CN115180614A - Continuous carbon nanotube aggregate synthesis device and use method - Google Patents

Continuous carbon nanotube aggregate synthesis device and use method Download PDF

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Publication number
CN115180614A
CN115180614A CN202210919338.1A CN202210919338A CN115180614A CN 115180614 A CN115180614 A CN 115180614A CN 202210919338 A CN202210919338 A CN 202210919338A CN 115180614 A CN115180614 A CN 115180614A
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temperature
furnace
reaction
carrier gas
combination
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钟小华
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Wuhan Carbon Weng Technology Co ltd
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Wuhan Carbon Weng Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Abstract

A continuous carbon nanotube aggregate synthesis device and a use method thereof are provided, wherein the synthesis device comprises a pressure vessel, an air inlet preheating system and a high-temperature reaction furnace; the application method comprises placing reactant raw materials in a pressure container, wherein the reactant raw materials comprise a carbon source, a catalyst and a reaction auxiliary agent; heating and pressurizing the pressure container to enable the reactant raw materials to be combined and gasified and to be mixed with each other, so as to obtain a gasified reactant; meanwhile, inputting the reaction carrier gas combination into an air inlet preheating system to preheat the reaction carrier gas combination so as to obtain thermal reaction carrier gas; subsequently, the gasification reactant and the thermal reaction carrier gas obtained as described above are introduced into a high-temperature reaction furnace together, and the high-temperature reaction furnace is heated to obtain a carbon nanotube aggregate. The design not only has higher efficiency of catalyzing and growing the carbon nano tube, but also has better quality of the carbon nano tube.

Description

Continuous carbon nanotube aggregate synthesis device and use method
Technical Field
The invention relates to a device and a method for a carbon nano tube film, belongs to the field of carbon nano tube preparation, and particularly relates to a device for synthesizing a continuous carbon nano tube aggregate and a using method thereof.
Background
Among the existing methods for synthesizing continuous carbon nanotube aggregates, chemical vapor deposition (CVD direct synthesis) generally uses a syringe pump to deliver reactant materials into a reactor, and the reactant materials are transported to a high temperature zone under the action of a carrier gas, and undergo a catalytic pyrolysis reaction to synthesize the continuous carbon nanotube aggregates, which can synthesize the continuous carbon nanotube aggregates, but has the following disadvantages:
because the different raw materials required temperature of gasification is different, lead to different raw materials by the time difference of gasification, then different raw materials enter into the gasification reaction zone and have the precedence, further lead to different raw materials can not carry out catalytic pyrolysis reaction simultaneously, cause the efficiency of catalytic growth carbon nanotube to reduce, simultaneously, reduce the quality of synthetic carbon nanotube.
The information disclosed in this background section is only for enhancement of understanding of the general background of the application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects and problems of low efficiency and poor quality of the synthesized carbon nano tube in the prior art, and provides a continuous carbon nano tube aggregate synthesizing device and a using method thereof, wherein the efficiency of synthesizing the carbon nano tube is high, and the quality of the carbon nano tube is good.
In order to achieve the above purpose, the technical solution of the invention is as follows:
a continuous carbon nanotube aggregate synthesizing apparatus, the synthesizing apparatus comprising: the system comprises a pressure container, an air inlet preheating system and a high-temperature reaction furnace;
the pressure container is connected with the high-temperature reaction furnace through a gas transmission pipeline, and a gas inlet preheating system is connected on the gas transmission pipeline between the pressure container and the high-temperature reaction furnace; the pressure container and the air inlet preheating system are communicated with the interior of the high-temperature reaction furnace.
The air inlet preheating system comprises a low-temperature furnace, a metal pipe, an air inlet pipe and an air outlet pipe, wherein the metal pipe is sleeved on the outer wall of the low-temperature furnace, one end of the low-temperature furnace is connected with the air inlet pipe, the other end of the low-temperature furnace is connected with one end of the air outlet pipe, and the other end of the air outlet pipe is connected with a gas transmission pipeline; a first flowmeter is arranged on the gas outlet pipe, and a second flowmeter is arranged on a gas transmission pipeline between the pressure container and the gas outlet pipe;
the high-temperature reaction furnace comprises a high-temperature furnace and a quartz tube arranged in the high-temperature furnace, and the pressure container is connected with the quartz tube through a gas transmission pipeline.
The furnace temperature of the low-temperature furnace is as follows: 200-800 ℃.
A method of using a continuous carbon nanotube aggregate synthesis apparatus, the method comprising the steps of:
firstly, placing a reactant raw material combination into a pressure container, wherein the reactant raw material combination comprises a carbon source, a catalyst and a reaction auxiliary agent; heating and pressurizing the pressure container to enable the reactant raw materials to be combined and gasified and to be mixed with each other, so as to obtain a gasified reactant;
meanwhile, inputting the reaction carrier gas combination into an air inlet preheating system to preheat the reaction carrier gas combination so as to obtain thermal reaction carrier gas;
then, the obtained gasification reactant and the thermal reaction carrier gas are input into a high-temperature reaction furnace together, and the high-temperature reaction furnace is heated to obtain the carbon nano tube aggregate.
The gasification reactant and hot reaction carrier gas are input into the high-temperature reaction furnace together, and the input flow of the gasification reactant is controlled by a first flow meter;
and the gasification reactant and the hot reaction carrier gas are input into the high-temperature reaction furnace together, and the input flow of the hot reaction carrier gas is controlled by a second flowmeter.
The first flow meter controls the flow of the gasification reactants to be as follows: 0.1L-10L/min; the flow of the thermal reaction carrier gas controlled by the second flowmeter is as follows: 0.1L-50L/min.
The carbon source comprises any one or any combination of methanol, ethanol, gasoline, n-hexane, toluene, xylene and tetrahydrofuran;
the catalyst comprises any one or any combination of ferrocene, nickel acetate and cobalt acetate;
the reaction auxiliary agent comprises any one or any combination of thiophene, sulfur and metal organic molybdenum;
the reaction carrier gas combination comprises hydrogen and other gases, and the other gases comprise any one or any combination of nitrogen, argon and helium.
The reactant raw material combination is any one of the following combinations:
ethanol/ferrocene/sulfur, toluene/ferrocene/sulfur, xylene/ferrocene/sulfur, n-hexane/ferrocene/sulfur, xylene/ferrocene/thiophene, toluene/ferrocene/thiophene, n-hexane/ferrocene/thiophene, tetrahydrofuran/ferrocene/thiophene.
The dosage ratio of the carbon source, the catalyst and the reaction auxiliary agent is as follows: fe = 10-1000: 1 (molar ratio); s: fe = 0.01-1: 1 (molar ratio); wherein C is a carbon source, fe is a catalyst, and S is a reaction auxiliary agent;
the reaction carrier gas composition comprises the following components in percentage by volume: hydrogen to other gases =5% -100%: 95% -0%, and the other gas is any one or any combination of the following gases: nitrogen, argon, helium.
The heating temperature in the heating and pressurizing of the pressure container is as follows: the pressure is between 200 and 300 ℃, and the pressurizing pressure is as follows: 0.001-10 Mpa;
the reaction carrier gas combination is preheated at the temperature of: the temperature is 300-600 ℃;
the high-temperature reaction furnace is heated, and the heating temperature is as follows: 1060 ℃ to 1300 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a continuous carbon nanotube aggregate synthesis device and a using method thereof, wherein the synthesis device comprises a pressure container, an air inlet preheating system and a high-temperature reaction furnace, the air inlet preheating system comprises a low-temperature furnace, a metal pipe, an air inlet pipe and an air outlet pipe, the metal pipe is sleeved on the outer wall of the low-temperature furnace, one end of the low-temperature furnace is connected with the air inlet pipe, the other end of the low-temperature furnace is connected with one end of the air outlet pipe, and the other end of the air outlet pipe is connected with a gas transmission pipeline; a first flowmeter is arranged on the gas outlet pipe, and a second flowmeter is arranged on the gas transmission pipeline between the pressure container and the gas outlet pipe; the high-temperature reaction furnace comprises a high-temperature furnace and a quartz tube arranged in the high-temperature furnace, and the pressure container is connected with the quartz tube through a gas transmission pipeline; in application, different reaction raw materials are gasified together by a pressure container and are fully mixed with each other; meanwhile, the gas inlet preheating system preheats the reaction carrier gas, so that the phenomenon that the temperature difference between the reaction carrier gas and the reactant raw material is too large to influence the catalytic pyrolysis reaction is avoided; the gasified reaction raw materials and the reaction carrier gas enter the high-temperature reaction furnace together through the control of the flow meter to carry out catalytic pyrolysis reaction to synthesize the carbon nano tube aggregate, so that the operation time is saved, the operation efficiency is improved, the reaction raw materials are uniformly mixed in advance and simultaneously carry out catalytic pyrolysis reaction, and the synthesized carbon nano tube aggregate has uniform quality and higher purity. Therefore, the invention not only has higher efficiency of synthesizing the carbon nano tube, but also has better quality of the synthesized carbon nano tube.
2. In the invention, the use method comprises the following steps: firstly, putting reactant raw material combination into a pressure container, heating and pressurizing the pressure container to gasify the reactant raw material combination, and mixing the reactant raw material combination and the reactant raw material combination to obtain gasified reactant; meanwhile, inputting the reaction carrier gas combination into an air inlet preheating system to preheat the reaction carrier gas combination so as to obtain thermal reaction carrier gas; then, controlling the input flow of the obtained gasification reactant through a first flow meter, controlling the input flow of thermal reaction carrier gas through a second flow meter, inputting the thermal reaction carrier gas and the thermal reaction carrier gas into the high-temperature reaction furnace together, and heating the high-temperature reaction furnace to obtain a carbon nano tube aggregate; in application, the reactant raw material combination is gasified and fully and uniformly mixed in the pressure container, meanwhile, the preheating of the reaction carrier gas is synchronously carried out, and the gasified reactant raw material combination and the thermal reaction carrier gas are simultaneously input into the high-temperature reaction furnace for catalytic pyrolysis reaction under the accurate control of the flow meter, so that the condition that different raw materials are required to be subjected to different gasification operations is avoided, the synthesis efficiency is reduced, and the quality of the synthesized carbon nano tube is reduced. Therefore, the invention not only has higher efficiency of catalyzing and growing the carbon nano tube, but also has better quality of the synthesized carbon nano tube.
3. In the device for synthesizing the continuous carbon nanotube aggregate and the using method, a carbon source comprises any one or any combination of methanol, ethanol, gasoline, normal hexane, toluene, xylene and tetrahydrofuran; the catalyst comprises any one or any combination of ferrocene, nickel acetate and cobalt acetate; the reaction auxiliary agent comprises any one or any combination of thiophene, sulfur and metal organic molybdenum; the reaction carrier gas combination comprises hydrogen and other gases, and the other gases comprise any one or any combination of nitrogen, argon and helium; in application, these raw materials are relatively easily available, and are combined by different requirements, which is beneficial to reducing the cost. Therefore, the invention can synthesize the carbon nano tube aggregate with low cost.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is a schematic view of the structure of the inlet preheating system and the high temperature heating furnace of the present invention.
Fig. 3 is a schematic step diagram of a method for using a continuous carbon nanotube aggregate synthesizing apparatus according to the present invention.
In the figure: the device comprises a pressure container 1, an air inlet preheating system 2, a low-temperature furnace 21, a metal tube 22, an air inlet tube 23, an air outlet tube 24, a high-temperature reaction furnace 3, a high-temperature furnace 31, a quartz tube 32, a gas transmission pipeline 4, a reactant raw material combination 5, a reaction carrier gas combination 6, a carbon nano tube aggregate 7, a first flowmeter 8 and a second flowmeter 9.
Detailed Description
The present invention will be described in further detail with reference to the following description and embodiments in conjunction with the accompanying drawings.
Referring to fig. 1 to 3, a continuous carbon nanotube aggregate synthesizing apparatus, the synthesizing apparatus comprising: the system comprises a pressure vessel 1, an air inlet preheating system 2 and a high-temperature reaction furnace 3;
the pressure vessel 1 is connected with the high-temperature reaction furnace 3 through a gas transmission pipeline 4, and a gas inlet preheating system 2 is connected on the gas transmission pipeline 4 between the pressure vessel 1 and the high-temperature reaction furnace 3; the pressure vessel 1 and the air inlet preheating system 2 are communicated with the interior of the high-temperature reaction furnace 3.
The air inlet preheating system 2 comprises a low-temperature furnace 21, a metal pipe 22, an air inlet pipe 23 and an air outlet pipe 24, wherein the metal pipe 22 is sleeved on the outer wall of the low-temperature furnace 21, one end of the low-temperature furnace 21 is connected with the air inlet pipe 23, the other end of the low-temperature furnace 21 is connected with one end of the air outlet pipe 24, and the other end of the air outlet pipe 24 is connected with the air transmission pipeline 4; a first flowmeter 8 is arranged on the gas outlet pipe, and a second flowmeter 9 is arranged on the gas transmission pipeline 4 between the pressure container 1 and the gas outlet pipe 24;
the high-temperature reaction furnace 3 comprises a high-temperature furnace 31 and a quartz tube 32 arranged in the high-temperature furnace 31, and the pressure container 1 is connected with the quartz tube 32 through a gas transmission pipeline 4.
The furnace temperature of the low temperature furnace 21 is: 200-800 ℃.
A method of using a continuous carbon nanotube aggregate synthesis apparatus, the method of using comprising the steps of:
firstly, placing a reactant raw material combination 5 into a pressure vessel 1, wherein the reactant raw material combination 5 comprises a carbon source, a catalyst and a reaction auxiliary agent; heating and pressurizing the pressure container 1 to gasify the reactant raw material combination 5, and mixing the reactant raw material combination and the reactant raw material combination with each other to obtain a gasified reactant;
meanwhile, inputting the reaction carrier gas combination 6 into the inlet gas preheating system 2 to preheat the reaction carrier gas combination 6, thereby obtaining thermal reaction carrier gas;
subsequently, the gasification reactant obtained as described above and a thermal reaction carrier gas are fed together into the high-temperature reaction furnace 3, and the high-temperature reaction furnace 3 is heated to obtain the carbon nanotube aggregate 7.
The gasification reactant and the hot reaction carrier gas are input into the high-temperature reaction furnace 3 together, and the input flow of the gasification reactant is controlled by a first flowmeter 8;
the gasification reactant and the thermal reaction carrier gas are input into the high-temperature reaction furnace 3 together, and the input flow of the thermal reaction carrier gas is controlled by a second flowmeter 9.
The flow rate of the gasification reactant controlled by the first flow meter 8 is as follows: 0.1L-10L/min; the flow rate of the thermal reaction carrier gas controlled by the second flowmeter 9 is as follows: 0.1L-50L/min.
The carbon source comprises any one or any combination of methanol, ethanol, gasoline, n-hexane, toluene, xylene and tetrahydrofuran;
the catalyst comprises any one or any combination of ferrocene, nickel acetate and cobalt acetate;
the reaction auxiliary agent comprises any one or any combination of thiophene, sulfur and metal organic molybdenum;
the reaction carrier gas combination 6 comprises hydrogen gas and other gases including any one or any combination of nitrogen, argon, helium.
The reactant raw material combination 5 is any one of the following combinations:
ethanol/ferrocene/sulfur, toluene/ferrocene/sulfur, xylene/ferrocene/sulfur, n-hexane/ferrocene/sulfur, xylene/ferrocene/thiophene, toluene/ferrocene/thiophene, n-hexane/ferrocene/thiophene, tetrahydrofuran/ferrocene/thiophene.
The dosage ratio of the carbon source, the catalyst and the reaction auxiliary agent is as follows: fe = 10-1000: 1 (molar ratio); s: fe = 0.01-1: 1 (molar ratio); wherein C is a carbon source, fe is a catalyst, and S is a reaction auxiliary agent;
the reaction carrier gas combination 6 comprises the following components in percentage by volume: hydrogen to other gases =5% -100%: 95% -0%, and the other gas is any one or any combination of the following gases: nitrogen, argon, helium.
The heating temperature in heating and pressurizing the pressure vessel 1 is as follows: the pressure is between 200 and 300 ℃, and the pressurizing pressure is as follows: 0.001-10 Mpa;
the reaction carrier gas combination 6 is preheated at the temperature of: the temperature is 300-600 ℃;
the high-temperature reaction furnace 3 is heated at the following temperature: 1060 ℃ to 1300 ℃.
The principle of the invention is illustrated as follows:
in the device and the method for synthesizing the continuous carbon nanotube aggregate, the pressure gauge is arranged at the top of the pressure container, the pressure container can be monitored through the pressure gauge, if the pressure is too high, danger is shown, and if the pressure is too low, the reactant is completely consumed; the pressure performance parameters of the pressure container adopted in the synthesis device are as follows: 0.001 MPa-10 MPa; the length of a metal pipe of the air inlet preheating system is 1000 mm-2000 mm; the diameter of the air inlet pipe is 2 mm-6 mm, and the diameter of the air outlet pipe is 2 mm-4 mm.
When the method is applied, firstly, a carbon source, a catalyst and a reaction auxiliary agent are proportioned as required to prepare a reactant raw material combination, then the reactant raw material combination is placed into a pressure container at one time, the pressure container is heated and pressurized, the reactant raw material combination can be gasified into molecular size under the action of high temperature and high pressure, the gasified reactant raw material molecules are uniformly mixed together, meanwhile, a reaction carrier gas is proportioned into the reaction carrier gas combination as required, the reaction carrier gas combination is input into a low-temperature furnace through an air inlet, the low-temperature furnace is heated by using a metal pipe to preheat the reaction carrier gas combination, the gasification work and the preheating work are carried out simultaneously, and the operation steps and the operation time are greatly saved; after the gasification work and the preheating work are finished, the gasification reactant and the thermal reaction carrier gas are in the optimal proportion under the control of the flow meter; the gasification reactant and the thermal reaction carrier gas are input into the high-temperature reaction furnace together, the high-temperature reaction furnace is heated, and the reactant raw materials grow on the quartz tube 32 at the same time, so as to obtain the carbon nano tube aggregate; because different reactant raw materials are gasified and uniformly mixed and then enter the high-temperature reaction furnace at the same time, the carbon nano tube cannot be reacted unevenly because of sequentially entering the high-temperature reaction furnace, the reaction uniformity is improved, and the quality of the carbon nano tube is further improved.
Example 1:
a continuous carbon nanotube aggregate synthesizing apparatus, the synthesizing apparatus comprising: the system comprises a pressure vessel 1, an air inlet preheating system 2 and a high-temperature reaction furnace 3; the pressure vessel 1 is connected with the high-temperature reaction furnace 3 through a gas transmission pipeline 4, and a gas inlet preheating system 2 is connected on the gas transmission pipeline 4 between the pressure vessel 1 and the high-temperature reaction furnace 3; the pressure vessel 1 and the air inlet preheating system 2 are communicated with the interior of the high-temperature reaction furnace 3. The inlet air preheating system 2 comprises a low-temperature furnace 21, a metal pipe 22, an inlet pipe 23 and an outlet pipe 24, wherein the metal pipe 22 is sleeved on the outer wall of the low-temperature furnace 21, one end of the low-temperature furnace 21 is connected with the inlet pipe 23, the other end of the low-temperature furnace 21 is connected with one end of the outlet pipe 24, and the other end of the outlet pipe 24 is connected with the gas transmission pipeline 4; a first flowmeter 8 is arranged on the gas outlet pipe, and a second flowmeter 9 is arranged on the gas transmission pipeline 4 between the pressure container 1 and the gas outlet pipe 24; the high-temperature reaction furnace 3 comprises a high-temperature furnace 31 and a quartz tube 32 arranged in the high-temperature furnace 31, and the pressure container 1 is connected with the quartz tube 32 through a gas transmission pipeline 4.
The using method of the synthesis device comprises the following steps: firstly, placing a reactant raw material combination 5 into a pressure vessel 1, wherein the reactant raw material combination 5 comprises a carbon source, a catalyst and a reaction auxiliary agent; heating and pressurizing the pressure container 1 to gasify the reactant raw material combination 5, and mixing the reactant raw material combination and the reactant raw material combination with each other to obtain a gasified reactant; meanwhile, inputting the reaction carrier gas combination 6 into the inlet gas preheating system 2 to preheat the reaction carrier gas combination 6, thereby obtaining thermal reaction carrier gas; subsequently, the gasification reactant obtained as described above and a hot reaction carrier gas are introduced into the high-temperature reaction furnace 3 together, and the high-temperature reaction furnace 3 is heated to obtain the carbon nanotube aggregate 7.
Example 2:
the basic content is the same as that of the embodiment 2, except that:
the gasification reactant and the hot reaction carrier gas are input into the high-temperature reaction furnace 3 together, and the input flow rate of the gasification reactant is controlled by a first flow meter 8 (preferably a rotor flow meter); the gasification reactant is fed into the high temperature reactor 3 together with a hot reaction carrier gas, the flow rate of which is controlled by a second flow meter 9 (preferably a rotameter).
When the catalytic pyrolysis reactor is applied, the preferred rotor flow meter can improve the control precision of flow, reduce the control difficulty of catalytic pyrolysis reaction, and improve the stability of catalytic pyrolysis reaction.
Example 3:
the basic contents are the same as example 1, except that:
the carbon source comprises any one or any combination of methanol, ethanol, gasoline, n-hexane, toluene, xylene and tetrahydrofuran; the catalyst comprises any one or any combination of ferrocene, nickel acetate and cobalt acetate; the reaction auxiliary agent comprises any one or any combination of thiophene, sulfur and metal organic molybdenum; the reaction carrier gas combination 6 comprises hydrogen and other gases, and the other gases comprise any one or any combination of nitrogen, argon and helium; the reactant raw material combination 5 is any one of the following combinations: ethanol/ferrocene/sulfur, toluene/ferrocene/sulfur, xylene/ferrocene/sulfur, n-hexane/ferrocene/sulfur, xylene/ferrocene/thiophene, toluene/ferrocene/thiophene, n-hexane/ferrocene/thiophene, tetrahydrofuran/ferrocene/thiophene.
When the method is applied, the optimal combination of the carbon source, the catalyst and the reaction auxiliary agent is selected according to different requirements, so that the product quality is improved, the cost is reduced, and the economic benefit is improved.
Example 4:
the basic contents are the same as example 1, except that:
the heating temperature in the heating and pressurizing of the pressure vessel 1 is as follows: the pressure is between 200 and 300 ℃, and the pressurizing pressure is as follows: 0.001 Mpa-10 Mpa.
When the gasification furnace is used, the temperature can gasify the reactants, but does not cause decomposition of the reactants, so that the stability of the reactants during gasification is improved.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention as set forth in the appended claims.

Claims (10)

1. A continuous carbon nanotube aggregate synthesizing apparatus, comprising: the device comprises a pressure container (1), an air inlet preheating system (2) and a high-temperature reaction furnace (3);
the pressure container (1) is connected with the high-temperature reaction furnace (3) through a gas transmission pipeline (4), and a gas inlet preheating system (2) is connected on the gas transmission pipeline (4) between the pressure container (1) and the high-temperature reaction furnace (3); the pressure vessel (1) and the air inlet preheating system (2) are communicated with the interior of the high-temperature reaction furnace (3).
2. The apparatus for synthesizing continuous carbon nanotube assembly as set forth in claim 1, wherein:
the inlet air preheating system (2) comprises a low-temperature furnace (21), a metal pipe (22), an air inlet pipe (23) and an air outlet pipe (24), wherein the metal pipe (22) is sleeved on the outer wall of the low-temperature furnace (21), one end of the low-temperature furnace (21) is connected with the air inlet pipe (23), the other end of the low-temperature furnace (21) is connected with one end of the air outlet pipe (24), and the other end of the air outlet pipe (24) is connected with the air transmission pipeline (4); a first flowmeter (8) is arranged on the air outlet pipe, and a second flowmeter (9) is arranged on the gas transmission pipeline (4) between the pressure container (1) and the air outlet pipe (24);
the high-temperature reaction furnace (3) comprises a high-temperature furnace (31) and a quartz tube (32) arranged in the high-temperature furnace (31), and the pressure container (1) is connected with the quartz tube (32) through a gas transmission pipeline (4).
3. The apparatus for synthesizing continuous carbon nanotube assembly as set forth in claim 2, wherein:
the furnace temperature of the low-temperature furnace (21) is as follows: 200-800 ℃.
4. A method of using the apparatus for continuous carbon nanotube aggregate synthesis of claim 1, 2 or 3, comprising the steps of:
firstly, placing a reactant raw material combination (5) into a pressure container (1), wherein the reactant raw material combination (5) comprises a carbon source, a catalyst and a reaction auxiliary agent; heating and pressurizing the pressure container (1) to gasify the reactant raw material combination (5) and mutually mix the reactant raw material combination to obtain a gasified reactant;
meanwhile, inputting the reaction carrier gas combination (6) into the air inlet preheating system (2) to preheat the reaction carrier gas combination (6) so as to obtain hot reaction carrier gas;
subsequently, the gasification reactant obtained as described above is introduced into the high-temperature reaction furnace (3) together with a hot reaction carrier gas, and the high-temperature reaction furnace (3) is heated to obtain a carbon nanotube aggregate (7).
5. The method of claim 4, wherein the apparatus comprises:
the gasification reactant and hot reaction carrier gas are input into the high-temperature reaction furnace (3) together, and the input flow rate of the gasification reactant is controlled by a first flow meter (8);
the gasification reactant and the hot reaction carrier gas are input into the high-temperature reaction furnace (3) together, and the input flow rate of the hot reaction carrier gas is controlled by a second flow meter (9).
6. The method of claim 5, wherein the apparatus comprises:
the flow rate of the gasification reactant controlled by the first flow meter (8) is as follows: 0.1L-10L/min; the flow rate of the thermal reaction carrier gas controlled by the second flowmeter (9) is as follows: 0.1L-50L/min.
7. The method of claim 4, wherein the apparatus comprises:
the carbon source comprises any one or any combination of methanol, ethanol, gasoline, n-hexane, toluene, xylene and tetrahydrofuran;
the catalyst comprises any one or any combination of ferrocene, nickel acetate and cobalt acetate;
the reaction auxiliary agent comprises any one or any combination of thiophene, sulfur and metal organic molybdenum;
the reaction carrier gas combination (6) comprises hydrogen and other gases, and the other gases comprise any one or any combination of nitrogen, argon and helium.
8. The method of claim 7, wherein the apparatus comprises:
the reactant raw material combination (5) is any one of the following combinations:
ethanol/ferrocene/sulfur, n-hexane/ferrocene/sulfur, toluene/ferrocene/sulfur, xylene/ferrocene/thiophene, n-hexane/ferrocene/thiophene, toluene/ferrocene/thiophene, tetrahydrofuran/ferrocene/thiophene.
9. The method of claim 4, wherein the apparatus comprises:
the dosage ratio of the carbon source, the catalyst and the reaction auxiliary agent is as follows: fe = 10-1000: 1 (molar ratio); s: fe = 0.01-1: 1 (molar ratio); wherein C is a carbon source, fe is a catalyst, and S is a reaction auxiliary agent;
the reaction carrier gas combination (6) comprises the following components in percentage by volume: hydrogen to other gases =5% -100%: 95% -0%, and the other gas is any one or any combination of the following gases: nitrogen, argon, helium.
10. The method of claim 4, wherein the apparatus comprises:
the heating temperature in the heating and pressurizing of the pressure container (1) is as follows: the pressure is between 200 and 300 ℃, and the pressurizing pressure is as follows: 0.001-10 Mpa;
the reaction carrier gas combination (6) is preheated at the temperature: the temperature is 300-600 ℃;
the high-temperature reaction furnace (3) is heated at the following temperature: 1060 ℃ to 1300 ℃.
CN202210919338.1A 2022-08-02 2022-08-02 Continuous carbon nanotube aggregate synthesis device and use method Pending CN115180614A (en)

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Citations (7)

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