CN113353919B - Single-walled carbon nanotube preparation facilities - Google Patents

Single-walled carbon nanotube preparation facilities Download PDF

Info

Publication number
CN113353919B
CN113353919B CN202010144941.8A CN202010144941A CN113353919B CN 113353919 B CN113353919 B CN 113353919B CN 202010144941 A CN202010144941 A CN 202010144941A CN 113353919 B CN113353919 B CN 113353919B
Authority
CN
China
Prior art keywords
heating
walled carbon
heat
distributor
collecting box
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.)
Active
Application number
CN202010144941.8A
Other languages
Chinese (zh)
Other versions
CN113353919A (en
Inventor
刘强
何斌
李朋
张超
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.)
Harbin Jinna Technology Co ltd
Original Assignee
Harbin Jinna 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 Harbin Jinna Technology Co ltd filed Critical Harbin Jinna Technology Co ltd
Priority to CN202010144941.8A priority Critical patent/CN113353919B/en
Publication of CN113353919A publication Critical patent/CN113353919A/en
Application granted granted Critical
Publication of CN113353919B publication Critical patent/CN113353919B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/164Preparation involving continuous processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/159Carbon nanotubes single-walled

Abstract

A single-walled carbon nanotube preparation device belongs to the technical field of carbon nano material preparation devices. The invention solves the problem of low manufacturing efficiency in the existing single-walled carbon nanotube preparation process. The heating sleeve and the two end heat-insulating rings are sleeved outside the quartz tube, the heating sleeve comprises a heat-insulating sleeve sleeved on the quartz tube and a plurality of heating wires wound on the inner wall of the heat-insulating sleeve, and one end of each heating wire is penetrated on the heat-insulating sleeve and correspondingly connected with an armored thermocouple; the distributor is fixedly arranged above the furnace body component, a carbon source is atomized by the distributor and carbon source carrying gas introduced into the distributor and then sprayed into the reaction chamber, the material collecting box is arranged right below the furnace body component, the end part heat preservation ring positioned below is fixedly connected with the upper part of the material collecting box through a flange, and the bottom end of the quartz tube is communicated with an inlet of the material collecting box; the heating jacket is fixedly arranged on the lifting assembly at the outer part, and the lifting assembly is used for realizing the ascending and descending of the heating jacket relative to the inner quartz tube.

Description

Single-walled carbon nanotube preparation facilities
Technical Field
The invention relates to a single-walled carbon nanotube preparation device, and belongs to the technical field of carbon nanomaterial preparation devices.
Background
Carbon nanotubes can be classified into single-walled carbon nanotubes (SWNTs), double-walled carbon nanotubes (DWNTs), and multi-walled carbon nanotubes (MWNTs) according to the number of layers of carbon atoms forming the wall of the tube. Among them, the single-walled carbon nanotube can be regarded as a seamless hollow tube formed by a single-walled graphite layer being curled at a predetermined helix angle around a central axis. The single-walled carbon nanotube is composed of a graphite layer rolled into a cylindrical shape, has an extremely high aspect ratio, and is a typical one-dimensional nanomaterial. Due to the one-dimensional tubular molecular structure of the single-walled carbon nanotube (a small difference in the arrangement of atomic structures will cause a great difference in the photoelectric properties of the carbon nanotube), special properties such as excellent mechanical, electrical and optical properties are exhibited, for example: the single-walled carbon nanotube has extremely high Young modulus, tensile strength and thermal conductivity, so that the single-walled carbon nanotube has potential and wide application value in different fields of composite materials, electrode materials of new energy batteries, optoelectronic devices, biomedicine, heat transfer elements, biological and chemical sensors and the like.
The chemical vapor deposition method in the current method for preparing single-wall carbon nanotubes is generally as follows: depositing catalyst particles on the surface of the substrate, introducing a gas carbon source, and performing catalytic cracking at high temperature to form the single-walled carbon nanotube. Based on factors such as catalyst selection, carbon source selection, temperature control and the like, the single-walled carbon nanotubes prepared by the conventional method easily contain multi-walled carbon nanotubes, have high impurity content and poor morphology uniformity. Application number 201711244268.X discloses a preparation method and related application of a single-walled carbon nanotube, and introduces a reaction device of the single-walled carbon nanotube, which comprises the following steps: 1) Replacing the gas in the reaction cavity with inert gas; 2) Depositing an active element oxide on a substrate, and injecting a liquid carbon source into a liquid carbon storage device; 3) Rotating the liquid carbon storage device at a certain rotating speed, and heating to evaporate the liquid carbon source; 4) Heating to 600-1000 deg.c at certain temperature raising rate, and introducing reducing gas to prepare the single-wall carbon nanotube. However, the single-walled carbon nanotubes prepared by the device and the method grow on the substrate, and need to be cooled and separated later, so that the manufacturing efficiency is limited.
Another application No. 201710142068.7 discloses an ultra-long single-walled carbon nanotube horizontal array, a preparation method and a reaction device, which comprises the following steps: 1) Reducing the catalyst precursor into an active catalyst in a reducing atmosphere, and then rapidly cooling to a non-reaction temperature; 2) Placing the second substrate and the first substrate loaded with the active catalyst together in a stable laminar flow atmosphere with a carbon source, and then quickly heating to a growth temperature for reaction to obtain an ultra-long single-walled carbon nanotube horizontal array; 3) The reaction device at least comprises a reaction cavity and a heating device, and the reaction cavity can be rapidly heated and cooled to meet the temperature requirement required by the reaction. Therefore, the patent has strict requirements on the temperature rise and the temperature drop of the reaction cavity, and also needs to grow the single-walled carbon nanotube on the substrate (base), which also has the problem of low manufacturing efficiency.
Disclosure of Invention
The invention aims to solve the problem of low manufacturing efficiency in the existing single-walled carbon nanotube preparation process, and further provides a single-walled carbon nanotube preparation device.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a single-walled carbon nanotube preparation device, which comprises a distributor, a furnace body component, a lifting component and a material collecting box,
the furnace body component comprises a quartz tube, a heating sleeve and two end heat-insulating rings, wherein a reaction cavity is arranged in the quartz tube, the heating sleeve and the two end heat-insulating rings are sleeved outside the quartz tube, the two end heat-insulating rings are fixedly arranged at the upper end and the lower end of the heating sleeve respectively, the heating sleeve comprises a heat-insulating sleeve sleeved on the quartz tube and a plurality of heating wires sequentially wound on the inner wall of the heat-insulating sleeve from top to bottom, and one end of each heating wire is arranged on the heat-insulating sleeve in a penetrating manner and is correspondingly connected with an armored thermocouple;
the distributor is fixedly arranged above the furnace body component, a carbon source is atomized by the distributor and carbon source carrying gas introduced into the distributor and then sprayed into the reaction chamber, the material collecting box is arranged right below the furnace body component, the end part heat preservation ring positioned below is fixedly connected with the upper part of the material collecting box through a flange, and the bottom end of the quartz tube is communicated with an inlet of the material collecting box;
the heating jacket is fixedly arranged on the lifting assembly at the outer part, and the lifting assembly is used for realizing the ascending and descending of the heating jacket relative to the inner quartz tube.
Further, the lifting assembly comprises a support frame, a motor reducer assembly, a vertical threaded rod fixedly installed at the output end of the motor reducer assembly and a sliding block connected to the threaded rod in a matched mode, the motor reducer assembly is fixedly installed on the support frame, the upper end portion and the lower end portion of the threaded rod are respectively connected to the support frame in a coaxial rotating mode, one end, away from the threaded rod, of the sliding block is fixedly connected to the outer wall of the heating sleeve, an upper travel switch and a lower travel switch are installed on the support frame on one side of the threaded rod, the upper travel switch controls the limit position of the sliding block to ascend, and the lower travel switch controls the limit position of the sliding block to descend.
Furthermore, the support frame is of a cubic frame structure, and the motor reducer assembly and the material collecting box are fixedly arranged on the support frame.
Furthermore, the number of the heating wires is seven, the heat-insulating sleeve is divided into seven mutually independent sections which are respectively controlled by seven armored thermocouples, and the lower half part of the heating wires are distributed more densely than the upper half part of the heating wires.
Further, the distributor includes mixing tube, atomizer and cooling tube, and wherein the atomizer intercommunication is installed in the bottom of mixing tube, and the top processing of mixing tube has the carbon source to carry the gas import, and the carbon source import has been seted up to the upper portion lateral wall of mixing tube, the sealed suit of cooling tube is in the mixing tube outside, and the upper portion lateral wall of cooling tube has seted up cooling water inlet and cooling water outlet relatively, and the distributor is through adorning the top rigid coupling of ring flange and furnace body subassembly on the cooling tube admittedly, and the lower part of distributor is inserted and is established in the quartz capsule.
Furthermore, the outside of the cooling pipe is sleeved with a heat-insulating layer.
Furthermore, a window is formed in the material collecting box.
Furthermore, the heating sleeve and the quartz tube are in clearance fit.
Further, a single-walled carbon nanotube preparation facilities still includes tail gas processing system, tail gas processing system includes tail gas treatment jar, tail gas pipe, some firearm and dust excluding hood, tail gas treatment jar erects subaerial, and through tail gas pipe and material collecting box intercommunication, the drain has been seted up to the bottom of tail gas treatment jar, and the filler and the gas vent have been seted up at the top of tail gas treatment jar, and some firearm are installed on the gas vent top, the dust excluding hood is installed directly over the discharge port of some firearm.
Compared with the prior art, the invention has the following effects:
reaction chamber and material collecting box are relatively independent in this application, can realize continuous production and collect single walled carbon nanotube, have avoided the process of heating and cooling to reduce the energy consumption, shortened the product manufacturing time, improved work efficiency, reduced manufacturing cost, and can be according to actual production needs, scale of proportional expansion equipment.
The heating sleeve and the two end heat preservation rings provide stable conditions of high temperature and constant micro-positive pressure for reaction. The furnace body assembly realizes the accurate temperature control function through the control function of the armored thermocouple, and realizes the stable temperature condition for the reaction materials entering the reaction cavity.
Drawings
FIG. 1 is a front view (partially in section) of the present application;
FIG. 2 is a left side schematic view of FIG. 1;
FIG. 3 is a schematic right-side view of FIG. 1;
FIG. 4 is an enlarged schematic view at P of FIG. 1;
FIG. 5 is an enlarged schematic view at I of FIG. 1;
FIG. 6 is a schematic diagram of a gas path (where "liquid" is a liquid carbon source and "reserved" is a gaseous carbon source).
Detailed Description
The first embodiment is as follows: the embodiment is described with reference to fig. 1 to 6, and a single-walled carbon nanotube preparation apparatus comprises a distributor 1, a furnace body assembly, a lifting assembly and a material collection box 2,
the furnace body component comprises a quartz tube 3, a heating sleeve 4 and two end heat-insulating rings 5, a reaction cavity is arranged in the quartz tube 3, the heating sleeve 4 and the two end heat-insulating rings 5 are sleeved outside the quartz tube 3, the two end heat-insulating rings 5 are fixedly arranged at the upper end and the lower end of the heating sleeve 4 respectively, the heating sleeve 4 comprises a heat-insulating sleeve 4-1 sleeved on the quartz tube 3 and a plurality of heating wires 4-2 sequentially wound on the inner wall of the heat-insulating sleeve 4-1 from top to bottom, and one end of each heating wire 4-2 is penetrated through the heat-insulating sleeve 4-1 and is correspondingly connected with an armored thermocouple 4-3;
the distributor 1 is fixedly arranged above the furnace body component, a carbon source is atomized by the distributor 1 and the carbon source carrying gas introduced into the distributor 1 and then sprayed into the reaction chamber, the material collecting box 2 is arranged right below the furnace body component, the end part heat preservation ring 5 positioned below is fixedly connected with the upper part of the material collecting box 2 through a flange, and the bottom end of the quartz tube 3 is communicated with the inlet of the material collecting box 2;
the heating jacket 4 is externally fixed to the lifting assembly and is raised and lowered relative to the inner quartz tube 3 by the lifting assembly. By providing the lifting assembly, the quartz tube 3 can be easily replaced. The lifting assembly can be a screw slider 10 structure, and can also be any other structure capable of realizing the ascending and descending of the heating jacket 4, such as a hydraulic cylinder or a pulley block.
The carbon source enters the distributor 1 through the feeding system, the used carbon source can be a gas carbon source or a liquid carbon source, the feeding system can be a feeding system in the prior art, the gas carbon source correspondingly enters the distributor 1 through the gas feeding system and is accurately controlled through the mass flow meter, the liquid carbon source correspondingly enters the distributor 1 through the liquid feeding system and is accurately controlled through the metering pump, the liquid feeding system can be further provided with a material preheating device, the temperature control range of the material preheating device is 100-500 ℃, and liquid atomization is facilitated.
The heating jacket 4 and the two end heat preservation rings 5 provide stable high temperature and constant micro-positive pressure conditions for the reaction. The furnace body assembly realizes an accurate temperature control function through the input of current and voltage provided by an external control part and the control function of the armored thermocouple 4-3, realizes the stable temperature condition of reaction materials entering a reaction cavity, and the end heat-insulating ring 5 and the heat-insulating sleeve 4-1 are made of the same material and insulate the quartz tube 3, so that the influence on the preparation process due to the thermal loss and the generation of thermal convection in the furnace body is prevented. The external control part is conventional technical means in the field and is not described in detail herein.
The material collecting box 2 is closely communicated with the lower part of the quartz tube 3 to form a transition cavity, and the transition cavity plays a role in cooling the single-walled carbon nanotube and the tail gas.
The distributor 1 atomizes the material which is accurately controlled and then leads the material into the reaction cavity, and the material reacts in the reaction cavity to generate black powder, namely a single-walled carbon nanotube, and the black powder falls into the material collecting box 2 along with the cooling of tail gas through the transition cavity.
Reaction chamber and material collecting box 2 relatively independent in this application can realize continuous production and collect single walled carbon nanotube, have avoided the process of heating and cooling to reduce the energy consumption, shortened the product manufacturing time, improved work efficiency, reduced manufacturing cost, and can be according to actual production needs, scale of proportional expansion equipment.
As shown in the schematic gas path diagram of fig. 6, a liquid carbon source is sequentially fed into a carbon source inlet through a manual valve, a liquid pump and a gasification device, a gas carbon source is sequentially fed into the carbon source inlet through the manual valve, a float flowmeter, an electromagnetic valve and a pneumatic valve, and the liquid carbon source and the gas carbon source are parallelly connected and enter the carbon source inlet; and the nitrogen and the hydrogen respectively enter the carbon source carrying gas inlet through the manual valve, the MFC and the liquid pump in sequence.
The method is suitable for preparing the single-walled carbon nanotube by a direct method, a substrate is not needed, liquid is atomized by a distributor and directly produces the single-walled carbon nanotube through high-temperature reaction, and the generated product is cooled by a transition cavity and a collecting box to obtain a finished product. In the prior art, the semi-finished product prepared by the substrate preparation method is cooled, and the carbon nano tube is required to be stripped from the substrate to obtain a final product; and the substrate area is limited, and the substrate can be saturated when growing to a certain degree, so that the substrate needs to be replaced by cooling equipment.
The lifting assembly comprises a support frame 7, a motor reducer assembly 8, a threaded rod 9 vertically fixedly installed at the output end of the motor reducer assembly 8 and a slider 10 connected to the threaded rod 9 in a matched mode, the motor reducer assembly 8 is fixedly installed on the support frame 7, the upper end and the lower end of the threaded rod 9 are respectively connected to the support frame 7 in a coaxial rotating mode, one end, far away from the threaded rod 9, of the slider 10 is fixedly connected to the outer wall of the heating sleeve 4, an upper travel switch 11 and a lower travel switch 12 are installed on the support frame 7 on one side of the threaded rod 9, the slider 10 is controlled to ascend through the upper travel switch 11, and the slider 10 is controlled to descend through the lower travel switch 12. By adopting the design, the rotary motion of the electric surface is converted into linear displacement through the structure of the screw rod slide block 10, so that the heating jacket 4 is lifted and lowered, and the slide block 10, namely the lifting and lowering limit positions of the heating jacket 4, are controlled through the upper and lower stroke switches 12. The upper end and the lower end of the threaded rod 9 are limited by the supporting frame 7, so that the threaded rod 9 is prevented from inclining to influence the up-and-down movement of the sliding block 10. Slider 10 and heating jacket 4 between can be connected through the connecting piece, promptly the surface at heating jacket 4 is established to the connecting piece full package or half package, slider 10 and connecting piece pass through threaded connection, so convenient to detach just can guarantee that heating jacket 4 keeps coaxial with inside quartz capsule 3 throughout rising and decline in-process.
The support frame 7 is of a cubic frame structure, and the motor reducer assembly 8 and the material collecting box 2 are fixedly arranged on the support frame 7. By such design, the supporting frame 7 provides rigid support and stable installation for the lifting assembly and the material collection rib, etc., thereby realizing the requirement of precise installation.
The number of the heating wires 4-2 is seven, the heat-insulating sleeve 4-1 is divided into seven mutually independent sections which are respectively controlled by seven armored thermocouples 4-3, and the heating wires 4-2 at the lower half part are distributed more densely than the heating wires 4-2 at the upper half part. The design completely meets the temperature condition of 600-1500 ℃ for preparing the single-walled carbon nanotube, and can better control the temperature in the reaction cavity.
The distributor 1 comprises a mixing pipe 13, an atomizing spray head 14 and a cooling pipe 15, wherein the atomizing spray head 14 is communicated and arranged at the bottom end of the mixing pipe 13, a carbon source carrying gas inlet 13-1 is processed at the top end of the mixing pipe 13, a carbon source inlet 13-2 is formed in the upper side wall of the mixing pipe 13, the cooling pipe 15 is hermetically sleeved outside the mixing pipe 13, a cooling water inlet 15-1 and a cooling water outlet 15-2 are formed in the upper side wall of the cooling pipe 15 relatively, the distributor 1 is fixedly connected with the top end of the furnace body assembly through a flange plate fixedly arranged on the cooling pipe 15, and the lower part of the distributor 1 is inserted into the quartz pipe 3. By the design, carbon source and carbon source carrying gas are respectively fed into the mixing pipe 13 through the carbon source inlet 13-2 and the carbon source carrying gas inlet 13-1 to be mixed, and are finally atomized by the atomizing nozzle 14 and then sprayed into the reaction cavity. Still can set up gas distribution pipe 16 in the hybrid tube 13, processing has a plurality of through-holes on the gas distribution pipe 16, and carbon source carries gas and mixes in hybrid tube 13 through a plurality of through-holes and carbon source. Through the setting of distributor 1 in this application, can effectively improve single-walled carbon nanotube's purity and appearance control. Through setting up cooling tube 15, effectively avoid high temperature to damage to can atomize liquid material to nanometer yardstick, effectively improve reactivity, make the reaction more abundant.
The cooling pipe 15 is externally sleeved with an insulating layer 17.
The material collecting box 2 is provided with a window 2-1. So design, can observe the inside state of material collecting box 2 through window 2-1.
The heating sleeve 4 is in clearance fit with the quartz tube 3. So design, when the later stage of being convenient for need clear up quartz capsule 3, separation heating jacket 4 and quartz capsule 3 that can be smooth.
The utility model provides a single wall carbon nanotube preparation facilities still includes tail gas processing system, tail gas processing system includes tail gas treatment tank 18, tail gas pipe 19, some firearm 20 and dust excluding hood 21, tail gas treatment tank 18 erects subaerial, and communicates with material collecting box 2 through tail gas pipe 19, and drain 18-1 has been seted up to the bottom of tail gas treatment tank 18, and filler 18-2 and gas vent have been seted up at the top of tail gas treatment tank 18, and some firearm 20 is installed on the gas vent top, dust excluding hood 21 is installed directly over the discharge port of some firearm 20. So designed, one end of the tail gas conduit 19 is positioned at the upper part of the material collecting box 2, and the other end is positioned at the lower part of the tail gas processing tank 18. H-containing gas generated in the reaction chamber2、CO、CH4After the tail gas is treated by the tail gas treatment tank 18 and the igniter 20, only the nitrogen is left and is directly discharged into the atmosphere through the dust removal cover 21, so that the method is safer and more environment-friendly. The dust hood adopts the prior art, can also be a device capable of realizing dust removal such as a bag-type dust remover, and the tail gas treatment tank 18 is a precipitation tank which is the prior art, and the liquid in the tail gas treatment tank is water to prevent dust from flying.
The preparation method comprises the following steps:
(1) The furnace body component is heated to a set temperature according to a certain heating rate of 1h, and simultaneously the flow is 1L/minN2Making the reaction chamber in inert atmosphere; the rate of temperature rise can be 1 deg.C-20 deg.C/min, preferably 5 deg.C/min. The set temperature can be between 750 and 1500 ℃ and is preferably 900 ℃.
(2) After reaching the set temperature and keeping the temperature for 30min, introducing 1L/minH of flow2,N2Adjusting the flow rate to 0.3L/min, stabilizing for 30min, introducing the prepared carbon source into the reaction chamber through the distributor 1, reacting at high temperature to obtain black powder, namely single-walled carbon nanotube, naturally falling to the material collection box 2, igniting the tail gas by the igniter 20, and only leaving N2And can be directly discharged into the atmosphere. The reaction time can be controlled according to the needs, and the temperature is naturally reduced after the reaction is finished. ( The reaction can be terminated when the set reaction time is reached. The natural cooling refers to a state that the heater stops heating. The heat preservation layer 17 is passive and does not work when the temperature is reduced. )
(3) After equipment falls to the room temperature, improve heating jacket 4 through promoting the subassembly, then lift the flange between furnace body subassembly and the material collecting box 2 off, take off quartz capsule 3 and clear up the result that bonds in quartz capsule 3 (the bonding too much can lead to reaction space to diminish, the product quality reduces the scheduling problem, must regularly clear up, just can have stable production efficiency), the back of finishing is cleared up, resume the flange joint between furnace body subassembly and the material collecting box 2, and descend back to the normal position through promoting the subassembly with heating jacket 4. The next preparation can be carried out according to the requirement.
Other processes for the preparation of single-walled carbon nanotubes not described in the present application are partly referred to in the prior art.

Claims (8)

1. A single-walled carbon nanotube preparation device is characterized in that: it comprises a distributor (1), a furnace body component, a lifting component and a material collecting box (2),
the furnace body component comprises a quartz tube (3), a heating sleeve (4) and two end heat-insulating rings (5), a reaction cavity is arranged in the quartz tube (3), the heating sleeve (4) and the two end heat-insulating rings (5) are sleeved outside the quartz tube (3), the two end heat-insulating rings (5) are fixedly arranged at the upper end and the lower end of the heating sleeve (4) respectively, the heating sleeve (4) comprises a heat-insulating sleeve (4-1) sleeved on the quartz tube (3) and a plurality of heating wires (4-2) sequentially wound on the inner wall of the heat-insulating sleeve (4-1) from top to bottom, one end of each heating wire (4-2) penetrates through the heat-insulating sleeve (4-1) and is correspondingly connected with an armored thermocouple (4-3);
the distributor (1) is fixedly arranged above the furnace body component, a carbon source is atomized by the distributor (1) and the carbon source carrying gas introduced into the distributor (1) and then sprayed into the reaction chamber, the material collecting box (2) is arranged right below the furnace body component, an end heat-insulating ring (5) positioned below is fixedly connected with the upper part of the material collecting box (2) through a flange, and the bottom end of the quartz tube (3) is communicated with an inlet of the material collecting box (2);
the heating sleeve (4) is fixedly arranged on the lifting assembly at the outer part, and the lifting assembly is used for realizing the ascending and descending of the heating sleeve relative to the inner quartz tube (3);
the lifting assembly comprises a support frame (7), a motor reducer assembly (8), a vertical threaded rod (9) fixedly installed at the output end of the motor reducer assembly (8) and a sliding block (10) connected to the threaded rod (9) in a matched mode, the motor reducer assembly (8) is fixedly installed on the support frame (7), the upper end portion and the lower end portion of the threaded rod (9) are respectively connected to the support frame (7) in a coaxial rotating mode, one end, far away from the threaded rod (9), of the sliding block (10) is fixedly connected with the outer wall of the heating sleeve (4), an upper travel switch (11) and a lower travel switch (12) are installed on the support frame (7) on one side of the threaded rod (9), the upper travel switch (11) and the lower travel switch (12) are used for controlling the ascending limit position of the sliding block (10) and the descending limit position of the sliding block (10) through the lower travel switch (12).
2. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 1, wherein: the support frame (7) is of a cubic frame structure, and the motor reducer assembly (8) and the material collecting box (2) are fixedly arranged on the support frame (7).
3. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 2, wherein: the number of the heating wires (4-2) is seven, the heat-insulating sleeve (4-1) is divided into seven mutually independent sections and is independently controlled by seven armored thermocouples (4-3), and the lower half part of the heating wires (4-2) is distributed more densely than the upper half part of the heating wires (4-2).
4. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 1, 2 or 3, wherein: distributor (1) includes mixing tube (13), atomizer (14) and cooling tube (15), and wherein atomizer (14) intercommunication is installed in the bottom of mixing tube (13), and the top processing of mixing tube (13) has carbon source to carry gas inlet (13-1), and carbon source inlet (13-2) have been seted up to the upper portion lateral wall of mixing tube (13), cooling tube (15) sealed suit is outside in mixing tube (13), and cooling tube (15) upper portion lateral wall has seted up relatively cooling water inlet (15-1) and cooling water outlet (15-2), and distributor (1) is through the top rigid coupling of the ring flange of adorning on cooling tube (15) with the furnace body subassembly, and the lower part of distributor (1) is inserted and is established in quartz capsule (3).
5. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 4, wherein: the cooling pipe (15) is sleeved with a heat-insulating layer (17).
6. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 4, wherein: the material collecting box (2) is provided with a window (2-1).
7. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 6, wherein: the heating sleeve (4) is in clearance fit with the quartz tube (3).
8. The apparatus for preparing single-walled carbon nanotubes as claimed in claim 7, wherein: the utility model provides a single walled carbon nanotube preparation facilities still includes tail gas processing system, tail gas processing system includes tail gas treatment tank (18), tail gas pipe (19), some firearm (20) and dust excluding hood (21), tail gas treatment tank (18) erect subaerial, and through tail gas pipe (19) and material collecting box (2) intercommunication, drain (18-1) have been seted up to the bottom of tail gas treatment tank (18), and the top of tail gas treatment tank (18) has been seted up and has been added mouth of a river (18-2) and gas vent, installs on the gas vent top in some firearm (20), dust excluding hood (21) are installed directly over the discharge port of some firearm (20).
CN202010144941.8A 2020-03-04 2020-03-04 Single-walled carbon nanotube preparation facilities Active CN113353919B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010144941.8A CN113353919B (en) 2020-03-04 2020-03-04 Single-walled carbon nanotube preparation facilities

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010144941.8A CN113353919B (en) 2020-03-04 2020-03-04 Single-walled carbon nanotube preparation facilities

Publications (2)

Publication Number Publication Date
CN113353919A CN113353919A (en) 2021-09-07
CN113353919B true CN113353919B (en) 2022-11-01

Family

ID=77523443

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010144941.8A Active CN113353919B (en) 2020-03-04 2020-03-04 Single-walled carbon nanotube preparation facilities

Country Status (1)

Country Link
CN (1) CN113353919B (en)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4292137A (en) * 1979-09-07 1981-09-29 Sumitomo Heavy Industries, Ltd. Door lifter for coke oven
US5942110A (en) * 1997-12-29 1999-08-24 Norris; Samuel C Water treatment apparatus
FI20070231A0 (en) * 2007-03-21 2007-03-21 Beneq Oy Device for producing nanotubes
WO2007098948A1 (en) * 2006-03-02 2007-09-07 Clyvia Technology Gmbh Depolymerisation installation and method for the operation and maintenance thereof
CN101087730A (en) * 2004-12-13 2007-12-12 日机装株式会社 Process for producing monolayer carbon nanotube
CN105439119A (en) * 2015-12-02 2016-03-30 苏州捷迪纳米科技有限公司 Vertical continuous preparing device for carbon nano tube fibers and preparing method
CN107555421A (en) * 2017-10-31 2018-01-09 南京旭羽睿材料科技有限公司 A kind of graphene growth protection device
CN209049165U (en) * 2018-10-29 2019-07-02 陕西思维印务有限公司 A kind of spray dust-reducing system
CN110668432A (en) * 2019-09-27 2020-01-10 北京碳垣新材料科技有限公司 Device for growing graphene by taking metal powder liquid phase as substrate

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7250148B2 (en) * 2002-07-31 2007-07-31 Carbon Nanotechnologies, Inc. Method for making single-wall carbon nanotubes using supported catalysts
CN201352050Y (en) * 2009-02-23 2009-11-25 石毓忠 Far infrared fast thermal-circulation energy-saving oven
CN207738888U (en) * 2017-12-29 2018-08-17 晶创铭盛电子科技(香河)有限公司 A kind of single crystal growing furnace Novel crucible driving device

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4292137A (en) * 1979-09-07 1981-09-29 Sumitomo Heavy Industries, Ltd. Door lifter for coke oven
US5942110A (en) * 1997-12-29 1999-08-24 Norris; Samuel C Water treatment apparatus
CN101087730A (en) * 2004-12-13 2007-12-12 日机装株式会社 Process for producing monolayer carbon nanotube
WO2007098948A1 (en) * 2006-03-02 2007-09-07 Clyvia Technology Gmbh Depolymerisation installation and method for the operation and maintenance thereof
FI20070231A0 (en) * 2007-03-21 2007-03-21 Beneq Oy Device for producing nanotubes
CN105439119A (en) * 2015-12-02 2016-03-30 苏州捷迪纳米科技有限公司 Vertical continuous preparing device for carbon nano tube fibers and preparing method
CN107555421A (en) * 2017-10-31 2018-01-09 南京旭羽睿材料科技有限公司 A kind of graphene growth protection device
CN209049165U (en) * 2018-10-29 2019-07-02 陕西思维印务有限公司 A kind of spray dust-reducing system
CN110668432A (en) * 2019-09-27 2020-01-10 北京碳垣新材料科技有限公司 Device for growing graphene by taking metal powder liquid phase as substrate

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
浮动催化剂化学气相沉积法可控制备半导体性单壁碳纳米管;郭舒予;《中国优秀硕士学位论文全文数据库》;20160601;全文 *
用浮动催化裂解法制取单壁碳纳米管;韦进全等;《清华大学学报(自然科学版)》;20010830(第08期);全文 *

Also Published As

Publication number Publication date
CN113353919A (en) 2021-09-07

Similar Documents

Publication Publication Date Title
US10774449B2 (en) Device for producing carbon nanotube fibers and method for producing carbon nanotube fibers using same
CN100391831C (en) Method of preparing carbon nanocages
CN101456580B (en) Method for preparing stannic oxide nano wire
WO2022062446A1 (en) Continuous preparation system and preparation method for single-wall carbon nanotubes
CN102950291B (en) Production method of submicron-order tin-copper alloy powder
US10144647B2 (en) Ultrathin carbon nanotube film and preparation method and apparatus thereof
KR20180074226A (en) Apparatus for boron nitride nanotubes and method of manufacturing boron nitride nanotubes using the same
CN113353919B (en) Single-walled carbon nanotube preparation facilities
CN111892040B (en) Method for preparing graphene by arc process
CN108467024B (en) Fluidized bed for batch preparation of carbon nanotubes based on chemical vapor deposition method
KR101220846B1 (en) Apparatus for preparing catalyst for synthesis of carbon nano tube
CN114887552B (en) Injection structure for preparing carbon nanotube material and application thereof
US20140199546A1 (en) Multi-branched n-doped carbon nanotubes and the process for making same
CN210366999U (en) A device for preparing graphite alkene
CN218261985U (en) Device for continuously preparing carbon nano tube by chemical vapor deposition method
KR101930918B1 (en) the fabricating method of metal oxides-carbon nano tube composite and the use thereof
CN220597056U (en) Device for continuously producing carbon nano tube with assistance of inductor
CN107459030A (en) Produce the synthesizer of CNT in batches
CN216273120U (en) Continuous reaction device for synthesizing carbon nano tube by chemical vapor deposition method
CN110217778A (en) A kind of device and preparation method thereof of continuous preparation high quality carbon nanotube
KR101626645B1 (en) Apparatus for producing polysilicon and preparation of polysilicon using same
CN111115614B (en) Carbon nano tube prepared by catalytic cracking of hydrocarbon by rotary method, device and method
CN116889838A (en) Device and method for improving yield of single-walled carbon nanotubes prepared by floating catalytic method
CN115928266A (en) Equipment for continuously preparing carbon nano tube long fiber
KR101755764B1 (en) Apparatus for producing polysilicon and preparation of polysilicon using same

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
GR01 Patent grant
GR01 Patent grant