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CN212954323U - Gas phase damping method carbon nano tube generator - Google Patents

Gas phase damping method carbon nano tube generator Download PDF

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Publication number
CN212954323U
CN212954323U CN202020309388.4U CN202020309388U CN212954323U CN 212954323 U CN212954323 U CN 212954323U CN 202020309388 U CN202020309388 U CN 202020309388U CN 212954323 U CN212954323 U CN 212954323U
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gas
filter
carbon nanotube
port
cooling chamber
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宀冲北
岳山
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Chengdu Kehui Electromechanical Technology Co.,Ltd.
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Inner Mongolia Juncheng New Energy Technology Co ltd
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Abstract

The utility model relates to a gas phase damping method carbon nanotube generator, which comprises a filter and a cooling chamber which is positioned below the filter and is communicated with the filter; a heating furnace disposed outside the filter for heating the filter; the upper part of the filter is provided with a waste gas port and a feed inlet, the lower part of the filter is provided with a first gas inlet, a gas source valve and a discharge port, and a vibrating screen and one or more circles of gas phase damping rings are sequentially arranged between the feed inlet and the first gas inlet as well as between the feed inlet and the gas source valve; the discharge gate switches on with the cooling chamber, is provided with the nitrogen gas mouth between discharge gate and the cooling chamber, is provided with the baiting valve between nitrogen gas mouth and the cooling chamber, and this scheme mainly used gaseous phase damping method preparation or purification carbon nanotube's response device to reduce carbon nanotube's impurity, avoid metal to remain, can also solve traditional preparation technology catalyst and the insufficient problem of hydrocarbon contact.

Description

Gas phase damping method carbon nano tube generator
Technical Field
The utility model relates to a carbon nanotube reaction equipment, concretely relates to gaseous phase damping method carbon nanotube generator.
Background
The carbon nano tube is a novel material which is attractive to the world, has an ultra-large specific surface area, light weight, but ultra-strong mechanical strength, excellent conductivity and good physical and chemical stability, and has wide application prospects in the fields of lithium ion battery conductive agents, catalyst carriers, drug carriers, reinforced blending materials, electronic devices and the like.
Carbon nanotubes have been produced by Chemical Vapor Deposition (CVD) at low cost in large quantities. The chemical vapor deposition method is to crack hydrocarbon by using a catalyst, and to deposit carbon atoms with active metal atoms as catalyst crystal nuclei to form carbon nanotubes. According to the principle of the chemical vapor deposition method, the more fully the catalyst active component contacts with the carbon source gas, the more carbon atoms generated by the cracking of the carbon-hydrogen bond are deposited and grown on the surface of the active metal, the more carbon nanotubes are grown, and the better the growth morphology is. In engineering production, the chemical deposition method mainly adopts a moving method and a boiling method (also called a fluidized bed method). The moving method uses the material boat as a carrier, the catalyst is put into the material boat to move in the tube furnace of the tube furnace, and the carbon nano tube grows in the condition equipment area; in the production process of the moving method, the catalyst is fixed in the material boat and completely depends on the carbon source gas to be deposited on the catalyst stacking surface of the material boat and permeate into the catalyst, namely, the catalyst is passively contacted with the carbon source gas, so the defects that the catalyst is not fully contacted with hydrocarbon, the growth of the carbon nano tube is influenced and the like exist, the catalyst can only be used for preparing the carbon nano tube with low multiplying power, and methane is usually used as a carbon source. Meanwhile, catalyst metals (mainly Fe-based, Ni-based, Co-based, and the like) used in the CVD method remain in the carbon nanotubes, and many of them are coated on the ends of the carbon nanotubes. This has severely hindered the application of carbon nanotubes in some industries where the requirements for metal impurities are high, such as in lithium ion battery conductive agents and precision electronic devices.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's not enough, provide a gaseous phase damping method carbon nanotube generator, mainly used gaseous phase damping method preparation or purification carbon nanotube's response device to reduce carbon nanotube's impurity, avoid the metal to remain, can also solve traditional preparation technology catalyst and the insufficient problem of hydrocarbon contact.
The purpose of the utility model is realized through the following technical scheme:
a vapor damping carbon nanotube generator comprising:
the cooling chamber is positioned below the filter and communicated with the filter;
a heating furnace disposed outside the filter for heating the filter;
the upper part of the filter is provided with a waste gas port and a feed inlet, the lower part of the filter is provided with a first gas inlet, a gas source valve and a discharge port, and a vibrating screen and one or more circles of gas phase damping rings are sequentially arranged between the feed inlet and the first gas inlet as well as between the feed inlet and the gas source valve;
the discharge port is communicated with the cooling chamber, a nitrogen port is arranged between the discharge port and the cooling chamber, and a discharge valve is arranged between the nitrogen port and the cooling chamber.
The working principle is illustrated, taking a purified carbon nanotube as an example, after the multi-walled carbon nanotube synthesized by a catalyst is loaded into a vibrating screen through a feed inlet, closing the feed inlet, opening an exhaust gas port, opening a nitrogen port to introduce nitrogen, replacing air in a filter purification chamber, when the oxygen content is lower than 1%, closing the exhaust gas port and the nitrogen port, raising the temperature to 1100 ℃, feeding the filter purification chamber by using the vibrating screen, simultaneously opening an air source valve of a gas-phase damping ring, generating gas-phase damping by using the gas-phase damping ring, and damping the falling speed of the carbon nanotube in the purification chamber; and opening the first gas inlet to introduce chlorine gas at 1.5m3/h for reaction for 0.5 h. Stopping introducing chlorine after the reaction is finished, opening the waste gas port and the nitrogen port, introducing nitrogen, keeping the temperature at 1100 ℃ for 10 minutes, stopping heating, continuously introducing nitrogen, and closing the waste gas port and the nitrogen port when the temperature is lower than 40 ℃; and opening the discharge valve, taking out the carbon nano tube, putting the carbon nano tube into a sample bag, sealing, and absorbing tail gas in the whole process by using a sodium hydroxide aqueous solution.
Furthermore, the heating furnace is a vertical heating furnace and is arranged on the side wall of the filter in a surrounding mode.
Further, the exhaust gas port is provided at the top end of the filter.
Further, the vibrating screen is a pneumatic ultrasonic vibrating screen.
Furthermore, the discharge gate is located the bottom of filter, and the charge door setting is at filter lower part lateral wall, and first air inlet, air supply valve set up at filter upper portion lateral wall.
Further, the first air inlet and the air source valve are symmetrically arranged.
Further, the cooling chamber is provided with an air outlet, and the air outlet is provided with a control valve.
Furthermore, the discharge port is connected with the cooling chamber through a pipeline, the side wall of the pipeline is provided with the nitrogen port, and the discharge valve is arranged on the pipeline between the nitrogen port and the cooling chamber.
Further, when the gas phase damping ring is a plurality of rings, the distance between adjacent gas phase damping rings is gradually increased from the feed inlet to the discharge outlet.
Further, both ends of the filter are conical.
The utility model has the advantages that:
1) feeding the carbon nano tube ultrasonic vibration sieve in a purification chamber, moving the carbon nano tube from top to bottom by means of the self gravity of the carbon nano tube, and contacting the purification chamber with purified gas to enable metal impurities in the carbon nano tube to react with the purified gas to generate metal chloride, wherein the metal chloride is discharged from an exhaust gas port after passing through a filter in a gaseous state at a lower temperature to realize the separation of the metal impurities from the carbon nano tube, and finally preparing the hollow fibrous high-purity carbon nano tube; the ultrasonic vibration sieve can realize the quantitative supply of the carbon nano tube;
2) the multistage gas-phase damping rings are arranged in the purification chamber to damp and control the falling speed of the carbon nano tube, so that the floating time of the carbon nano tube in the purification chamber is prolonged, the carbon nano tube is fully contacted with purified gas, the purified gas can fully react with metal impurities in the carbon nano tube, the metal impurities can be fully removed, and the obtained carbon nano tube has good appearance, uniform particle size and high purity;
3) the carbon nano tubes of different catalysts can be purified by adjusting the frequency of the ultrasonic vibration sieve, the mesh number of the sieve, the feeding and metering of the carbon nano tubes, the purification temperature, the number of gas-phase damping rings and other measures, and the application range of the purification production of the carbon nano tubes is greatly enlarged.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
The technical solution of the present invention is described in further detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.
As shown in fig. 1, a vapor damping method carbon nanotube generator includes: a filter 1, and a cooling chamber 2 located below the filter 1 and in communication therewith; a heating furnace 3 disposed outside the filter 1 for heating the filter 1; the upper part of the filter 1 is provided with a waste gas port 6 and a feed inlet 7, the lower part of the filter 1 is provided with a first gas inlet 8, a gas source valve 9 and a discharge port 14, a vibrating screen 4 and one or more circles of gas-phase damping rings 5 are sequentially arranged between the feed inlet 7 and the first gas inlet 8 as well as between the feed inlet 7 and the gas source valve 9, and in order to improve the purity of the carbon nano tube, the gas-phase damping rings 5 are generally designed into a plurality of circles; the discharge port 14 is communicated with the cooling chamber 2, a nitrogen port 10 is arranged between the discharge port 14 and the cooling chamber 2, and a discharge valve 11 is arranged between the nitrogen port and the cooling chamber 2. As a preferred embodiment, the heating furnace 3 is a vertical heating furnace and is arranged on the side wall of the filter 1 in a surrounding manner, namely, the heating furnace 3 is annular and is arranged coaxially with the filter 1. The waste gas port 6 is arranged at the top end of the filter 1, and the vibrating screen 4 adopts a pneumatic ultrasonic vibrating screen. The discharge port 14 is positioned at the bottom end of the filter 1, the feed port 7 is arranged on the side wall of the lower part of the filter 1, and the first air inlet 8 and the air source valve 9 are arranged on the side wall of the upper part of the filter 1. The first air inlet 8 and the air supply valve 9 are symmetrically arranged. The cooling chamber 2 is provided with an air outlet 13, which air outlet 13 is provided with a control valve 12. The discharge port 14 is connected with the cooling chamber 2 through a pipeline, a nitrogen port 10 is arranged on the side wall of the pipeline, and a discharge valve 11 is arranged on the pipeline between the nitrogen port 10 and the cooling chamber 2. When the gas phase damping ring 5 is a plurality of rings, the distance between the adjacent gas phase damping rings 5 is gradually increased from the feed opening 7 to the discharge opening 14. The filter 1 is tapered at both ends.
The operation method for purifying the carbon nano tube comprises the following steps: will be provided with100g iron-based catalyst (SiO as carrier)2) After the synthesized multi-walled carbon nanotube is loaded into a vibrating screen 4 through a feed inlet 7, the feed inlet 7 is closed, an exhaust gas port 6 is opened, a first air inlet 8 is opened to introduce nitrogen to replace the air in a purifying chamber of a filter 1, when the oxygen content is lower than 1%, the exhaust gas port 6 and a nitrogen gas port 10 are closed, the temperature is raised to 1100 ℃, the vibrating screen 4 feeds the purified chamber of the filter 1, and an air source valve 9 of a gas-phase damping ring 5 is opened, wherein the number of the gas-phase damping ring 5 is 12, the gas-phase damping ring 5 generates gas-phase damping, and the falling speed of the damping carbon nanotube in the purifying chamber is reduced; and the first gas inlet 8 is opened to introduce chlorine gas with the concentration of 1.5m3/h, and the reaction lasts for 0.5 h. Stopping introducing chlorine after the reaction is finished, opening the waste gas port 6 and the nitrogen port 10, introducing nitrogen, keeping the temperature constant at 1100 ℃ for 10 minutes, stopping heating, continuing introducing nitrogen, and closing the waste gas port 6 and the nitrogen port 10 when the temperature is lower than 40 ℃; and opening the discharge valve 11, taking out the carbon nano tubes, putting the carbon nano tubes into a sample bag, sealing the sample bag, discharging tail gas in the whole process through the gas outlet 13, and then absorbing the tail gas by using a sodium hydroxide aqueous solution. After the chlorine gas is used for purifying the carbon nano tube catalyst metal, the shapes are completely consistent, which shows that the carbon nano tube is purified by the chlorine gas without any damage and influence on the carbon nano tube.
An operation mode for preparing carbon nano tubes by catalytic cracking of hydrocarbons by a gas phase damping method is characterized in that 70 g of 6% iron-based catalyst (the carrier is SiO2, and iron oxide is ferric oxide) is taken, and the catalyst is loaded into a vibrating screen 4 through a feed inlet 7; closing the feed inlet 7, opening the nitrogen port 10 and the waste gas port 6, introducing oxygen in a nitrogen displacement device, closing the nitrogen port 10, the feed inlet 7 and the waste gas port 6 after the oxygen content of the system is less than 2%, heating the heating furnace 3 to 660 ℃, starting the vibrating screen 4, controlling the catalyst feeding amount according to the amount of 1g/min, then opening the first air inlet 8, introducing propylene, controlling the propylene flow to be 1.7m3/h, opening the air source valve 9 of the gas phase damping ring 5, wherein the gas phase damping ring 5 is 20 rings, opening the waste gas port 6 to regulate the air pressure, ensuring that the pressure difference in the system is about +250Pa, and the reaction time is about 1 hour; the carbon-hydrogen bond of the propylene gas is cracked into carbon atoms and hydrogen in a small part at 660 ℃ in the initial stage, the hydrogen reduces iron oxide in the catalyst into elemental metal iron, the elemental metal iron is used as a crystal nucleus to catalyze and crack the carbon-hydrogen bond of more hydrocarbons, the carbon atoms are deposited by taking the iron as the crystal nucleus to generate a carbon nano tube, and part of the hydrogen generated by cracking generates water after reducing the iron oxide into the elemental iron and is discharged as waste gas; another part of the hydrogen is discharged through the off-gas port 6. The carbon-hydrogen bond in the cracking chamber is cracked into carbon and hydrogen, carbon atoms are continuously and uniformly loaded on the surface of the iron-based catalyst to grow into the carbon nano tube, meanwhile, part of generated hydrogen is used as carrier gas in a furnace tube of the rotary furnace, and part of generated hydrogen escapes from the reaction furnace and is collected by a gas collecting system.
And after the reaction is finished, stopping heating the heating furnace 3, closing the first air inlet 8, opening the nitrogen port 10, introducing waste gas in a nitrogen displacement system, cooling, after the nitrogen displacement is carried out for 30 minutes, closing the nitrogen port 10, opening the discharge valve 11, allowing the material to enter the cooling chamber 2, cooling to room temperature, and taking out the material to obtain the hollow fibrous carbon nanotube with good appearance, relatively uniform diameter and mainly distributed diameter of 10-15 nm.
The foregoing is illustrative of the preferred embodiments of the present invention, and it is to be understood that the invention is not limited to the precise forms disclosed herein, and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the invention as defined by the appended claims. But that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention, which is to be limited only by the claims appended hereto.

Claims (10)

1. A gas phase damping method carbon nanotube generator, comprising:
a filter (1) and a cooling chamber (2) located below the filter (1) and in communication therewith;
a heating furnace (3) which is arranged outside the filter (1) and used for heating the filter (1);
the device is characterized in that a waste gas port (6) and a feed inlet (7) are formed in the upper part of the filter (1), a first air inlet (8), an air source valve (9) and a discharge port (14) are formed in the lower part of the filter (1), and a vibrating screen (4) and one or more circles of gas phase damping rings (5) are sequentially arranged among the feed inlet (7), the first air inlet (8) and the air source valve (9);
the discharge port (14) is communicated with the cooling chamber (2), a nitrogen port (10) is arranged between the discharge port (14) and the cooling chamber (2), and a discharge valve (11) is arranged between the nitrogen port and the cooling chamber (2).
2. The vapor-damped carbon nanotube generator according to claim 1, wherein said heating furnace (3) is a vertical heating furnace and is disposed in a surrounding manner on a side wall of said filter (1).
3. The vapor-damped carbon nanotube generator according to claim 1, wherein the exhaust gas port (6) is provided at a tip end of the filter (1).
4. The gas-phase damping carbon nanotube generator according to claim 1, wherein the vibrating screen (4) is a pneumatic ultrasonic vibrating screen.
5. The gas-phase damping carbon nanotube generator according to claim 1, wherein the discharge port (14) is located at the bottom end of the filter (1), the feed port (7) is disposed at the lower side wall of the filter (1), and the first gas inlet (8) and the gas source valve (9) are disposed at the upper side wall of the filter (1).
6. The vapor-damped carbon nanotube generator according to claim 5, wherein the first gas inlet (8) and the gas source valve (9) are symmetrically disposed.
7. The gas-phase damping carbon nanotube generator according to claim 1, wherein the cooling chamber (2) is provided with a gas outlet (13), the gas outlet (13) being provided with a control valve (12).
8. The vapor-damped carbon nanotube generator according to claim 7, wherein the discharge port (14) is connected to the cooling chamber (2) via a pipe, the nitrogen port (10) is provided on a side wall of the pipe, and the discharge valve (11) is provided on the pipe between the nitrogen port (10) and the cooling chamber (2).
9. The gas-phase damping carbon nanotube generator according to claim 1, wherein when the gas-phase damping rings (5) are formed in a plurality of rings, the distance between adjacent gas-phase damping rings (5) is gradually increased from the feed opening (7) to the discharge opening (14).
10. The vapor-damped carbon nanotube generator according to claim 1, wherein both ends of said filter (1) are tapered.
CN202020309388.4U 2020-03-13 2020-03-13 Gas phase damping method carbon nano tube generator Active CN212954323U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202020309388.4U CN212954323U (en) 2020-03-13 2020-03-13 Gas phase damping method carbon nano tube generator

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202020309388.4U CN212954323U (en) 2020-03-13 2020-03-13 Gas phase damping method carbon nano tube generator

Publications (1)

Publication Number Publication Date
CN212954323U true CN212954323U (en) 2021-04-13

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Application Number Title Priority Date Filing Date
CN202020309388.4U Active CN212954323U (en) 2020-03-13 2020-03-13 Gas phase damping method carbon nano tube generator

Country Status (1)

Country Link
CN (1) CN212954323U (en)

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Effective date of registration: 20210816

Address after: 610000 plant 1, No. 388, section 3, Chenglong Avenue, Chengdu Economic and Technological Development Zone (Longquanyi District), Sichuan Province

Patentee after: Chengdu Kehui Electromechanical Technology Co.,Ltd.

Address before: 017000 Room 102, Zhongke synthetic oil apartment building, Dalu Industrial Park, Zhungeer banner, Ordos City, Inner Mongolia Autonomous Region

Patentee before: Inner Mongolia Juncheng New Energy Technology Co.,Ltd.

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