CN112225200A - Method and device for continuously preparing high-purity carbon nano tube - Google Patents

Method and device for continuously preparing high-purity carbon nano tube Download PDF

Info

Publication number
CN112225200A
CN112225200A CN202011102872.0A CN202011102872A CN112225200A CN 112225200 A CN112225200 A CN 112225200A CN 202011102872 A CN202011102872 A CN 202011102872A CN 112225200 A CN112225200 A CN 112225200A
Authority
CN
China
Prior art keywords
reactor
pipe
acid gas
communicated
inert gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011102872.0A
Other languages
Chinese (zh)
Inventor
马伟斌
杨锦
张权
张洋岳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiaozuo Rongchuang Graphite Technology Co ltd
Original Assignee
Jiaozuo Rongchuang Graphite Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiaozuo Rongchuang Graphite Technology Co ltd filed Critical Jiaozuo Rongchuang Graphite Technology Co ltd
Priority to CN202011102872.0A priority Critical patent/CN112225200A/en
Publication of CN112225200A publication Critical patent/CN112225200A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/17—Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/04—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being spirally coiled
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/30—Purity
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a method and a device for continuously preparing high-purity carbon nanotubes, which comprises a raw material tank, a preheating reactor, a purification reactor and a cooling tank which are sequentially connected from top to bottom; a helical blade is arranged in the preheating reactor; a spiral slideway is arranged in the purification reactor; the purification reactor is communicated with an acid gas inlet pipe A and an inert gas inlet pipe A; the side wall of the upper part of the purification reactor is communicated with a waste gas exhaust pipe; the spiral slideway is fixed on the support column; the support column is a hollow cylinder. The invention has simple structure and convenient operation; the preheating reactor can control the preheating time of the unpurified carbon nano tube, so that the unpurified carbon nano tube is fully preheated; in the purification reactor, unpurified carbon nanotubes fully react with acid gas, so that the purification effect is good; the cooling tank can recycle the waste heat of the purified carbon nano tube, thereby saving resources.

Description

Method and device for continuously preparing high-purity carbon nano tube
Technical Field
The invention belongs to the technical field of carbon nanotube production, and particularly relates to a method and a device for continuously preparing high-purity carbon nanotubes.
Background
Carbon nanotubes, also known as buckytubes, are one-dimensional quantum materials with a special structure (radial dimension is nanometer magnitude, axial dimension is micrometer magnitude, both ends of the tube are basically sealed). Carbon nanotubes are coaxial circular tubes consisting of several to tens of layers of carbon atoms arranged in a hexagonal pattern. Since the carbon nano tube was discovered in the last 90 th century, the carbon nano tube has attracted great interest of scientists of various countries due to unique structure, special physicochemical characteristics and potential application prospect, and is one of the research hotspots in the fields of physics, chemistry, materials science and the like.
The existing methods for preparing carbon nanotubes mainly include arc discharge methods, laser etching methods, chemical vapor deposition methods, solid phase pyrolysis methods, flame synthesis methods, glow discharge methods, polymerization synthesis methods, and the like. In many carbon nanotube preparation processes, catalysts are required in other methods except some direct current arc methods which do not require catalysts. The catalyst is selected from transition metals such as iron, cobalt, nickel, manganese and the like and oxides thereof. Along with the growth of the carbon nano tube, the metal active component is coated by the carbon layer to cause the inactivation of the catalyst, so that the metal catalyst is inevitably remained in the obtained crude product of the carbon nano tube, and the existence of the metal impurities can directly influence the performance of the carbon nano tube, thereby greatly restricting the application of the carbon nano tube in various fields. Therefore, in order to obtain high purity carbon nanotubes, the crude carbon nanotubes must be purified.
In the prior art, the purification methods of the carbon nano tube comprise acid cleaning purification, chlorine purification, high-temperature purification and the like, but all have certain defects. The pickling cost is relatively low, but a large amount of sewage is generated in the purification process; the high-temperature purification energy consumption is too large, the productivity is small, the continuous production cannot be realized, and the cost is high; the chlorine purification is difficult to solve the continuous production and the production efficiency is low.
Disclosure of Invention
The invention aims to overcome the technical problems in the prior art and provides a method and a device for continuously preparing high-purity carbon nanotubes.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a device for continuously preparing high-purity carbon nano tubes comprises a raw material tank, a preheating reactor, a purification reactor and a cooling tank which are sequentially connected from top to bottom; the raw material tank, the preheating reactor, the purification reactor and the cooling tank are all connected with air pumps; the preheating reactor and the cooling tank are both communicated with a protective gas inlet pipe; the raw material tank is communicated with the preheating reactor through a connecting pipe A, the preheating reactor is communicated with the purification reactor through a connecting pipe B, and the purification reactor is communicated with the cooling tank through a connecting pipe C;
the left side of the air pump of the raw material tank is connected with an exhaust filter; the upper end of the raw material tank is communicated with a feeding pipe;
the upper part of the connecting pipe A is provided with a blanking valve A, and the lower part of the connecting pipe A is provided with a quantitative blanking device; a protective gas inlet pipe is communicated with the pipe wall of the connecting pipe A above the blanking valve A; a blanking valve B is arranged on the connecting pipe B; a blanking valve C is arranged on the connecting pipe C;
a helical blade is arranged in the preheating reactor;
a spiral slideway is arranged in the purification reactor; the purification reactor is communicated with an acid gas inlet pipe A and an inert gas inlet pipe A; the side wall of the upper part of the purification reactor is communicated with a waste gas exhaust pipe;
the bottom of the cooling tank is connected with a discharge pipe; the discharging pipe is provided with a discharging valve D.
Preferably, the helical blade is fixedly arranged on the rotating shaft; a driving wheel is fixedly arranged at the upper end of the rotating shaft, and a driving motor drives the driving wheel to rotate through a driving belt;
the tail part of the connecting pipe A is a conical blanking end A; the projection of the blanking end A falls on the spiral blade;
the bottom of the preheating reactor is obliquely pointed to the lower right; the connecting pipe B is positioned on the right side of the rotating shaft.
Preferably, the spiral slideway is fixed on the supporting column; the supporting column is a hollow cylinder;
the center of the support column is provided with an acid gas main pipe; a plurality of acid gas branch pipes are communicated with the acid gas main pipe; the acid gas branch pipe penetrates through the side wall of the support column; the top of the acid gas main pipe is closed, and the bottom of the acid gas main pipe is communicated with the acid gas inlet pipe A;
the acid gas branch pipes positioned in the support columns are all provided with one-way valves;
and a cavity between the acid gas main pipe and the support column is filled with a heat insulation material.
Preferably, the tail part of the connecting pipe B is a conical blanking end B; the projection of the blanking end B falls in the spiral slideway; the bottom of the purification reactor is obliquely pointed to the lower right; connecting tube C is located to the right of the bottom of the purification reactor.
Preferably, the cooling tank is internally provided with an acid gas coil and an inert gas coil;
the head of the acid gas coil is communicated with the acid gas inlet pipe A; the head of the inert gas coil is communicated with an inert gas inlet pipe A; the tail part of the acid gas coil pipe penetrates through the side wall of the cooling tank and is communicated with an acid gas inlet pipe B and an inert gas inlet pipe C; the tail part of the inert gas coil is communicated with an inert gas inlet pipe B.
Preferably, the lower end of the connection pipe C is located at the center of the upper end surface of the cooling tank.
Preferably, the acid gas inlet pipe B is externally connected with acid gas; the acid gas is one of chlorine and hydrogen chloride; the inert gas inlet pipe B, the inert gas inlet pipe C and the protective gas inlet pipe are all externally connected with inert gas; the inert gas is one of nitrogen, argon and helium.
A method for continuously preparing high-purity carbon nanotubes comprises the following steps:
s1, closing the blanking valve A, the blanking valve B, the blanking valve C and the blanking valve D, and filling unpurified carbon nano tubes into the raw material tank; then, enabling the quantitative feeder to be in an open state, and performing inert gas replacement on the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank by using a vacuum pump; the oxygen content in the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank after replacement is lower than 0.15 percent;
s2, starting the preheating reactor and the purifying reactor to ensure that the temperature in the preheating reactor is 700-900 ℃ and the temperature in the purifying reactor is 1000-1300 ℃;
s3, opening a blanking valve A, a blanking valve B and a blanking valve C, and starting a quantitative blanking device; sending unpurified carbon nanotubes into the preheating reactor through a quantitative feeder under the action of gravity through a connecting pipe A; preheating is completed in the preheating reactor along with the helical blades of the preheating reactor; the preheated unpurified carbon nano tube enters the purification reactor through a connecting pipe B;
s4, continuously introducing an acid gas and an inert gas into the purification reactor, wherein the volume ratio of the acid gas to the inert gas is 1: 1-5: 1; the mass ratio of the unpurified carbon nano tube to the mixed gas of the acid gas and the inert gas is 1: 10-2: 1;
the unpurified carbon nano tube is purified in the mixed gas of acid gas and inert gas in the process of sliding along the spiral slideway; the purified carbon nano tube falls into a cooling tank along a connecting pipe C;
the waste gas generated in the purification process is discharged through a waste gas exhaust pipe and is treated in a centralized way;
and S5, discharging the carbon nano tubes from the discharge pipe after the carbon nano tubes are cooled by the cooling tank.
The invention has the following action principle:
the present invention uses a raw material tank, a preheating reactor, a purification reactor, and a cooling tank, and in the purification reactor, unpurified carbon nanotubes are purified by acid gas and high temperature.
The helical blades are arranged in the preheating reactor, and the residence time of the unpurified carbon nano tubes in the preheating reactor can be controlled by the rotating direction and the rotating speed of the helical blades, so that the unpurified carbon nano tubes are preheated in the preheating reactor.
The purification reactor is internally provided with a spiral slideway, and the use of the spiral slideway prolongs the residence time of the unpurified carbon nano tubes in the purification reactor, so that the unpurified carbon nano tubes have enough time for purification. The support column is internally provided with an acid gas main pipe, and the acid gas main pipe is communicated with a plurality of acid gas branch pipes. The use of multiple acid gas branch pipes facilitates the sufficient mixing of the acid gas and the inert gas.
The cooling tank is internally provided with an acid gas coil and an inert gas coil, so that the acid gas and the inert gas introduced into the purification reactor can be discharged into the alcoholization reactor after heat exchange in the cooling tank, and the waste heat of the purified carbon nano tube can be recycled. The inert gas inlet pipe C can conveniently discharge the gas in the acid gas coil pipe for inert gas replacement.
The invention achieves the following beneficial effects:
the invention has simple structure and convenient operation; the preheating reactor can control the preheating time of the unpurified carbon nano tube, so that the unpurified carbon nano tube is fully preheated; in the purification reactor, unpurified carbon nanotubes fully react with acid gas, so that the purification effect is good; the cooling tank can recycle the waste heat of the purified carbon nano tube, thereby saving resources.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is an enlarged view of the feed tank, pre-heater reactor of FIG. 1;
FIG. 3 is an enlarged view of the purification reactor and cooling tank of FIG. 1.
In the figure: 1. a raw material tank; 2. pre-heating the reactor; 3. a purification reactor; 4. a cooling tank; 5. an air pump; 6. a shielding gas inlet pipe; 7. a connecting pipe A; 8. a connecting pipe B; 9. a connecting pipe C; 10. an exhaust gas filter; 11. a feed pipe; 12. a discharge valve A; 13. a quantitative feeder; 14. a discharge valve B; 15. a discharge valve C; 16. a helical blade; 17. a rotating shaft; 18. a drive motor; 19. a transmission belt; 20. a blanking end A; 21. a spiral slideway; 22. an acid gas inlet pipe A; 23. an inert gas inlet pipe A; 24. an exhaust gas duct; 25. a support pillar; 26. a sour gas main pipe; 27. a sour gas branch pipe; 28. a one-way valve; 29. a discharging end B; 30. a discharge pipe; 31. a sour gas coil pipe; 32. an inert gas coil; 33. an acid gas inlet pipe B; 34. an inert gas inlet pipe C; 35. an inert gas inlet pipe B; 36. and a discharge valve D.
Detailed Description
The invention will be further described with reference to the drawings and specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
As shown in fig. 1 to 3, an apparatus for continuously preparing high purity carbon nanotubes comprises a raw material tank 1, a pre-heating reactor 2, a purification reactor 3, and a cooling tank 4, which are connected in sequence from top to bottom; the raw material tank 1, the preheating reactor 2, the purification reactor 3 and the cooling tank 4 are all connected with an air pump 5; the preheating reactor 2 and the cooling tank 4 are both communicated with a protective gas inlet pipe 6; the raw material tank 1 is communicated with the preheating reactor 2 through a connection pipe a7, the preheating reactor 2 is communicated with the purification reactor 3 through a connection pipe B8, and the purification reactor 3 is communicated with the cooling tank 4 through a connection pipe C9.
The left side of the air pump of the raw material tank 1 is connected with an exhaust filter 10, and the upper end of the raw material tank 1 is communicated with an inlet pipe 11.
The upper part of the connecting pipe A7 is provided with a blanking valve A12, and the lower part of the connecting pipe A7 is provided with a quantitative blanking device 13; the pipe wall of the connecting pipe A7 above the blanking valve A12 is communicated with a protective gas inlet pipe 6; a blanking valve B14 is arranged on the connecting pipe B8; the connecting pipe C9 is provided with a blanking valve C15.
The preheating reactor 2 is provided with helical blades 16. The helical blade 16 is fixedly arranged on the rotating shaft 17; the upper end of the rotating shaft 17 is fixedly provided with a driving wheel, and a driving motor 18 drives the driving wheel to rotate through a driving belt 19. The tail part of the connecting pipe A7 is a conical blanking end A20; the projection of the discharge end a20 falls on the helical blade 16. The bottom of the preheating reactor 2 is obliquely pointed to the lower right; the connection tube B8 is located on the right side of the rotation shaft 17.
A spiral slideway 21 is arranged in the purification reactor 3; the purification reactor 3 is communicated with an acid gas inlet pipe A22 and an inert gas inlet pipe A23; the side wall of the upper part of the purification reactor 3 is communicated with an exhaust gas calandria 24.
The spiral slideway 21 is fixed on the supporting column 25; the support column 25 is a hollow cylinder; the center of the supporting column 25 is provided with an acid gas main pipe 26; five acid gas branch pipes 27 are communicated with the acid gas main pipe 26; the acid gas branch pipe 27 penetrates through the side wall of the supporting column 25; the top of the acid gas main pipe 26 is closed, and the bottom of the acid gas main pipe 26 is communicated with an acid gas inlet pipe A22; the acid gas branch pipes 27 positioned in the supporting columns 25 are all provided with one-way valves 28; and a cavity between the acid gas main pipe 26 and the support column 25 is filled with a heat insulation material.
The tail part of the connecting pipe B8 is a conical blanking end B29; the projection of the blanking end B29 falls in the spiral slideway 21; the bottom of the purification reactor 3 is obliquely directed to the lower right; connecting pipe C9 is located at the right side of the bottom of purification reactor 3.
The bottom of the cooling tank 4 is connected with a discharge pipe 30. An acid gas coil 31 and an inert gas coil 32 are arranged in the cooling tank 4;
the head of the sour gas coil 31 is communicated with a sour gas inlet pipe A22; the head of the inert gas coil 32 is communicated with an inert gas inlet pipe A23; the tail part of the acid gas coil 31 penetrates through the side wall of the cooling tank 4 and is communicated with an acid gas inlet pipe B33 and an inert gas inlet pipe C34; the rear of the inert gas coil 32 is in communication with an inert gas inlet tube B35.
The lower end of the connecting pipe C9 is positioned at the center of the upper end surface of the cooling tank 4; the discharge pipe 30 is provided with a discharge valve D36.
The acid gas inlet pipe B33 is externally connected with acid gas; the acid gas is one of chlorine and hydrogen chloride; the inert gas inlet pipe B35, the inert gas inlet pipe C34 and the protective gas inlet pipe 6 are externally connected with inert gas; the inert gas is one of nitrogen, argon and helium.
Example 2
A method for continuously preparing high-purity carbon nanotubes comprises the following steps:
s1, closing the blanking valve A, the blanking valve B, the blanking valve C and the blanking valve D, and filling unpurified carbon nano tubes into the raw material tank; then, enabling the quantitative feeder to be in an open state, and performing inert gas replacement on the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank by using a vacuum pump; the oxygen content in the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank after replacement is lower than 0.15 percent;
s2, starting the preheating reactor and the purifying reactor to ensure that the temperature in the preheating reactor is 800 ℃ and the temperature in the purifying reactor is 1250 ℃;
s3, opening a blanking valve A, a blanking valve B and a blanking valve C, and starting a quantitative blanking device; sending unpurified carbon nanotubes into the preheating reactor through a quantitative feeder under the action of gravity through a connecting pipe A; preheating is completed in the preheating reactor along with the helical blades of the preheating reactor; the preheated unpurified carbon nano tube enters the purification reactor through a connecting pipe B;
s4, continuously introducing an acid gas and an inert gas into the purification reactor, wherein the volume ratio of the acid gas to the inert gas is 1: 1; the mass ratio of the unpurified carbon nano tubes to the mixed gas of the acid gas and the inert gas is 1: 1; the acid gas is chlorine, and the inert gas is nitrogen;
the unpurified carbon nano tube is purified in the mixed gas of acid gas and inert gas in the process of sliding along the spiral slideway; the purified carbon nano tube falls into a cooling tank along a connecting pipe C;
the waste gas generated in the purification process is discharged through a waste gas exhaust pipe and is treated in a centralized way;
and S5, discharging the carbon nano tubes from the discharge pipe after the carbon nano tubes are cooled by the cooling tank.
Example 3
A method for continuously preparing high-purity carbon nanotubes comprises the following steps:
s1, closing the blanking valve A, the blanking valve B, the blanking valve C and the blanking valve D, and filling unpurified carbon nano tubes into the raw material tank; then, enabling the quantitative feeder to be in an open state, and performing inert gas replacement on the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank by using a vacuum pump; the oxygen content in the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank after replacement is lower than 0.15 percent;
s2, starting the preheating reactor and the purifying reactor to enable the temperature in the preheating reactor to be 700 ℃ and the temperature in the purifying reactor to be 1000 ℃;
s3, opening a blanking valve A, a blanking valve B and a blanking valve C, and starting a quantitative blanking device; sending unpurified carbon nanotubes into the preheating reactor through a quantitative feeder under the action of gravity through a connecting pipe A; preheating is completed in the preheating reactor along with the helical blades of the preheating reactor; the preheated unpurified carbon nano tube enters the purification reactor through a connecting pipe B;
s4, continuously introducing an acid gas and an inert gas into the purification reactor, wherein the volume ratio of the acid gas to the inert gas is 3: 1; the mass ratio of the unpurified carbon nano tubes to the mixed gas of the acid gas and the inert gas is 1: 10; the acid gas is hydrogen chloride, and the inert gas is argon;
the unpurified carbon nano tube is purified in the mixed gas of acid gas and inert gas in the process of sliding along the spiral slideway; the purified carbon nano tube falls into a cooling tank along a connecting pipe C;
the waste gas generated in the purification process is discharged through a waste gas exhaust pipe and is treated in a centralized way;
and S5, discharging the carbon nano tubes from the discharge pipe after the carbon nano tubes are cooled by the cooling tank.
Example 4
A method for continuously preparing high-purity carbon nanotubes comprises the following steps:
s1, closing the blanking valve A, the blanking valve B, the blanking valve C and the blanking valve D, and filling unpurified carbon nano tubes into the raw material tank; then, enabling the quantitative feeder to be in an open state, and performing inert gas replacement on the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank by using a vacuum pump; the oxygen content in the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank after replacement is lower than 0.15 percent;
s2, starting the preheating reactor and the purifying reactor to ensure that the temperature in the preheating reactor is 900 ℃ and the temperature in the purifying reactor is 1300 ℃;
s3, opening a blanking valve A, a blanking valve B and a blanking valve C, and starting a quantitative blanking device; sending unpurified carbon nanotubes into the preheating reactor through a quantitative feeder under the action of gravity through a connecting pipe A; preheating is completed in the preheating reactor along with the helical blades of the preheating reactor; the preheated unpurified carbon nano tube enters the purification reactor through a connecting pipe B;
s4, continuously introducing an acid gas and an inert gas into the purification reactor, wherein the volume ratio of the acid gas to the inert gas is 5: 1; the mass ratio of the unpurified carbon nano tubes to the mixed gas of the acid gas and the inert gas is 2: 1; the acid gas is chlorine, and the inert gas is helium;
the unpurified carbon nano tube is purified in the mixed gas of acid gas and inert gas in the process of sliding along the spiral slideway; the purified carbon nano tube falls into a cooling tank along a connecting pipe C;
the waste gas generated in the purification process is discharged through a waste gas exhaust pipe and is treated in a centralized way;
and S5, discharging the carbon nano tubes from the discharge pipe after the carbon nano tubes are cooled by the cooling tank.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.

Claims (8)

1. A device for continuously preparing high-purity carbon nano tubes comprises a raw material tank, a preheating reactor, a purification reactor and a cooling tank which are sequentially connected from top to bottom; the raw material tank, the preheating reactor, the purification reactor and the cooling tank are all connected with air pumps; the preheating reactor and the cooling tank are both communicated with a protective gas inlet pipe; the method is characterized in that: the raw material tank is communicated with the preheating reactor through a connecting pipe A, the preheating reactor is communicated with the purification reactor through a connecting pipe B, and the purification reactor is communicated with the cooling tank through a connecting pipe C;
the left side of the air pump of the raw material tank is connected with an exhaust filter; the upper end of the raw material tank is communicated with a feeding pipe;
the upper part of the connecting pipe A is provided with a blanking valve A, and the lower part of the connecting pipe A is provided with a quantitative blanking device; a protective gas inlet pipe is communicated with the pipe wall of the connecting pipe A above the blanking valve A; a blanking valve B is arranged on the connecting pipe B; a blanking valve C is arranged on the connecting pipe C;
a helical blade is arranged in the preheating reactor;
a spiral slideway is arranged in the purification reactor; the purification reactor is communicated with an acid gas inlet pipe A and an inert gas inlet pipe A; the side wall of the upper part of the purification reactor is communicated with a waste gas exhaust pipe;
the bottom of the cooling tank is connected with a discharge pipe; the discharging pipe is provided with a discharging valve D.
2. The apparatus for continuously preparing high purity carbon nanotubes according to claim 1, wherein: the helical blade is fixedly arranged on the rotating shaft; a driving wheel is fixedly arranged at the upper end of the rotating shaft, and a driving motor drives the driving wheel to rotate through a driving belt;
the tail part of the connecting pipe A is a conical blanking end A; the projection of the blanking end A falls on the spiral blade;
the bottom of the preheating reactor is obliquely pointed to the lower right; the connecting pipe B is positioned on the right side of the rotating shaft.
3. The apparatus for continuously preparing high purity carbon nanotubes according to claim 2, wherein: the spiral slideway is fixed on the support column; the supporting column is a hollow cylinder;
the center of the support column is provided with an acid gas main pipe; a plurality of acid gas branch pipes are communicated with the acid gas main pipe; the acid gas branch pipe penetrates through the side wall of the support column; the top of the acid gas main pipe is closed, and the bottom of the acid gas main pipe is communicated with the acid gas inlet pipe A;
the acid gas branch pipes positioned in the support columns are all provided with one-way valves;
and a cavity between the acid gas main pipe and the support column is filled with a heat insulation material.
4. The apparatus for continuously preparing high purity carbon nanotubes according to claim 3, wherein: the tail part of the connecting pipe B is a conical blanking end B; the projection of the blanking end B falls in the spiral slideway; the bottom of the purification reactor is obliquely pointed to the lower right; connecting tube C is located to the right of the bottom of the purification reactor.
5. The apparatus for continuously preparing high purity carbon nanotubes according to claim 4, wherein: an acid gas coil and an inert gas coil are arranged in the cooling tank;
the head of the acid gas coil is communicated with the acid gas inlet pipe A; the head of the inert gas coil is communicated with an inert gas inlet pipe A; the tail part of the acid gas coil pipe penetrates through the side wall of the cooling tank and is communicated with an acid gas inlet pipe B and an inert gas inlet pipe C; the tail part of the inert gas coil is communicated with an inert gas inlet pipe B.
6. The apparatus for continuously preparing high purity carbon nanotubes according to claim 5, wherein: the lower end of the connecting pipe C is positioned in the center of the upper end surface of the cooling tank.
7. The apparatus for continuously preparing high purity carbon nanotubes according to claim 5, wherein: the acid gas inlet pipe B is externally connected with acid gas; the acid gas is one of chlorine and hydrogen chloride; the inert gas inlet pipe B, the inert gas inlet pipe C and the protective gas inlet pipe are all externally connected with inert gas; the inert gas is one of nitrogen, argon and helium.
8. The method for continuously preparing the high-purity carbon nano tube by using the device of any one of claims 1 to 7 is characterized by comprising the following steps:
s1, closing the blanking valve A, the blanking valve B, the blanking valve C and the blanking valve D, and filling unpurified carbon nano tubes into the raw material tank; then, enabling the quantitative feeder to be in an open state, and performing inert gas replacement on the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank by using a vacuum pump; the oxygen content in the raw material tank, the connecting pipe A, the preheating reactor, the purification reactor and the cooling tank after replacement is lower than 0.15 percent;
s2, starting the preheating reactor and the purifying reactor to ensure that the temperature in the preheating reactor is 700-900 ℃ and the temperature in the purifying reactor is 1000-1300 ℃;
s3, opening a blanking valve A, a blanking valve B and a blanking valve C, and starting a quantitative blanking device; sending unpurified carbon nanotubes into the preheating reactor through a quantitative feeder under the action of gravity through a connecting pipe A; preheating is completed in the preheating reactor along with the helical blades of the preheating reactor; the preheated unpurified carbon nano tube enters the purification reactor through a connecting pipe B;
s4, continuously introducing an acid gas and an inert gas into the purification reactor, wherein the volume ratio of the acid gas to the inert gas is 1: 1-5: 1; the mass ratio of the unpurified carbon nano tube to the mixed gas of the acid gas and the inert gas is 1: 10-2: 1;
the unpurified carbon nano tube is purified in the mixed gas of acid gas and inert gas in the process of sliding along the spiral slideway; the purified carbon nano tube falls into a cooling tank along a connecting pipe C;
the waste gas generated in the purification process is discharged through a waste gas exhaust pipe and is treated in a centralized way;
and S5, discharging the carbon nano tubes from the discharge pipe after the carbon nano tubes are cooled by the cooling tank.
CN202011102872.0A 2020-10-15 2020-10-15 Method and device for continuously preparing high-purity carbon nano tube Pending CN112225200A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011102872.0A CN112225200A (en) 2020-10-15 2020-10-15 Method and device for continuously preparing high-purity carbon nano tube

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011102872.0A CN112225200A (en) 2020-10-15 2020-10-15 Method and device for continuously preparing high-purity carbon nano tube

Publications (1)

Publication Number Publication Date
CN112225200A true CN112225200A (en) 2021-01-15

Family

ID=74113625

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011102872.0A Pending CN112225200A (en) 2020-10-15 2020-10-15 Method and device for continuously preparing high-purity carbon nano tube

Country Status (1)

Country Link
CN (1) CN112225200A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114100184A (en) * 2021-12-02 2022-03-01 上海氢田新材料科技有限公司 Catalyst removing device for high-temperature-resistant material
CN116281964A (en) * 2023-05-22 2023-06-23 湖南科晶新能源科技有限公司 Efficient carbon nano tube purification method and purification equipment

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1061042A1 (en) * 1999-06-15 2000-12-20 Iljin Nanotech Co., Ltd. Method for gas phase purification of carbon nanotubes by thermal treatment in diffusion furnace
CN102010730A (en) * 2010-12-19 2011-04-13 昆明理工大学 Biomass spiral pyrolytic process and antipyretic device
CN107473205A (en) * 2017-10-19 2017-12-15 焦作集越纳米材料技术有限公司 A kind of purification process of CNT
CN110079347A (en) * 2019-05-29 2019-08-02 青岛科技大学 A kind of biomass moving bed pyrolysis reactor of helix tube
CN110282614A (en) * 2019-06-26 2019-09-27 山东晶石大展纳米科技有限公司 A kind of system and method being carried out continuously Purification of Carbon Nanotubes
CN111348643A (en) * 2020-03-13 2020-06-30 内蒙古骏成新能源科技有限公司 Carbon nano tube purified by gas phase damping method, device and purification method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1061042A1 (en) * 1999-06-15 2000-12-20 Iljin Nanotech Co., Ltd. Method for gas phase purification of carbon nanotubes by thermal treatment in diffusion furnace
CN102010730A (en) * 2010-12-19 2011-04-13 昆明理工大学 Biomass spiral pyrolytic process and antipyretic device
CN107473205A (en) * 2017-10-19 2017-12-15 焦作集越纳米材料技术有限公司 A kind of purification process of CNT
CN110079347A (en) * 2019-05-29 2019-08-02 青岛科技大学 A kind of biomass moving bed pyrolysis reactor of helix tube
CN110282614A (en) * 2019-06-26 2019-09-27 山东晶石大展纳米科技有限公司 A kind of system and method being carried out continuously Purification of Carbon Nanotubes
CN111348643A (en) * 2020-03-13 2020-06-30 内蒙古骏成新能源科技有限公司 Carbon nano tube purified by gas phase damping method, device and purification method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114100184A (en) * 2021-12-02 2022-03-01 上海氢田新材料科技有限公司 Catalyst removing device for high-temperature-resistant material
CN116281964A (en) * 2023-05-22 2023-06-23 湖南科晶新能源科技有限公司 Efficient carbon nano tube purification method and purification equipment
CN116281964B (en) * 2023-05-22 2023-08-11 湖南科晶新能源科技有限公司 Efficient carbon nano tube purification method and purification equipment

Similar Documents

Publication Publication Date Title
CN109437157B (en) Floating catalyst chemical vapor deposition method for single-walled carbon nanotube
CN107601458B (en) Preparation method of single-walled carbon nanotube
CN112225200A (en) Method and device for continuously preparing high-purity carbon nano tube
WO2021147531A1 (en) Method and device for preparing carbon nanotubes and hydrogen
CN112250061A (en) Continuous preparation system and preparation method of single-walled carbon nanotubes
CN108557809A (en) A kind of graphene preparation method
CN109607513B (en) Method for preparing single-walled carbon nanotube without sulfur impurities by controllable growth promoter
CN113149115B (en) Multistage heterostructure membrane for photo-thermal seawater desalination and preparation method
CN111167460A (en) Preparation of H by direct cracking of natural gas2Catalyst with CNTs (carbon nanotubes), and preparation method and application thereof
CN109004240A (en) A kind of preparation method of high-specific surface area iron nitrogen C catalyst
CN101891184A (en) Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method
Qu et al. Two-dimensional nanomaterials: synthesis and applications in photothermal catalysis
CN101139092B (en) Method for preparing nanometer carbon tube on the aluminum foil
CN109395759B (en) Fe with core-shell structure3C nano particle and preparation method and application thereof
CN107311146A (en) A kind of serialization prepares the device and method of nano-carbon material
CN114590800A (en) Method for continuously preparing graphene by magnetically-driven sliding arc plasma high-voltage discharge
CN206089049U (en) Go to carbon nanotube purification system that mixes in succession
CN110040720A (en) High-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method
CN115304055A (en) Method for recovering polyethylene waste plastics and carbon nano tube prepared by method
CN114852996A (en) System and method for preparing single-walled carbon nanotube by electric explosion method
CN111115614B (en) Carbon nano tube prepared by catalytic cracking of hydrocarbon by rotary method, device and method
CN108236963B (en) Biomass gas purification catalyst and use method thereof
CN111441106A (en) Method for preparing high-quality graphene fibers by high-energy microwave irradiation
CN1292984C (en) Process and device for producing nano carbon fiber
CN211847156U (en) Graphene growth system

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210115