage coagulation bath to obtain a single-walled carbon nanotube bundle, and finally, rolling by a winding collecting device to obtain the final single-walled carbon nanotube.
In the first step, the organic metal compound is any one of carbonyl iron, ferrocene, nickel-dicyclopentadienyl and cobaltocene or any one of the derivatives of the materials, and the concentration of the precursor of the organic metal compound for growing the single-wall carbon nano tube is 2-20%;
the promoter is any one of sulfur powder, selenium powder, thiophene and carbon disulfide, and the concentration of a precursor for growing the single-wall carbon nano tube is 0.01-2%;
the organic solvent is any one of benzene, toluene, xylene, acetone, liquid alkane, petroleum ether, ethanol and methanol.
The second step heats the evaporator to a pre-specified temperature of 100 to 500 ℃.
The inert gas in the third step is any one of nitrogen, argon and helium;
the plasma arc gas is any one of nitrogen, argon, helium, hydrogen and steam and mixed gas of two or three of the gases in any mixing proportion, and the flow is 10L/min-500L/min;
the hearth temperature of the plasma arc furnace is 600-1900 ℃;
the anode is a high-melting-point alloy containing a second-phase catalyst, and is an alloy formed by iron, cobalt and nickel and refractory metals of molybdenum, tungsten, tantalum, niobium, hafnium and zirconium, wherein the refractory metal element proportion is 20-80%.
In the fourth step, the feeding rate of the evaporation feeding device is 1 to 100g/min;
the carbon source gas is any one of methane, ethylene, acetylene, propylene or propane; the carrier gas is a mixed gas of nitrogen, argon, helium and hydrogen;
wherein the volume fraction of the carbon source gas is 5-45%; the volume fraction of the hydrogen is 0.1-80%, the rest is inert gas, and the flow is 1L/min-500L/min.
And step five, the winding and collecting speed of the winding and collecting device is 10 to 10000m/min.
The beneficial effects of the invention are as follows:
1. the molten liquid metal is used as an anode plasma arc furnace to provide a heat source for the growth of the single-walled carbon nanotubes, ultrahigh transient high temperature can be generated, the central plasma arc temperature can reach 20000 ℃ theoretically, the high-efficiency cracking of growth precursors and the catalyst evaporation can be ensured, huge driving energy is provided for the growth of the single-walled carbon nanotubes, the rapid reaction of high-concentration catalyst particles and a cracking carbon source is realized, the growth efficiency is greatly improved, and the yield is 2-3 orders of magnitude higher than that of the conventional floating chemical vapor deposition and plasma torch method.
2. According to the characteristics of the main catalyst and the second phase catalyst components, a separate feeding scheme is adopted, an organic metal compound serving as the main catalyst is fed in an evaporation pyrolysis mode, the second phase catalyst is mainly refractory metal, and is generated in situ in a furnace in a mode of directly thermally evaporating anode metal by adopting a plasma arc, so that the uneven components caused by the decomposition of catalyst raw materials and uneven evaporation temperature are avoided, the growth activity of the composite catalyst is obviously improved, and the high efficiency of the single-walled carbon nanotube is realized.
3. The second phase catalyst can control the evaporation rate of the anode metal by regulating and controlling the proportion of refractory metal components, so that the proportion of the main catalyst and the second phase catalyst is regulated and controlled, and the high-efficiency composite catalyst is obtained in a high-temperature plasma arc environment, meanwhile, the consumption of the anode metal is also delayed, the service life of the anode is prolonged, and long-acting stable operation is realized.
4. The aqueous solution containing the surfactant is used as the shrinkage coagulating bath, so that the wettability of the shrinkage coagulating bath to the carbon nano tube can be obviously improved, the shrinkage efficiency is obviously improved, the continuous and stable collection of the carbon nano tube fiber is obtained, and the broken ends caused by uneven infiltration are avoided.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 is a scanning electron micrograph of a single wall carbon nanotube product of the present invention;
FIG. 3 is a transmission electron micrograph of a single wall carbon nanotube of the present invention;
FIG. 4 is a Raman spectrum of a single-walled carbon nanotube according to the present invention;
FIG. 5 is a comparative table of product characterization indicators according to an embodiment of the present invention.
The figure shows: 1. a plasma arc furnace; 2. a cathode; 3. an anode; 4. an evaporation feeding device; 5. a reaction gas inlet; 6. shrinking and solidifying bath; 7. a winding and collecting device; 8. a discharge port; 41. heating the evaporator; 42. and a feed pump.
Detailed Description
In order to make the technical solution of the present invention better understood by a person skilled in the art, the present invention will be more clearly and more fully described below with reference to the accompanying drawings in the embodiments, and of course, the described embodiments are only a part of, but not all of, the present invention, and other embodiments obtained by a person skilled in the art without making any inventive effort are within the scope of the present invention.
As shown in fig. 1, a continuous preparation device of single-walled carbon nanotubes comprises a plasma arc furnace 1, wherein a cathode 2 and an anode 3 are arranged in the plasma arc furnace 1, the cathode 2 is connected with an evaporation feeding device 4, a reaction air inlet 5 and a discharge outlet 8 are arranged on the plasma arc furnace 1, a shrinkage solidification bath 6 is distributed at the discharge outlet 8, and a winding collecting device 7 is distributed above the shrinkage solidification bath 6;
the evaporation feed device 4 comprises a heating evaporator 41 connected with the cathode 2, and the heating evaporator 41 is connected with a feed pump 42.
The feed pump 42 is a syringe pump or peristaltic pump or the like.
The cathode 2 is a graphite electrode, the anode 3 is a high-melting-point alloy, a second-phase catalyst composed of refractory metal is contained in the anode 3, and the anode 3 takes part in the reaction by molten liquid metal; after voltage is applied, plasma arc discharge between the anode and the cathode is realized, anode metal can be melted or partially melted, the power supply power is 10-500 kW, the current is 100-5000A, and the voltage is 1-300V.
The shrinkage coagulation bath 6 is water or an aqueous solution containing a surfactant; the surfactant may be cationic, anionic, and nonionic surfactants, and combinations thereof.
A continuous process for the preparation of single-walled carbon nanotubes, comprising the steps of:
the first step: dissolving a cocatalyst consisting of a metal organic compound formed by any one of iron, cobalt and nickel and a chalcogen simple substance or a compound thereof in an organic solvent to prepare a single-walled carbon nanotube growth precursor;
and a second step of: loading a single-walled carbon nanotube growth precursor into the evaporation feed apparatus 4 while preheating the heating evaporator 41 to a specified temperature;
and a third step of: under the protection of hearth inert gas, introducing plasma arc gas from a cathode 2, energizing and exciting to generate a plasma arc, melting an anode 3 arranged in a plasma arc furnace 1 into a liquid state, and raising the hearth temperature of the plasma arc furnace 1 to a specified temperature;
fourth step: starting an evaporation feeding device 4, injecting a single-wall carbon nanotube growth precursor into a heating evaporator 41, introducing the single-wall carbon nanotube growth precursor into a plasma arc furnace from a cathode 2 under the drive of inert gas, introducing carbon source gas and carrier gas for reaction, and continuously discharging a product out of the plasma arc furnace 1 along with tail gas;
fifth step: the discharged single-walled carbon nanotube products are subjected to coagulation bath by a shrinkage coagulation bath 6 to obtain single-walled carbon nanotube bundles, and finally the single-walled carbon nanotube bundles are wound by a winding collecting device 7 to obtain the final single-walled carbon nanotubes.
In the first step, the organic metal compound is any one of carbonyl iron, ferrocene, nickel-dicyclopentadienyl and cobaltocene or any one of the derivatives of the materials, and the concentration of the precursor of the organic metal compound for growing the single-wall carbon nano tube is 2-20%; for example ferrocene derivatives include: the physical and chemical properties of the mono-polynuclear ferrocene complex, the ferrocenyl polymer, the chiral ferrocene complex, the ferrocene cluster derivative and the like are basically the same, so that the effect achieved by participating in the reaction is basically the same;
the promoter is any one of sulfur powder, selenium powder, thiophene and carbon disulfide, and the concentration of a precursor for growing the single-wall carbon nano tube is 0.01 to 2 percent;
the organic solvent is any one of benzene, toluene, xylene, acetone, liquid alkane, petroleum ether, ethanol and methanol.
The second step heats the evaporator 41 to a pre-specified temperature of 100 to 500 ℃.
The inert gas in the third step is any one of nitrogen, argon and helium;
the plasma arc gas is any one of nitrogen, argon, helium, hydrogen and steam and mixed gas of two or three of the gases in any mixing proportion, and the flow is 10L/min-500L/min;
the hearth temperature of the plasma arc furnace 1 is 600-1900 ℃;
the anode 3 is a high-melting-point alloy containing a second-phase catalyst, and is an alloy formed by iron, cobalt and nickel and refractory metals of molybdenum, tungsten, tantalum, niobium, hafnium and zirconium, wherein the refractory metal element proportion is 20-80%.
In the fourth step, the feeding rate of the evaporation feeding device 4 is 1 to 100g/min;
the carbon source gas is any one of methane, ethylene, acetylene, propylene or propane; the carrier gas is a mixed gas of nitrogen, argon, helium and hydrogen;
wherein the volume fraction of the carbon source gas is 5-45%; the volume fraction of the hydrogen is 0.1-80%, the rest is inert gas, and the flow is 1L/min-500L/min.
And step five, the winding and collecting speed of the winding and collecting device is 10 to 10000m/min.
The single-walled carbon nanotubes produced using the apparatus and method described above are presented in the following examples:
example 1
The power of the plasma arc furnace 1 is 150kW, the current is 100A, and the voltage is 10V; firstly preparing a single-walled carbon nanotube growth precursor solution, wherein 5% of ferrocene, 1% of thiophene and 96% of toluene are mixed; the precursor solution is charged into the evaporation feed apparatus 4 while the heating evaporator 41 is preheated to 350 ℃; then, argon inert gas is introduced into a hearth of the plasma arc furnace 1 for protection, argon arc gas is further introduced from the cathode 2, the flow rate is 50L/min, the plasma arc is generated by energizing and excitation, fe 40% -Mo 60% alloy of anode 3 metal in a graphite crucible of the plasma arc furnace 1 is melted into liquid state, and the temperature of the hearth is increased to 1500 ℃; starting an evaporation feeding device 4, and adjusting the feeding flow to 10g/min; simultaneously introducing carbon source gas and carrier gas, wherein the volume fraction ratio is 20% of methane, 40% of hydrogen and 40% of argon, and the total flow is 200L/min; the product is continuously produced at the discharge port 8, passes through the shrinkage coagulation bath 6, and is wound by the winding collecting device 7, wherein the winding linear speed is 100m/min. Fig. 2 shows a scanning electron micrograph of a single-walled carbon nanotube product, fig. 3 shows a transmission electron micrograph of a single-walled carbon nanotube product, and fig. 4 shows a raman spectrum of a single-walled carbon nanotube.
Example 2
The power of the plasma arc furnace 1 is 10kW, the current is 100A, and the voltage is 100V; firstly preparing a single-walled carbon nanotube growth precursor solution, wherein 2% of ferrocene, 0.01% of sulfur powder and 94.99% of toluene are contained; the precursor solution is charged into the evaporation feed apparatus 4 while preheating the heating evaporator 41 to 100 ℃; then, argon inert gas is introduced into a hearth of the plasma arc furnace 1 for protection, argon arc gas is further introduced from the cathode 2, the flow is 10L/min, the plasma arc is generated by energizing and excitation, the Fe 80% -W20% alloy of the anode 3 metal arranged in the graphite crucible is melted into a liquid state, and the temperature of the hearth is increased to 800 ℃; starting an evaporation feeding device 4, and adjusting the feeding flow to 1g/min; simultaneously introducing carbon source gas and carrier gas, wherein the volume fraction ratio is 45% of ethylene, 10% of hydrogen and 45% of nitrogen, and the total flow is 1L/min; the product is continuously produced at the discharge port 8, passes through the shrinkage coagulation bath 6, and then is wound by the winding collecting device 7, wherein the winding linear speed is 5m/min.
Example 3
The power of the plasma arc furnace 1 is 500kW, the current is 5000A, and the voltage is 100V; firstly preparing a single-walled carbon nanotube growth precursor solution, wherein 20% of ferrocene, 5% of thiophene and 75% of benzene are mixed; the precursor solution is charged into the evaporation feed apparatus 4 while the heating evaporator 41 is preheated to 500 ℃; then, argon inert gas is introduced into a hearth of the plasma arc furnace 1 for protection, argon arc gas is further introduced from the cathode 2, the flow rate is 500L/min, the plasma arc is generated by electrifying and exciting, the Fe 20% -Ta 80% alloy of the anode 3 metal in the graphite crucible of the plasma arc furnace 1 is melted into a liquid state, and the temperature of the hearth is increased to 1900 ℃; starting the evaporation feeding device 4, and adjusting the feeding flow to 100g/min; simultaneously introducing carbon source gas and carrier gas, wherein the volume fraction ratio is 10% of propylene, 80% of hydrogen and 10% of argon, and the total flow is 500L/min; the product can be continuously generated at the discharge port 8, and after the product passes through the shrinkage coagulation bath 6, the product is wound by a winding collecting device 7, and the winding linear speed is 10000m/min.
Comparative example 1
The comparative example adopts the same precursor solution as in example 1, adopts a floating chemical vapor deposition process for growth, has the same parameters of hearth temperature, carbon source gas, carrier gas and the like, and has a relatively low yield, the winding collection rate can only reach 2-5 m/min, and the product characterization index is shown in fig. 5 for comparison.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A continuous preparation device of single-walled carbon nanotubes is characterized in that: the device comprises a plasma arc furnace (1), wherein a cathode (2) and an anode (3) are arranged in the plasma arc furnace (1), the cathode (2) is connected with an evaporation feeding device (4), a reaction air inlet (5) and a discharge outlet (8) are arranged on the plasma arc furnace (1), a shrinkage solidification bath (6) is distributed at the discharge outlet (8), and a winding collecting device (7) is distributed above the shrinkage solidification bath (6);
the cathode (2) is a graphite electrode, the anode (3) is a high-melting-point alloy, a second-phase catalyst composed of refractory metals is contained in the anode (3), and the anode (3) takes part in the reaction by molten liquid metal.
2. The continuous production apparatus for single-walled carbon nanotubes according to claim 1, wherein: the evaporation feeding device (4) comprises a heating evaporator (41) connected with the cathode (2), and the heating evaporator (41) is connected with a feeding pump (42).
3. The continuous production apparatus for single-walled carbon nanotubes according to claim 2, wherein: the feed pump (42) is a syringe pump or peristaltic pump or the same type of product.
4. The continuous production apparatus for single-walled carbon nanotubes according to claim 1, wherein: the shrinkage coagulation bath (6) is water or an aqueous solution containing a surfactant.
5. A production method using a continuous production apparatus for single-walled carbon nanotubes according to any of claims 1 to 4, characterized in that: the method comprises the following steps:
the first step: dissolving a cocatalyst consisting of a metal organic compound formed by any one of iron, cobalt and nickel and a chalcogen simple substance or a compound thereof in an organic solvent to prepare a single-walled carbon nanotube growth precursor;
and a second step of: loading a single-walled carbon nanotube growth precursor into an evaporation feeding device (4), and simultaneously preheating a heating evaporator (41) to a specified temperature;
and a third step of: under the protection of hearth inert gas, a cathode (2) is charged with plasma arc gas, and is electrified to excite to generate plasma arc, so that an anode (3) arranged in the plasma arc furnace (1) is melted into a liquid state, and the hearth temperature of the plasma arc furnace (1) is increased to a specified temperature;
fourth step: starting an evaporation feeding device (4), injecting a single-walled carbon nanotube growth precursor into a heating evaporator (41), introducing the single-walled carbon nanotube growth precursor into a plasma arc furnace from a cathode (2) under the drive of inert gas, introducing carbon source gas and carrier gas for reaction, and continuously discharging a product out of the plasma arc furnace (1) along with tail gas;
fifth step: the discharged single-walled carbon nanotube products are subjected to coagulation bath through a shrinkage coagulation bath (6) to obtain single-walled carbon nanotube bundles, and finally the single-walled carbon nanotube bundles are wound by a winding collecting device (7) to obtain the final single-walled carbon nanotubes.
6. The continuous production method of single-walled carbon nanotubes according to claim 5, wherein: in the first step, the metal organic compound is any one of carbonyl iron, ferrocene, nickel-dicyclopentadienyl and cobaltocene or any one of the derivatives of the materials, and the concentration of the precursor of the metal organic compound for growing the single-wall carbon nano tube is 2-20%;
the promoter is any one of sulfur powder, selenium powder, thiophene and carbon disulfide, and the concentration of a precursor for growing the single-wall carbon nano tube is 0.01-2%;
the organic solvent is any one of benzene, toluene, xylene, acetone, liquid alkane, petroleum ether, ethanol and methanol.
7. The continuous production method of single-walled carbon nanotubes according to claim 5, wherein: the second step heats the evaporator (41) to a pre-specified temperature of 100 to 500 ℃.
8. The continuous production method of single-walled carbon nanotubes according to claim 5, wherein: the inert gas in the third step is any one of nitrogen, argon and helium;
the plasma arc gas is any one of nitrogen, argon, helium, hydrogen and steam and mixed gas of two or three of the gases in any mixing proportion, and the flow is 10L/min-500L/min;
the hearth temperature of the plasma arc furnace (1) is 600-1900 ℃;
the anode (3) is a high-melting-point alloy containing a second-phase catalyst and is an alloy formed by iron, cobalt and nickel and refractory metals of molybdenum, tungsten, tantalum, niobium, hafnium and zirconium, wherein the refractory metal element proportion is 20-80%.
9. The continuous production method of single-walled carbon nanotubes according to claim 5, wherein: in the fourth step, the feeding rate of the evaporation feeding device (4) is 1 to 100g/min;
the carbon source gas is any one of methane, ethylene, acetylene, propylene or propane; the carrier gas is a mixed gas of nitrogen, argon, helium and hydrogen;
wherein the volume fraction of the carbon source gas is 5-45%; the volume fraction of the hydrogen is 0.1-80%, the rest is inert gas, and the flow is 1L/min-500L/min.
10. The continuous production method of single-walled carbon nanotubes according to claim 5, wherein: and step five, the winding and collecting speed of the winding and collecting device is 10 to 10000m/min.
CN202410093966.8A 2024-01-23 2024-01-23 Continuous preparation device and preparation method of single-walled carbon nanotubes Pending CN117865132A (en)

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