CN114314565A - Carbon nanotube purification device - Google Patents
Carbon nanotube purification device Download PDFInfo
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- CN114314565A CN114314565A CN202111549132.6A CN202111549132A CN114314565A CN 114314565 A CN114314565 A CN 114314565A CN 202111549132 A CN202111549132 A CN 202111549132A CN 114314565 A CN114314565 A CN 114314565A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 238000000746 purification Methods 0.000 title claims abstract description 141
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 133
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 133
- 238000010521 absorption reaction Methods 0.000 claims abstract description 170
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000460 chlorine Substances 0.000 claims abstract description 53
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 53
- 238000003860 storage Methods 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 239000007789 gas Substances 0.000 claims description 123
- 239000012159 carrier gas Substances 0.000 claims description 33
- 239000011261 inert gas Substances 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 13
- 239000000919 ceramic Substances 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 5
- 239000012494 Quartz wool Substances 0.000 claims description 4
- 229910001510 metal chloride Inorganic materials 0.000 abstract description 20
- 238000007599 discharging Methods 0.000 abstract description 16
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- CODVACFVSVNQPY-UHFFFAOYSA-N [Co].[C] Chemical compound [Co].[C] CODVACFVSVNQPY-UHFFFAOYSA-N 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The carbon nanotube purification device provided by the embodiment of the invention comprises a high-temperature purification furnace, an impurity absorption furnace and an exhaust assembly, wherein the high-temperature purification furnace comprises a carbon nanotube feeding bin, a purification furnace body, a first heating element and a carbon nanotube storage tank; the impurity absorption furnace comprises an absorption medium feeding bin, an absorption furnace body, a second heating element and an absorption medium storage tank; the exhaust assembly comprises an exhaust pipeline and a third heating element, and two ends of the exhaust pipeline are respectively connected to the purification furnace body and the absorption furnace body and used for discharging gas in the purification furnace body into the absorption furnace body. The metal catalyst impurities in the carbon nano tubes and the chlorine-containing gas react in the high-temperature purification furnace body to generate metal chloride steam, the metal chloride steam enters the absorption furnace body through the exhaust pipeline and is adsorbed and deposited on the absorption medium in the absorption furnace body, so that the metal chloride in the tail gas is effectively removed, and the pollution is reduced.
Description
Technical Field
The invention relates to the technical field of nano material production, in particular to a carbon nano tube purification device.
Background
The carbon nanotubes prepared by the chemical vapor deposition method usually contain metal catalyst impurities, and when the carbon nanotubes are applied to lithium ion batteries, the existence of the metal catalyst impurities may pierce through a diaphragm, so that the batteries are short-circuited, and safety problems are caused. Therefore, the metal catalyst impurities in the carbon nanotubes need to be removed, and the purity of the carbon nanotubes needs to be improved. In the related art, the metal catalyst impurities can be removed by adopting a chlorination purification method, and the metal catalyst impurities in the carbon nanotubes react with chlorine-containing gas at a high temperature to generate metal chlorides and are evaporated for removal, but the treatment of the purified tail gas is not reasonable enough, and more metal chlorides can still remain to cause pollution.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a carbon nano tube purification device which can effectively remove metal chloride in tail gas and reduce pollution.
The carbon nanotube purification device provided by the embodiment of the invention comprises a high-temperature purification furnace, an impurity absorption furnace and an exhaust assembly, wherein the high-temperature purification furnace comprises a carbon nanotube feeding bin, a purification furnace body, a first heating element and a carbon nanotube storage tank, one end of the purification furnace body is communicated with the carbon nanotube feeding bin, the other end of the purification furnace body is communicated with the carbon nanotube storage tank, the purification furnace body is provided with a chlorine-containing gas inlet and a carrier gas inlet, the chlorine-containing gas inlet is used for introducing chlorine-containing gas, the carrier gas inlet is used for introducing inert gas, and the first heating element is connected with the purification furnace body; the impurity absorption furnace comprises an absorption medium feeding bin, an absorption furnace body, a second heating element and an absorption medium storage tank, wherein one end of the absorption furnace body is communicated with the absorption medium feeding bin, the other end of the absorption furnace body is communicated with the absorption medium storage tank, the absorption furnace body is provided with a tail gas discharge port, and the second heating element is connected to the absorption furnace body; the exhaust assembly comprises an exhaust pipeline and a third heating element, the third heating element is connected to the exhaust pipeline, two ends of the exhaust pipeline are respectively connected to the purification furnace body and the absorption furnace body, and the exhaust pipeline is used for supplying gas inside the purification furnace body to be discharged inside the absorption furnace body.
The carbon nanotube purification device provided by the embodiment of the invention at least has the following beneficial effects: the metal catalyst impurities in the carbon nano tubes and the chlorine-containing gas react in the high-temperature purification furnace body to generate metal chloride steam, the metal chloride steam enters the absorption furnace body through the exhaust pipeline and is adsorbed and deposited on the absorption medium in the absorption furnace body, so that the metal chloride in the tail gas is effectively removed, and the pollution is reduced.
In some embodiments of the present invention, the chlorine-containing gas inlet and the carrier gas inlet are disposed on the same side of the purification furnace, and the exhaust conduit is connected to the other side of the purification furnace.
In some embodiments of the present invention, two chlorine-containing gas inlets and two carrier gas inlets are respectively disposed at two ends of the purification furnace body, the exhaust duct is connected between the two ends of the purification furnace body, and the chlorine-containing gas inlets are closer to the exhaust duct than the carrier gas inlets.
In some embodiments of the invention, the vent assembly further comprises a filter element housed inside the vent conduit, the filter element being in circumferential contact with an inner wall of the vent conduit.
In some embodiments of the invention, the material of the filter element is one of a porous ceramic core, a quartz porous plate, a quartz sand core, a porous graphite core, a porous ceramic filled with quartz wool, or a quartz hollow column.
In some embodiments of the present invention, the absorption furnace body has a shielding gas inlet, the shielding gas inlet and the tail gas discharge port are respectively disposed at two ends of the absorption furnace body, and the shielding gas inlet is used for introducing an inert gas.
In some embodiments of the present invention, the high temperature purification furnace further comprises a carbon nanotube feed valve and a carbon nanotube discharge valve, the carbon nanotube feed valve is installed at one end of the purification furnace body connected to the carbon nanotube feed bin, and the carbon nanotube discharge valve is installed at one end of the purification furnace body connected to the carbon nanotube storage tank.
In some embodiments of the present invention, the impurity absorption furnace further comprises an absorption medium feeding valve and an absorption medium discharging valve, the absorption medium feeding valve is installed at one end of the absorption furnace body connected with the absorption medium feeding bin, and the absorption medium discharging valve is installed at one end of the absorption furnace body connected with the absorption medium storage tank.
In some embodiments of the present invention, the system further comprises a plurality of oxygen detectors, and the plurality of oxygen detectors are respectively disposed at the carbon nanotube feeding bin, the carbon nanotube storage tank, and the tail gas discharge port.
In some embodiments of the present invention, the exhaust gas purification device further comprises a spray assembly and an adsorption assembly, and the exhaust gas discharge port, the spray assembly and the adsorption assembly are sequentially communicated.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The invention is further described with reference to the following figures and examples, in which:
fig. 1 is a schematic view of a carbon nanotube purification apparatus according to some embodiments of the present invention;
fig. 2 is a schematic view illustrating gas flow of the carbon nanotube purification apparatus shown in fig. 1.
Reference numerals:
the high-temperature purification furnace 100, the carbon nanotube feeding bin 110, the purification furnace body 120, the chlorine-containing gas inlet 121, the carrier gas inlet 122, the first heating element 130, the carbon nanotube storage tank 140, the carbon nanotube feeding valve 150, the carbon nanotube discharging valve 160, the impurity absorption furnace 200, the absorption medium feeding bin 210, the absorption furnace body 220, the tail gas discharge port 221, the shielding gas inlet 222, the second heating element 230, the absorption medium storage tank 240, the absorption medium feeding valve 250, the absorption medium discharging valve 260, the exhaust assembly 300, the exhaust pipeline 310, the third heating element 320, the filter element 330, the oxygen detector 400, the spray assembly 500, and the adsorption assembly 600.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it should be understood that the orientation or positional relationship referred to in the description of the orientation, such as the upper, lower, left, right, etc., is based on the orientation or positional relationship shown in the drawings, and is only for convenience of description and simplicity of description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, unless otherwise explicitly limited, terms such as arrangement, installation, connection and the like should be understood in a broad sense, and those skilled in the art can reasonably determine the specific meanings of the above terms in the present invention in combination with the specific contents of the technical solutions.
In the description of the present invention, reference to the description of "one embodiment," "some embodiments," or the like, means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The carbon nanotube purification device provided by the embodiment of the invention comprises a high-temperature purification furnace 100, an impurity absorption furnace 200 and an exhaust assembly 300, wherein the high-temperature purification furnace 100 comprises a carbon nanotube feeding bin 110, a purification furnace body 120, a first heating element 130 and a carbon nanotube storage tank 140, one end of the purification furnace body 120 is communicated with the carbon nanotube feeding bin 110, the other end of the purification furnace body 120 is communicated with the carbon nanotube storage tank 140, the purification furnace body 120 is provided with a chlorine-containing gas inlet 121 and a carrier gas inlet 122, the chlorine-containing gas inlet 121 is used for introducing chlorine-containing gas, the carrier gas inlet 122 is used for introducing inert gas, and the first heating element 130 is connected to the purification furnace body 120; the impurity absorption furnace 200 comprises an absorption medium feeding bin 210, an absorption furnace body 220, a second heating member 230 and an absorption medium storage tank 240, wherein one end of the absorption furnace body 220 is communicated with the absorption medium feeding bin 210, the other end of the absorption furnace body 220 is communicated with the absorption medium storage tank 240, the absorption furnace body 220 is provided with a tail gas discharge port 221, and the second heating member 230 is connected with the absorption furnace body 220; the exhaust assembly 300 includes an exhaust pipe 310 and a third heating element 320, the third heating element 320 is connected to the exhaust pipe 310, two ends of the exhaust pipe 310 are respectively connected to the purification furnace body 120 and the absorption furnace body 220, and the exhaust pipe 310 is used for discharging the gas inside the purification furnace body 120 into the absorption furnace body 220.
For example, as shown in fig. 1, the carbon nanotube purification apparatus includes a high temperature purification furnace 100, an impurity absorption furnace 200 and an exhaust assembly 300, wherein the high temperature purification furnace 100 includes a carbon nanotube feeding bin 110, a purification furnace body 120, a first heating element 130 and a carbon nanotube storage tank 140, one end of the purification furnace body 120 is connected to the carbon nanotube feeding bin 110, the other end of the purification furnace body 120 is connected to the carbon nanotube storage tank 140, the purification furnace body 120 has a chlorine-containing gas inlet 121 and a carrier gas inlet 122, the chlorine-containing gas inlet 121 is used for introducing chlorine-containing gas, the carrier gas inlet 122 is used for introducing inert gas, and the first heating element 130 is connected to the purification furnace body 120; the impurity absorption furnace 200 comprises an absorption medium feeding bin 210, an absorption furnace body 220, a second heating member 230 and an absorption medium storage tank 240, wherein one end of the absorption furnace body 220 is communicated with the absorption medium feeding bin 210, the other end of the absorption furnace body 220 is communicated with the absorption medium storage tank 240, the absorption furnace body 220 is provided with a tail gas discharge port 221, and the second heating member 230 is connected with the absorption furnace body 220; the exhaust assembly 300 includes an exhaust pipe 310 and a third heating element 320, the third heating element 320 is connected to the exhaust pipe 310, two ends of the exhaust pipe 310 are respectively connected to the purification furnace body 120 and the absorption furnace body 220, and the exhaust pipe 310 is used for discharging the gas inside the purification furnace body 120 into the absorption furnace body 220.
Referring to fig. 2, in the high temperature purification furnace 100, the carbon nanotubes fall into the purification furnace body 120 from the carbon nanotube feeding bin 110, the chlorine-containing gas enters the purification furnace body 120 from the chlorine-containing gas inlet 121, the inert gas enters the high temperature purification furnace body 120 from the carrier gas inlet 122, the inert gas drives the chlorine-containing gas to mix with the carbon nanotubes and react with the carbon nanotubes, the purified carbon nanotubes fall into the carbon nanotube storage tank 140, the generated metal chloride vapor enters the absorption furnace body 220 through the exhaust pipe 310 under the driving of the inert gas, the absorption medium falls into the absorption furnace body 220 from the absorption medium feeding bin 210, the metal chloride can be adsorbed and deposited on the absorption medium, and the metal chloride in the tail gas can be effectively removed, thereby reducing pollution.
It is understood that the chlorine-containing gas may be one or more of chlorine, hydrogen chloride, chloroform, carbon tetrachloride, the inert gas may be one or more of nitrogen, argon, helium, and the absorption medium may be one of porous activated carbon, graphene nanoplatelets, acid-washed adsorbent, graphite powder, microwave/high temperature expanded graphite powder.
The purification furnace body 120 and the absorption furnace body 220 can be made of one of quartz, alumina, graphite and silicon carbide or made of high-temperature-resistant metal composite materials, the wallpaper of the length and the diameter of the purification furnace body 120 and the absorption furnace body 220 can be set to be 1: 7-1: 2, and the cross section of the inner cavity of the purification furnace body 120 and the absorption furnace body 220 can be circular or square. The temperature in the purification furnace body 120 is preferably 700 ℃ to 1100 ℃, the temperature in the absorption furnace body 220 is preferably 300 ℃ to 800 ℃, and the heat preservation time is preferably 30 minutes to 90 minutes. To ensure that the metal chloride enters the absorption furnace 220 in gaseous form, the temperature of the exhaust line 310 should be close to or the same as the temperature inside the purification furnace 120. To ensure the purification effect, the chlorine content of the chlorine-containing gas is preferably 3 to 10 times the ash mass of the carbon nanotubes.
The first heating member 130, the second heating member 230 and the third heating member 320 may be heated by one or more of resistance wire heating, intermediate frequency heating, silicon carbide rod, and silicon molybdenum rod. In order to ensure the adsorption effect of the metal chloride, the temperature of the absorption furnace body 220 should be lower than that of the purification furnace body 120.
The chlorine-containing gas inlet 121 and the carrier gas inlet 122 are disposed on the same side of the purification furnace 120, and the exhaust line 310 is connected to the other side of the purification furnace 120.
For example, as shown in fig. 1 and 2, the chlorine-containing gas inlet 121 and the carrier gas inlet 122 are disposed on the same side of the purification furnace 120 to facilitate the inert gas to transport the chlorine-containing gas, and the exhaust pipe 310 is connected to the other side of the purification furnace 120 to facilitate the chlorine-containing gas to be fully mixed with the carbon nanotubes for reaction and then to be exhausted from the exhaust pipe 310.
Two chlorine-containing gas inlets 121 and two carrier gas inlets 122 are provided, the two chlorine-containing gas inlets 121 are provided at both ends of the purification furnace 120, the two carrier gas inlets 122 are provided at both ends of the purification furnace 120, the exhaust duct 310 is connected between both ends of the purification furnace 120, and the chlorine-containing gas inlets 121 are closer to the exhaust duct 310 than the carrier gas inlets 122.
For example, as shown in FIG. 1, two chlorine-containing gas inlets 121 and two carrier gas inlets 122 are provided, two chlorine-containing gas inlets 121 are provided at both ends of the purification furnace 120, two carrier gas inlets 122 are provided at both ends of the purification furnace 120, the exhaust pipe 310 is connected between both ends of the purification furnace 120, and the chlorine-containing gas inlets 121 are located closer to the exhaust pipe 310 than the carrier gas inlets 122. Referring to fig. 2, chlorine-containing gas enters the interior of the purification furnace 120 through the two upper and lower chlorine-containing gas inlets 121, inert gas enters the interior of the purification furnace 120 through the two upper and lower carrier gas inlets 122, the inert gas drives the chlorine-containing gas to flow in the direction of the arrow, and the chlorine-containing gas is mixed with the carbon nanotubes and reacts with the carbon nanotubes, and then flows to the exhaust pipe 310 connected between the two ends of the purification furnace 120.
It should be noted that the exhaust assembly 300 further includes a filter element 330, the filter element 330 is accommodated inside the exhaust duct 310, and the filter element 330 is circumferentially contacted with the inner wall of the exhaust duct 310.
For example, as shown in fig. 1, the vent assembly 300 further includes a filter element 330, the filter element 330 being received inside the vent conduit 310, the filter element 330 being in circumferential contact with an inner wall of the vent conduit 310. Referring to fig. 2, the tail gas containing the metal chloride vapor flows to the absorption furnace body 220 through the exhaust pipe 310, and the filter element 330 can filter the tail gas to prevent the carbon nanotubes in the purification furnace body 120 and the absorption medium in the absorption furnace body 220 from being contaminated with each other.
The material of the filter element 330 is one of a porous ceramic core, a quartz porous plate, a quartz sand core, a porous graphite core, a porous ceramic containing quartz wool, or a quartz hollow column.
The filter element 330 is made of porous non-metallic materials such as a porous ceramic core, a quartz porous plate, a quartz sand core, a porous graphite core, porous ceramic filled with quartz wool or a quartz hollow column, and the like, so that the filter element has a good filtering effect and a long service life.
It is understood that the external size of the filter element 330 can be determined according to the internal size of the exhaust duct 310, the size of the gap of the filter element 330 can be determined according to actual requirements, and preferably, the size of the gap of the filter element 330 can be set to be 20-200 meshes.
It should be noted that the absorption furnace body 220 has a shielding gas inlet 222, the shielding gas inlet 222 and the tail gas discharge port 221 are respectively disposed at two ends of the absorption furnace body 220, and the shielding gas inlet 222 is used for introducing an inert gas.
For example, as shown in fig. 1, the absorption furnace body 220 has a shielding gas inlet 222, the shielding gas inlet 222 and the tail gas discharge port 221 are respectively disposed at two ends of the absorption furnace body 220, and the shielding gas inlet 222 is used for introducing inert gas. Referring to fig. 2, the inert gas enters the interior of the absorption furnace body 220 from the shielding gas inlet 222, and drives the tail gas entering the absorption furnace body 220 to flow to the tail gas discharge port 221 after being adsorbed by the absorption medium, and the flow path of the tail gas is reasonable, so that the tail gas adsorbed by the absorption medium can be conveniently discharged.
It should be noted that the high temperature purification furnace 100 further includes a carbon nanotube feeding valve 150 and a carbon nanotube discharging valve 160, the carbon nanotube feeding valve 150 is installed at one end of the purification furnace body 120 connected to the carbon nanotube feeding bin 110, and the carbon nanotube discharging valve 160 is installed at one end of the purification furnace body 120 connected to the carbon nanotube storage tank 140.
For example, as shown in fig. 1, the high temperature purification furnace 100 further includes a carbon nanotube feeding valve 150 and a carbon nanotube discharging valve 160, the carbon nanotube feeding valve 150 is installed at one end of the purification furnace body 120 connected to the carbon nanotube feeding bin 110 and is capable of controlling the feeding speed of the carbon nanotubes, and the carbon nanotube discharging valve 160 is installed at one end of the purification furnace body 120 connected to the carbon nanotube storage tank 140 and is capable of controlling the discharging speed of the carbon nanotubes, so that the reaction process in the purification furnace body 120 is more controllable.
It is understood that the carbon nanotube feed valve 150 and the carbon nanotube discharge valve 160 may be pneumatic valves, rotary valves, etc., or a combination of valves.
It should be noted that the impurity absorption furnace 200 further includes an absorption medium feed valve 250 and an absorption medium discharge valve 260, the absorption medium feed valve 250 is installed at one end of the absorption furnace body 220 connected to the absorption medium feed bin 210, and the absorption medium discharge valve 260 is installed at one end of the absorption furnace body 220 connected to the absorption medium storage tank 240.
For example, as shown in fig. 1, the impurity absorption furnace 200 further includes an absorption medium feeding valve 250 and an absorption medium discharging valve 260, the absorption medium feeding valve 250 is installed at one end of the absorption furnace body 220 connected to the absorption medium feeding bin 210 and can control the feeding speed of the absorption medium, and the absorption medium discharging valve 260 is installed at one end of the absorption furnace body 220 connected to the absorption medium storage tank 240 and can control the discharging speed of the absorption medium, so that the adsorption process in the absorption furnace body 220 is more controllable.
It is understood that the absorption medium feed valve 250 and the absorption medium discharge valve 260 may be pneumatic valves, rotary valves, etc., or a combination of valves.
It should be noted that the carbon nanotube purifying apparatus further includes a plurality of oxygen detectors 400, and the plurality of oxygen detectors 400 are respectively disposed at the carbon nanotube feeding bin 110, the carbon nanotube storage tank 140, and the tail gas discharge port 221.
For example, as shown in fig. 1, the carbon nanotube purifying apparatus further includes a plurality of oxygen detectors 400, and the plurality of oxygen detectors 400 are respectively disposed at the carbon nanotube feeding bin 110, the carbon nanotube storage tank 140, and the exhaust gas discharge port 221. Before the production starts, inert gas is introduced into the purification furnace 120 and the absorption furnace 220 to displace oxygen in the purification furnace 120 and the absorption furnace 220, thereby preventing corrosion caused by reaction between oxygen and the purification furnace 120 or the absorption furnace 220 in a high temperature environment. The oxygen detector 400 can measure the oxygen content at the location, the oxygen detectors 400 are respectively disposed at the carbon nanotube feeding bin 110, the carbon nanotube storage tank 140 and the tail gas discharge port 221, the inert gas is introduced through the carrier gas inlet 122 of the purification furnace 120, and the interiors of the purification furnace 120 and the absorption furnace 220, the carbon nanotube feeding bin 110 and the carbon nanotube storage tank 140 are gradually filled until the oxygen content values detected by the oxygen detectors 400 in the carbon nanotube feeding bin 110, the carbon nanotube storage tank 140 and the tail gas discharge port 221 are lower than a preset value, and the replacement is completed.
It should be noted that the carbon nanotube purification apparatus further includes a spray assembly 500 and an adsorption assembly 600, and the tail gas discharge port 221, the spray assembly 500 and the adsorption assembly 600 are sequentially communicated.
For example, as shown in fig. 1, the carbon nanotube purifying apparatus further includes a spray module 500 and an adsorption module 600, and the tail gas discharge port 221, the spray module 500 and the adsorption module 600 are sequentially communicated. In addition to the metal chloride vapor, a small amount of unreacted chlorine-containing gas may remain in the tail gas, and the spraying of the spraying assembly 500 and the adsorption of the adsorption assembly 600 remove a small amount of chlorine-containing gas in the tail gas, thereby further reducing the pollution of the tail gas.
The concept and technical effects of the present invention will be further clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention.
Example 1
The carbon nanotube purification device comprises a high-temperature purification furnace 100, an impurity absorption furnace 200 and an exhaust assembly 300, wherein the diameter of a purification furnace body 120 in the high-temperature purification furnace 100 is 30cm, and the length is 150 cm; the diameter of the absorption furnace body 220 in the impurity absorption furnace 200 is 20cm, and the length is 100 cm; the diameter of the exhaust duct 310 in the exhaust assembly 300 is 10cm, the length is 30cm, and the filter element 330 is a quartz sand core with a pore size of 30 meshes and the length is 10 cm.
Filling cobalt carbon nanotubes to be purified from the carbon nanotube feeding bin 110 to two thirds of the purification furnace body 120 through the carbon nanotube feeding valve 150, filling the absorption furnace body 220 with graphene micro powder from the absorption medium feeding bin 210 through the absorption medium feeding valve 250, opening the carrier gas inlet 122 on the purification furnace body 120 and the protective gas inlet 222 on the absorption furnace body 220, and introducing argon gas to perform gas replacement in the purification furnace body 120 and the absorption furnace body 220, wherein the flow rate of the replacement gas is 1000 sccm.
When the oxygen content is detected to be less than 0.01% by the oxygen detector 400, heating the purifying furnace body 120 to 950 ℃, preserving the heat, and introducing hydrogen chloride gas from the upper and lower chlorine-containing gas inlets 121 of the purifying furnace body 120 at the flow rate of 1000 sccm; argon gas is introduced from the upper and lower carrier gas inlets 122 of the purification furnace body 120, the flow rate is 1000sccm, after 60 minutes, the carbon nanotube discharging valve 160 is opened, and the purified carbon nanotubes fall into the carbon nanotube storage tank 140; the exhaust pipeline 310 is heated to 900 ℃ and then is insulated to ensure that the metal chloride enters the absorption furnace body 220 in a gas form, the absorption furnace body 220 is heated to 500 ℃ and then is insulated, and the metal chloride is adsorbed and deposited on the surface of the graphene micro powder in the absorption furnace body 220; argon gas is introduced from the shielding gas inlet 222 of the absorption furnace body 220 at a flow rate of 2000sccm, and the spraying assembly 500 is opened to treat the tail gas.
The ash content and the metal impurity content of the purified carbon nanotubes are shown in table 1.
Example 2
The same carbon nanotube purification apparatus and process as in example 1 were used, and the carbon nanotubes to be purified were iron-based carbon nanotubes, chlorine-containing gas was hydrogen chloride, and inert gas was argon.
The temperature of the purifying furnace body 120 is 650 ℃, the flow of hydrogen chloride gas introduced into the upper and lower chlorine-containing gas inlets 121 of the purifying furnace body 120 is 1000sccm, and the flow of argon gas introduced into the upper and lower carrier gas inlets 122 of the purifying furnace body 120 is 1500 sccm; the temperature of the absorption furnace body 220 was 300 ℃, and the flow rate of argon gas introduced into the shielding gas inlet 222 of the absorption furnace body 220 was 2000 sccm.
The ash content and the metal impurity content of the purified carbon nanotubes are shown in table 1.
Example 3
The carbon nanotube purification device comprises a high-temperature purification furnace 100, an impurity absorption furnace 200 and an exhaust assembly 300, wherein the diameter of a purification furnace body 120 in the high-temperature purification furnace 100 is 20cm, and the length is 100 cm; the diameter of the absorption furnace body 220 in the impurity absorption furnace 200 is 15cm, and the length is 80 cm; the exhaust duct 310 in the exhaust assembly 300 has a diameter of 8cm and a length of 30cm, and the filter element 330 is a porous ceramic column having a pore size of 30 mesh and a length of 10 cm.
Filling cobalt carbon nanotubes to be purified from the carbon nanotube feeding bin 110 to two thirds of the purification furnace body 120 through the carbon nanotube feeding valve 150, filling the absorption furnace body 220 with microwave expanded graphite powder from the absorption medium feeding bin 210 through the absorption medium feeding valve 250, opening the carrier gas inlet 122 on the purification furnace body 120 and the protective gas inlet 222 on the absorption furnace body 220, and introducing argon gas to perform gas replacement in the purification furnace body 120 and the absorption furnace body 220, wherein the flow rate of the replacement gas is 1000 sccm.
When the oxygen content is detected to be less than 0.01% by the oxygen detector 400, heating the purifying furnace body 120 to 1000 ℃, preserving the heat, and introducing chlorine gas from the upper and lower chlorine-containing gas inlets 121 of the purifying furnace body 120 at a flow rate of 1000 sccm; introducing nitrogen gas from the upper and lower carrier gas inlets 122 of the purification furnace body 120, wherein the flow rate is 1000sccm, opening the carbon nanotube discharge valve 160 after 40 minutes, and allowing the purified carbon nanotubes to fall into the carbon nanotube storage tank 140; the exhaust pipeline 310 is heated to 800 ℃ and then is insulated to ensure that the metal chloride enters the absorption furnace body 220 in a gas form, the absorption furnace body 220 is heated to 450 ℃ and then is insulated, and the metal chloride is adsorbed and deposited on the surface of the microwave expansion graphite powder in the absorption furnace body 220; nitrogen gas is introduced from the shielding gas inlet 222 of the absorption furnace body 220 at a flow rate of 2000sccm, and the spraying assembly 500 is opened to treat the tail gas.
The ash content and the metal impurity content of the purified carbon nanotubes are shown in table 1.
Example 4
The same carbon nanotube purification apparatus and process flow as in example 3 were used, and the carbon nanotubes to be purified were iron-based carbon nanotubes, chlorine-containing gas was chlorine gas, and inert gas was nitrogen gas.
The temperature of the purification furnace body 120 is 650 ℃, the chlorine flow introduced into the upper and lower chlorine-containing gas inlets 121 of the purification furnace body 120 is 1000sccm, and the nitrogen flow introduced into the upper and lower carrier gas inlets 122 of the purification furnace body 120 is 1000 sccm; the temperature of the absorption furnace body 220 is 300 ℃, and the flow rate of nitrogen introduced into the protective gas inlet 222 of the absorption furnace body 220 is 2000 sccm.
The ash content and the metal impurity content of the purified carbon nanotubes are shown in table 1.
The metal impurities Fe and Co in the purified carbon nanotube powder in the above examples were characterized by ICP (Inductively coupled plasma spectrometry); the ash test was carried out by calcining in a muffle furnace at a high temperature of 950 ℃ for 2 hours, and the relevant data are shown in Table 1.
Table 1 ash, metal impurity content of carbon nanotubes purified in examples 1 to 4
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A carbon nanotube purification apparatus, comprising:
the high-temperature purification furnace comprises a carbon nano tube feeding bin, a purification furnace body, a first heating element and a carbon nano tube storage tank, wherein one end of the purification furnace body is communicated with the carbon nano tube feeding bin, the other end of the purification furnace body is communicated with the carbon nano tube storage tank, the purification furnace body is provided with a chlorine-containing gas inlet and a carrier gas inlet, the chlorine-containing gas inlet is used for introducing chlorine-containing gas, the carrier gas inlet is used for introducing inert gas, and the first heating element is connected to the purification furnace body;
the impurity absorption furnace comprises an absorption medium feeding bin, an absorption furnace body, a second heating element and an absorption medium storage tank, wherein one end of the absorption furnace body is communicated with the absorption medium feeding bin, the other end of the absorption furnace body is communicated with the absorption medium storage tank, the absorption furnace body is provided with a tail gas discharge port, and the second heating element is connected to the absorption furnace body;
the exhaust assembly comprises an exhaust pipeline and a third heating element, the third heating element is connected to the exhaust pipeline, two ends of the exhaust pipeline are respectively connected to the purification furnace body and the absorption furnace body, and the exhaust pipeline is used for supplying gas inside the purification furnace body to be discharged inside the absorption furnace body.
2. The carbon nanotube purification apparatus according to claim 1, wherein the chlorine-containing gas inlet and the carrier gas inlet are disposed on the same side of the purification furnace, and the exhaust pipe is connected to the other side of the purification furnace.
3. The carbon nanotube purification apparatus according to claim 2, wherein the chlorine-containing gas inlet and the carrier gas inlet are provided in two, the two chlorine-containing gas inlets are provided at two ends of the purification furnace, the two carrier gas inlets are provided at two ends of the purification furnace, the exhaust duct is connected between the two ends of the purification furnace, and the chlorine-containing gas inlet is closer to the exhaust duct than the carrier gas inlets.
4. The carbon nanotube purification apparatus of claim 1, wherein the vent assembly further comprises a filter element housed inside the vent conduit, the filter element circumferentially contacting an inner wall of the vent conduit.
5. The carbon nanotube purification apparatus of claim 4, wherein the material of the filter element is one of a porous ceramic core, a quartz porous plate, a quartz sand core, a porous graphite core, a porous ceramic filled with quartz wool, or a hollow column of quartz.
6. The carbon nanotube purification apparatus according to claim 1, wherein the absorption furnace has a shielding gas inlet, the shielding gas inlet and the tail gas discharge port are respectively disposed at two ends of the absorption furnace, and the shielding gas inlet is used for introducing an inert gas.
7. The carbon nanotube purification apparatus according to any one of claims 1 to 6, wherein the high temperature purification furnace further comprises a carbon nanotube feed valve and a carbon nanotube discharge valve, the carbon nanotube feed valve is installed at one end of the purification furnace body connected to the carbon nanotube feed bin, and the carbon nanotube discharge valve is installed at one end of the purification furnace body connected to the carbon nanotube storage tank.
8. The carbon nanotube purification apparatus according to any one of claims 1 to 6, wherein the impurity absorption furnace further comprises an absorption medium feed valve and an absorption medium discharge valve, the absorption medium feed valve is installed at one end of the absorption furnace body connected to the absorption medium feed bin, and the absorption medium discharge valve is installed at one end of the absorption furnace body connected to the absorption medium storage tank.
9. The carbon nanotube purification apparatus according to any one of claims 1 to 6, further comprising a plurality of oxygen detectors respectively disposed at the carbon nanotube feeding bin, the carbon nanotube storage tank, and the exhaust gas discharge port.
10. The carbon nanotube purification apparatus according to any one of claims 1 to 6, further comprising a spray assembly and an adsorption assembly, wherein the tail gas discharge port, the spray assembly and the adsorption assembly are sequentially communicated.
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